CN110350081A - A kind of multifunction flexible Piezoelectric anisotropy film of ordered structure and preparation method thereof - Google Patents
A kind of multifunction flexible Piezoelectric anisotropy film of ordered structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses multifunction flexible Piezoelectric anisotropy films of a kind of ordered structure and preparation method thereof, are related to flexible piezoelectric Material Field, can prepare the high flexibility function piezoelectric membrane of a Species sensitivity, and preparation method simple process, low cost.The present invention includes: that polymer powder is dissolved in solvent, and piezoelectric monocrystal microplate is distributed in solvent, respectively obtains polymer solution and piezoelectric monocrystal microplate dispersion liquid；Sheet glass is inserted into polymer solution and is stood, then sheet glass is dried；Piezoelectric monocrystal microplate suspension is uniformly slowly dripped into the inclined glass sheet surface with layer polymerization object, and flows through suspension in polymer surfaces, then sheet glass is dried；Circulation executes, until glass sheet surface forms the multifunction flexible Piezoelectric anisotropy film of multilayer order structure.It invention can be widely used in the fields such as intelligent wearable device, flexible robot, collection of energy and biomedicine.
Description
Technical field
The present invention relates to the multifunction flexible Piezoelectric anisotropy of flexible piezoelectric Material Field more particularly to a kind of ordered structure is thin
Film and preparation method thereof.
Background technique
In recent years, flexible wearable equipment and artificial intelligence field are grown rapidly, and to its core component --- sensing
The requirement of device is also higher and higher, and this kind of flexible sensor is mainly made of some function films with special micro-structure.It is high
The exploitation of performance functionalization film is the prerequisite in flexible sensor field, and the performance of function film ontology is directly related to machine
The intelligence and multifunction of the carriers such as device people, Medical Devices, human body artificial limb and wearable device, and receive multidisciplinary research
The great attention of personnel.Early in 1991, T.R.Jensen et al., which has developed, had tactile for cover robotic surface
The functionalization film of function, although the functionalization film can perceive effect and the sending of external force using internal sensor array
Response, but the multi-functional and stability of these functionalization films is poor, after being used for multiple times, functionalization film is to extraneous force-responsive
Susceptibility apparent weaken occurs.With the development of sensing technology, in 2004, Tokyo Univ Japan, which develops, a to be had
Miniature rubber electric resistance sensor is drawn into molecular semiconductor crystal by the flexibility function film of feeling function, the functionalization film
Size is simultaneously fabricated on substrate material, and sensor forms the functionalization film that array is fabricated to flexible changeable shape, the function
Change film to be used for robot and pressure and temperature can be measured simultaneously.But since the sensor is sensed using resistive pressure
Device, and the functionalization film is relatively thin, under the action of same applied force, the specific torque of generation is smaller, therefore, the functionalization
Film has poor sensitivity.Chinese invention CN107123470A develops a kind of flexible functionalization film, the conductive thin
Film includes elastic substrates, nonrigid connector and the nano wire of pre-stretching.Nonrigid connector is located at the elastic substrates of pre-stretching and receives
Between rice conducting wire, nonrigid connector material part is embedded into formation mixed transition area in nano wire, to enhance the bonding of interlayer
Performance.Although functionalization film sensitivity with higher prepared by the invention, the preparation method of the functionalization film compared with
For complexity.In addition to this, Chinese invention CN108896219A is developed for a kind of flexible bionic functionalization film, wherein sensing layer
Including piezoresistance layer, membrane electrode, wherein piezoresistance layer has porous structure, contacts boundary to piezoresistance layer and membrane electrode using elastomer
Face region is filled, which can experience the presence of air-flow and pressure, and the flexible bionic function
Film can be changed with certain mechanical stability.
From the point of view of the Nomenclature Composition and Structure of Complexes of functionalization film, sensor mainly has condenser type, and pressure resistance type and friction are sensor-type, removes
It is above-mentioned outer, it is seldom to the research of piezoelectric type function film.Piezoelectric pressure indicator is generally by piezopolymer or inorganic functional
Material is combined with polymeric matrix.Up to the present, many micro nano structure functional materials, such as BaTiO3Nano wire, Ge/
Si nano wire, single-walled carbon nanotube (SWNT) and PZT nanometer stick array, it has therefore proved that, the device under small outer pressure condition (<
10kPa) there is very high sensitivity.Although these work have good effect to the sensitivity for improving functionalization film,
The preparation method of nano wire, nanometer rods and microarray is complex, repeatable poor and higher cost.Therefore, become for
Urgent problem to be solved.
Summary of the invention
The present invention provides a kind of multifunction flexible Piezoelectric anisotropy film and preparation method thereof of ordered structure, can prepare
The high flexibility function piezoelectric membrane of one Species sensitivity, and preparation method simple process, low cost.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of preparation method of the multifunction flexible Piezoelectric anisotropy film of ordered structure, comprising:
S1, polymer powder is dissolved in solvent, piezoelectric monocrystal microplate is distributed in solvent, polymer is respectively obtained
Solution and piezoelectric monocrystal microplate dispersion liquid；
S2, it will be stood in sheet glass insertion polymer solution, then sheet glass dried, glass sheet surface forms polymer and covers
Film；
S3, piezoelectric monocrystal microplate suspension is uniformly slowly dripped into glass sheet surface, makes piezoelectric monocrystal microplate described
It is tiled and is orientated with the direction crystal face 00l, then sheet glass is dried in polymer overlay film surface；
S4, circulation execute S2-S3, until glass sheet surface forms the multifunction flexible Piezoelectric anisotropy film of ordered structure.
Further, the preparation method of the multifunction flexible Piezoelectric anisotropy film of ordered structure further include:
Gold electrode is plated by ion sputtering on the multifunction flexible Piezoelectric anisotropy film of ordered structure, and upper and lower two
Face extraction wire；
Dimethyl silicone polymer is mixed with curing agent with weight ratio 10:1, and spin coating is covered in up and down the two of electrode
Face, the baking and curing at 80 DEG C, the piezoelectric membrane being completed.
Further, polymer includes polyvinyl alcohol, Kynoar, Kynoar base co-polymer, polylactic acid, poly- two
Methylsiloxane, polyurethane, polyacrylic resin, polyolefin.
Further, solvent includes water, N, N- dimethylene formamide, N-Methyl pyrrolidone it is one or more.
Further, the concentration of polymer solution is 0.5~3wt%.
Further, piezoelectric material monocrystalline microplate includes barium titanate single-crystal microplate, lead titanate monocrystal microplate, lead magnesio-niobate-
Lead titanate monocrystal microplate, sodium niobate monocrystalline microplate, potassium-sodium niobate monocrystalline microplate, lithium niobate monocrystal microplate, monocrystalline lithium tantalate microplate,
Single crystal quartz microplate.
Further, piezoelectric material monocrystalline microplate with a thickness of 1nm~100nm, long and width is 1 μm~10 μm.
Further, the concentration of piezoelectric monocrystal microplate dispersion liquid is 1~5wt%.
Further, the piezoelectric membrane being completed is with a thickness of 1-1000 μm.
The present invention also provides a kind of multifunction flexible Piezoelectric anisotropy films of ordered structure, are made by above-mentioned preparation method.
The beneficial effects of the present invention are:
The flexible piezoelectric laminated film for the ordering hybrid that the LBL self-assembly method that the present invention uses is formed,
The functionalization film has the characteristics that the sensitivity of height, response time is short and stable structure, compared to traditional condenser type,
Resistance-type and organic crystal tubular type sensor, the functionalization film in the present invention have preparation method simple, and it is expensive, difficult to avoid
The use of the nano materials such as processing, complicated microarray, nano wire or nanometer rods.
Also, these nano materials with micro-nano structure in process there is inevitably be unevenly distributed and
The problems such as repeatability is low.And the piezoelectric material monocrystalline microplate to tile in the present invention is easy in polymer surfaces orientations, layer with
The structure of the hybrid of Mussel shell is similar between layer, this kind of structure can not only improve the stability of film, and phase
Adjacent bed orientation piezoelectric material monocrystalline microplate can play complementation so that functionalization film of the invention have high sensitive and
Excellent mechanical property.
On the other hand, which can be converted to electric signal for the vibration of the vocal cords muscle of human body, according to human body sound
Difference with pronunciation generates corresponding electric signal, and has repeatability and higher reliability, the language in artificial intelligence
Sound identifying system field has potential application.
In addition to this, which can also perceive the faint physiological signal of human body, for example, pulse, heartbeat and fortune
Emotionally condition can play an important role in field of biomedicine.
In conclusion the high susceptibility that functionalization film has prepared by the present invention, preparation method are simple and low
The advantages such as cost provide possibility for its practical application in wearable device and field of biomedicine.
Detailed description of the invention
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to needed in the embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is ordered into the multifunction flexible Piezoelectric anisotropy film microstructure plan view of structure；
Fig. 2 is ordered into the multifunction flexible Piezoelectric anisotropy film microstructure three-dimensional figure of structure；
Fig. 3 is ordered into the structural plan figure after the multifunction flexible Piezoelectric anisotropy thin-film package of structure.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, With reference to embodiment to this
Invention is described in further detail.
Embodiment 1:
0.5g polyvinylidene fluoride copolymer P (VDF-TrFE) powder is dissolved in 100mL N,N-dimethylformamide first
(DMF) spare in solvent, then by 0.5g BaTiO3Monocrystalline microplate is distributed to 50mL DMF (N, N-
Dimethylformamide n,N-Dimethylformamide) in solvent, the suspended of piezoelectric monocrystal microplate is formed by ultrasound, stirring
Then clean sheet glass is inserted into above-mentioned P (VDF-TrFE) solution by liquid, after standing 3 minutes, then drying is inhaled with dropper
Take 10mL BaTiO3Monocrystalline microplate suspension uniformly slowly drips to inclined above-mentioned sheet glass, dries sheet glass.By sheet glass
It is added dropwise again after insertion P (VDF-TrFE) solution process and so on 150 times of the drying of monocrystalline microplate suspension, forms ordered structure
Multifunction flexible Piezoelectric anisotropy film, as shown in Figure 1, 2.
By magnetron sputtering, gold electrode is uniformly plated in laminated film upper and lower surface, and in upper and lower surface extraction wire.So
Dimethyl silicone polymer is mixed with curing agent with weight ratio 10:1 afterwards, and spin coating is covered in the upper and lower surface of electrode,
Solidify 10h in 80 DEG C of baking oven, the structure chart after encapsulation is as shown in Figure 3.After the completion of encapsulation, the sensitivity test of device is carried out.
Embodiment 2:
0.5g PVA (polyvinyl alcohol polyvinyl alcohol) powder is dissolved in 100mL deionized water first, it is standby
With then by 0.5g BaTiO3Monocrystalline microplate is distributed in 50mL deionized water, micro- by ultrasonic, stirring forms piezoelectric monocrystal
Then clean sheet glass is inserted into above-mentioned PVA aqueous solution by the suspension of piece, after standing 3 minutes, then dropper is used in drying
Draw 10mL BaTiO3Monocrystalline microplate suspension uniformly slowly drips to inclined above-mentioned sheet glass, drying.Sheet glass is inserted into
It is added dropwise again after PVA solution process and so on 150 times of the drying of monocrystalline microplate suspension, forms the multifunction flexible of ordered structure
Piezoelectric anisotropy film.
By magnetron sputtering, gold electrode is uniformly plated in laminated film upper and lower surface, and in upper and lower surface extraction wire.So
Dimethyl silicone polymer is mixed with curing agent with weight ratio 10:1 afterwards, and spin coating is covered in the upper and lower surface of electrode,
Solidify 10h in 80 DEG C of baking oven.After the completion of encapsulation, the sensitivity test of device is carried out.
Embodiment 3:
0.5g P (VDF-TrFE) powder is dissolved in 100mL DMF solvent first, it is spare, then by 0.5g
PbTiO3Monocrystalline microplate is distributed in 50mL DMF solvent, forms PbTiO by ultrasound, stirring3The suspension of monocrystalline microplate, so
Clean sheet glass is inserted into above-mentioned P (VDF-TrFE) solution afterwards, after standing 3 minutes, then drying draws 10mL with dropper
PbTiO3Monocrystalline microplate suspension uniformly slowly drips to inclined above-mentioned sheet glass, drying.Sheet glass is inserted into P (VDF-
TrFE it) is added dropwise again after solution process and so on 150 times of the drying of monocrystalline microplate suspension, forms the multi-functional soft of ordered structure
Property Piezoelectric anisotropy film.
By magnetron sputtering, gold electrode is uniformly plated in electric laminated film upper and lower surface, and in upper and lower surface extraction wire.
Then dimethyl silicone polymer is mixed with curing agent with weight ratio 10:1, and spin coating is covered in the upper and lower surface of electrode,
Solidify 10h in 80 DEG C of baking oven.After the completion of encapsulation, the sensitivity test of device is carried out.
Embodiment 4:
0.5g PVA powder is dissolved in 100mL deionized water first, it is spare, then by 0.5g Pb (Mg1/3Nb2/3)
O3-PbTiO3Monocrystalline microplate is distributed in 50mL deionized water, forms Pb (Mg by ultrasound, stirring1/3Nb2/3)O3-PbTiO3It is single
Then clean sheet glass is inserted into above-mentioned PVA aqueous solution by the suspension of brilliant microplate, after standing 3 minutes, then drying is used
Dropper draws 10mL Pb (Mg1/3Nb2/3)O3-PbTiO3Monocrystalline microplate suspension uniformly slowly drips to inclined above-mentioned glass
Piece, drying.Sheet glass is inserted into after PVA solution to process and so on 150 times that the drying of monocrystalline microplate suspension is added dropwise again, is formed
The multifunction flexible Piezoelectric anisotropy film of ordered structure.
By magnetron sputtering, gold electrode is uniformly plated in laminated film upper and lower surface, and in upper and lower surface extraction wire.So
Dimethyl silicone polymer is mixed with curing agent with weight ratio 10:1 afterwards, and spin coating is covered in the upper and lower surface of electrode,
Solidify 10h in 80 DEG C of baking oven.After the completion of encapsulation, the sensitivity test of device is carried out.
Embodiment 5:
3g dimethyl silicone polymer is uniformly mixed with 0.3g curing agent first, it is spare, then by 0.5g Pb (Mg1/ 3Nb2/3)O3-PbTiO3Monocrystalline microplate is distributed in 50mL DMF solvent, forms Pb (Mg by ultrasound, stirring1/3Nb2/3)O3-
PbTiO3Then clean sheet glass is inserted into above-mentioned dimethyl silicone polymer mixed sols by the suspension of monocrystalline microplate, quiet
After setting 3 minutes, then 100 DEG C of solidification 3h draw 10mL Pb (Mg with dropper1/3Nb2/3)O3-PbTiO3Monocrystalline microplate suspension is equal
It is even slowly to drip to inclined above-mentioned sheet glass, drying.Monocrystalline is added dropwise again after sheet glass is inserted into dimethyl silicone polymer solution
Process and so on 150 times of microplate suspension drying, form the multifunction flexible Piezoelectric anisotropy film of ordered structure.
By magnetron sputtering, gold electrode is uniformly plated in laminated film upper and lower surface, and in upper and lower surface extraction wire.So
Dimethyl silicone polymer is mixed with curing agent with weight ratio 10:1 afterwards, and spin coating is covered in the upper and lower surface of electrode,
Solidify 10h in 80 DEG C of baking oven.After the completion of encapsulation, the sensitivity test of device is carried out.
Comparative example 1:
0.5g P (VDF-TrFE) powder is dissolved in 100mL DMF solvent first, it is spare, then by 0.5g
BaTiO3Micro particles are distributed in 50mL DMF solvent, form BaTiO by ultrasound, stirring3The suspension of micro particles, so
Clean sheet glass is inserted into above-mentioned P (VDF-TrFE) solution afterwards, after standing 3 minutes, then drying draws 10mL with dropper
BaTiO3Micro particles suspension uniformly slowly drips to inclined above-mentioned sheet glass, drying.Sheet glass is inserted into P (VDF-
TrFE it) is added dropwise again after solution process and so on 150 times of the drying of micro particles suspension, forms the multi-functional soft of ordered structure
Property Piezoelectric anisotropy film.
By magnetron sputtering, gold electrode is uniformly plated in laminated film upper and lower surface, and in upper and lower surface extraction wire.So
Dimethyl silicone polymer is mixed with curing agent with weight ratio 10:1 afterwards, and spin coating is covered in the upper and lower surface of electrode,
Solidify 10h in 80 DEG C of baking oven.After the completion of encapsulation, the sensitivity test of device is carried out.
Comparative example 2:
0.5g P (VDF-TrFE) powder is dissolved in 100mL DMF solvent first, then inserts clean sheet glass
Enter in above-mentioned P (VDF-TrFE) solution, after standing 3 minutes, drying is dried again after sheet glass is inserted into P (VDF-TrFE) solution
Process and so on 150 times, formed flexible piezoelectric film.
By magnetron sputtering, gold electrode is uniformly plated in piezoelectric membrane upper and lower surface, and in upper and lower surface extraction wire.So
Dimethyl silicone polymer is mixed with curing agent with weight ratio 10:1 afterwards, and spin coating is covered in the upper and lower surface of electrode,
Solidify 10h in 80 DEG C of baking oven.After the completion of encapsulation, the sensitivity test of device is carried out.
The sensitivity test result for the film that above-described embodiment and comparative example are prepared is as follows:
The sensitivity and electrical response of the different embodiment and comparative example samples of table 1.
The beneficial effects of the present invention are:
The flexible piezoelectric laminated film for the ordering hybrid that the LBL self-assembly method that the present invention uses is formed,
The functionalization film has the characteristics that the sensitivity of height, response time is short and stable structure, compared to traditional condenser type,
Resistance-type and organic crystal tubular type sensor, the functionalization film in the present invention have preparation method simple, and it is expensive, difficult to avoid
The use of the nano materials such as processing, complicated microarray, nano wire or nanometer rods.
Also, these nano materials with micro-nano structure in process there is inevitably be unevenly distributed and
The problems such as repeatability is low.And the piezoelectric material monocrystalline microplate to tile in the present invention is easy in polymer surfaces orientations, layer with
The structure of the hybrid between Mussel shell is similar between layer, this kind of structure can not only improve the stability of film, and
The piezoelectric material monocrystalline microplate of adjacent layer orientation can play complementation, so that functionalization film of the invention has high sensitivity
Degree.
On the other hand, which can be converted to electric signal for the vibration of the vocal cords muscle of human body, according to human body sound
Difference with pronunciation generates corresponding electric signal, and has repeatability and higher reliability, the language in artificial intelligence
Sound identifying system field has potential application.
In addition to this, which can also perceive the faint physiological signal of human body, for example, pulse, heartbeat and fortune
Emotionally condition can play an important role in field of biomedicine.
In conclusion the high susceptibility that functionalization film has prepared by the present invention, preparation method are simple and low
The advantages such as cost provide possibility for its practical application in wearable device and field of biomedicine.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by those familiar with the art, all answers
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be subject to the protection scope in claims.
Claims (10)
1. a kind of preparation method of the multifunction flexible Piezoelectric anisotropy film of ordered structure characterized by comprising
S1, polymer powder is dissolved in solvent, piezoelectric monocrystal microplate is distributed in solvent, polymer solution is respectively obtained
With piezoelectric monocrystal microplate dispersion liquid；
S2, it sheet glass is inserted into the polymer solution stands, then sheet glass is dried, glass sheet surface forms polymer and covers
Film；
S3, piezoelectric monocrystal microplate suspension is uniformly slowly dripped into glass sheet surface, makes piezoelectric monocrystal microplate in the polymerization
It is tiled and is orientated with the direction crystal face 00l, then the sheet glass is dried in object overlay film surface；
S4, circulation execute S2-S3, until the multifunction flexible Piezoelectric anisotropy that the glass sheet surface forms the ordered structure is thin
Film.
2. the preparation method of the multifunction flexible Piezoelectric anisotropy film of ordered structure according to claim 1, feature exist
In, further includes:
Gold electrode is plated by ion sputtering on the multifunction flexible Piezoelectric anisotropy film of the ordered structure, and upper and lower two
Face extraction wire；
Dimethyl silicone polymer is mixed with curing agent with weight ratio 10:1, and spin coating is covered in up and down the two of the electrode
Face, the baking and curing at 80 DEG C, the piezoelectric membrane being completed.
3. the preparation method of the multifunction flexible Piezoelectric anisotropy film of ordered structure according to claim 1, feature exist
In the polymer includes polyvinyl alcohol, Kynoar, Kynoar base co-polymer, polylactic acid, polydimethylsiloxanes
Alkane, polyurethane, polyacrylic resin, polyolefin.
4. the preparation method of the multifunction flexible Piezoelectric anisotropy film of ordered structure according to claim 1, feature exist
In the solvent includes water, N, one of N- dimethylene formamide, N-Methyl pyrrolidone solvent or a variety of.
5. the preparation method of the multifunction flexible Piezoelectric anisotropy film of ordered structure according to claim 1, feature exist
In the concentration of the polymer solution is 0.5 ~ 3 wt%.
6. the preparation method of the multifunction flexible Piezoelectric anisotropy film of ordered structure according to claim 1, feature exist
In the piezoelectric material monocrystalline microplate includes barium titanate single-crystal microplate, lead titanate monocrystal microplate, niobic magnesium acid lead-lead titanate single-crystal
Microplate, sodium niobate monocrystalline microplate, potassium-sodium niobate monocrystalline microplate, lithium niobate monocrystal microplate, monocrystalline lithium tantalate microplate, single crystal quartz are micro-
Piece.
7. the preparation method of the multifunction flexible Piezoelectric anisotropy film of ordered structure according to claim 1 or 6, feature
Be, the piezoelectric material monocrystalline microplate with a thickness of 1nm ~ 100nm, long and width is 1 μm ~ 10 μm.
8. the preparation method of the multifunction flexible Piezoelectric anisotropy film of ordered structure according to claim 1, feature exist
In the concentration of the piezoelectric monocrystal microplate dispersion liquid is 1 ~ 5 wt%.
9. the preparation method of the multifunction flexible Piezoelectric anisotropy film of ordered structure according to claim 2, feature exist
In the piezoelectric membrane being completed is with a thickness of 1-1000 μm.
10. a kind of multifunction flexible Piezoelectric anisotropy film of ordered structure, which is characterized in that be made by above-mentioned preparation method.
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| CN111416033A (en) * | 2020-03-17 | 2020-07-14 | 清华大学深圳国际研究生院 | Flexible piezoelectric composite material, flexible piezoelectric device and preparation method thereof |
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| CN113540340B (en) * | 2021-07-08 | 2023-08-01 | 东南大学 | Preparation method of flexible piezoelectric nano generator based on mesoporous silicon |
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| WO2020252833A1 (en) | 2020-12-24 |
| CN110350081B (en) | 2021-09-17 |
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