CN104201280B - A kind of nanometer piezoelectric membrane and the preparation method of nano combined piezoelectric generator - Google Patents
A kind of nanometer piezoelectric membrane and the preparation method of nano combined piezoelectric generator Download PDFInfo
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- CN104201280B CN104201280B CN201410379806.6A CN201410379806A CN104201280B CN 104201280 B CN104201280 B CN 104201280B CN 201410379806 A CN201410379806 A CN 201410379806A CN 104201280 B CN104201280 B CN 104201280B
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Abstract
A kind of nanometer piezoelectric membrane and the preparation method of nano combined piezoelectric generator.It is characterized in that, use and there is the Bacterial cellulose of biocompatibility as matrix, having nanometer (or submicron) the piezoelectricity granule of high tension electricity coefficient as packing material, both are combined the thin film obtaining having piezoelectric properties, and are used for building flexible nano composite piezoelectric electromotor.The space three-dimensional network structure of Bacterial cellulose uniqueness can make piezoelectricity granule naturally be uniformly distributed wherein, and makes to be more uniformly stressed inside thin film, it is possible to nano combined piezoelectric generator output performance is greatly improved.This nano combined piezoelectric generator has biocompatibility, carries out energy acquisition, and preparation technology is simple, with low cost, has good application prospect in can implanting organism.
Description
Technical field
The present invention relates to nanometer piezoelectric membrane and the preparation method of nano generator of a kind of Bacterial cellulose and piezoelectricity Particles dispersed,
Have wide practical use in the field such as medical material, electronic material.
Background technology
Energy problem becomes to become increasingly conspicuous in human development, environmental pollution that traditional energy is brought and self reserves limited
Property forces people constantly to seek alternative new forms of energy.But, the energy contained in environment is ubiquitous, such as, vibrate, rub
The mechanical energy such as wiping and discarded heat energy etc., if these collection of energy are got up by certain changing the mechanism and are used,
Total amount is by considerable.In recent years, portable type electronic product popularize as driving the power supply of these electronic devices to propose higher
Requirement.Traditional electric power storage Technological expression goes out the deficiencies such as poor, the environmental pollution of persistency, develops a kind of environmental protection, sustainable independent confession
The technology of electricity becomes extremely urgent.Therefore, by effective means, the collection of energy in environment is got up, and be converted into continuable
Electric energy drives the electronic device of little scope, will be expected to become the excellent approach of solution the problems referred to above.
Nano generator is the energy conversion device developed rapidly in recent years, and they are imitated based on such as piezoelectric effect, franklinic electricity
Should, the different character such as pyroelectric effect, the energy originally may discarded in environment, such as mechanical energy, heat energy can be gathered.
Piezoelectric nano electromotor is the one in this kind of device, it make use of piezoelectric can produce when by stress polarization charge this
Fundamental property, can collect the mechanical energy in environment and convert it to electric energy.Nano generator the earliest is this based on ZnO
Deposition tube material, but its relatively low piezoelectric modulus limits the lifting of nano generator performance.Traditional piezoelectric ceramics is usual
There is higher piezoelectric modulus, but himself mostly is fragile material, complicated and diversified use environment can not be met.Nano combined
Piezoelectric generator can make up above-mentioned deficiency, and it uses the piezoelectric that piezoelectric modulus is higher to carry out being compounded to form receiving with organic matrix
Rice composite piezoelectric material, while realizing the flexibility of device, can significantly improve the performance of nano generator.Through finite element meter
Calculation and Analysis is known, the uniformity that piezoelectric nano-particles is distributed in organic matrix has a considerable influence to the piezoelectric property of composite piezoelectric thin films:
Particle distribution uniformity is the best, and the piezoelectricity Potential Distributing that electromotor produces under by stress condition is the most uniform, and then electromotor
Performance is the best.(the Park K I, Lee M, Liu Y, et al.Flexible nanocomposite generator made of such as K.Park
BaTiO3 nanoparticles and graphitic carbons.Advanced Materials, 2012,24 (22): 2999-3004.) pass through
To BaTiO3/ PDMS piezoelectric membrane introduces multi-walled carbon nano-tubes, makes BaTiO3Granule disperses more equal in PDMS matrix
Even, CNT being interspersed in PDMS makes the stress distribution within laminated film evenly simultaneously, enhances BaTiO3
Granule stress in the base, so that the output voltage of nano generator is obviously improved.But add and too much there is electric conductivity
CNT piezoelectricity electromotive force can be produced shielding action, thus the performance of nano generator is caused weakening.
Bacterial cellulose be a class by the cellulose of Microbe synthesis, the most most typically acetobacter xylinum.Bacterial cellulose is compared
Have the advantage that (1) purity is high in other native celluloses, without the lignin often having in plant cellulose, pectin and half
Cellulose etc.；(2) stable three-dimensional manometer fiber mesh structure；(3) mechanical strength is high, and it is fine that elastic modelling quantity can reach plant
Dimension element more than ten times, and tensile strength is high；(3) higher biocompatibility and good biodegradability.As one
Environmental friendliness, the material of rich content, Bacterial cellulose has wide practical use in the field such as medical material, electronic material.
Summary of the invention
The present invention proposes a kind of based on Bacterial cellulose and the nano combined piezoelectric membrane of piezoelectricity granule and nano combined piezo-electric generating
The preparation method of machine.
It is a kind of based on Bacterial cellulose with the preparation method of the nano combined piezoelectric membrane of piezoelectricity granule, it is characterised in that: to have
Biocompatibility, Bacterial cellulose with low cost are as matrix, to have nanometer (or submicron) the granule work of piezoelectric properties
For packing material, both are combined the thin film obtaining having piezoelectric properties.The method specifically comprises the following steps that
(1) use physical mechanical method or chemolysis method that Bacterial cellulose is dispersed into fiber fines in the liquid phase.Physical machine
Tool method includes, but is not limited to high speed dispersor dispersion, cell disruptor pulverizing, drying and grinding, ultrasonic disperse etc.；
The solvent that chemolysis method is used includes, but is not limited to trifluoroacetic acid etc..Above method all can make bacterial fibers
Element is scattered in liquid phase, forms semigel or the Bacterial cellulose slurry of solution state.
(2) nanometer (or submicron) granule with piezoelectric properties is added in Bacterial cellulose slurry, and be sufficiently mixed,
To mixed slurry.Every 40ml density is the Bacterial cellulose slurry piezoelectricity granule with 0.001-0.01mol of 0.9675g/ml
Mixing；Mixed method is: be first scattered in ethanol by piezoelectricity granule, then this alcohol dispersion liquid and Bacterial cellulose slurry
It is sufficiently mixed, obtains uniform mixed slurry.Nanometer (or submicron) granular materials with piezoelectric properties include (but
It is not limited to) lead titanate-zirconate, Barium metatitanate., lead magnesio-niobate, sodium niobate, potassium niobate, Lithium metaniobate etc..First piezoelectricity granule is divided
Dissipate in liquid phase, ultrasonic vibration 10～30min；Again it is mixed with Bacterial cellulose slurry, be sufficiently stirred for rear ultrasonic vibration
30～60min, obtain uniform mixed slurry.
(3) utilize physical method or chemical method that above-mentioned mixed slurry is processed.Physical method includes, but is not limited to right
Mixed slurry carries out vacuum filtration, solvent evaporation etc., and chemical method includes, but is not limited to add sea in mixed slurry
Sodium alginate and calcium chloride, form gel network by ionomer.Above method all can make nanofiber again be cross-linked into net
Network structure, and make piezoelectricity granule be uniformly distributed therein, obtain the nano combined piezoelectric membrane of hygrometric state.
(4) piezoelectric membrane nano combined to above-mentioned hygrometric state is dried.By hygrometric state film-clamp at the steel plate of two panels flat smooth or poly-
Between tetrafluoroethene plate, and mechanical compression (1MPa～10MPa) under vacuum (< 100Pa) state, at 70 DEG C
It is dried 24 hours, obtains the nano combined piezoelectric membrane of dried flat and flexibility.Photo in kind and scanning electron microscope (SEM) photograph such as Fig. 1
Shown in.
(5) piezoelectric membrane nano combined to dry state carries out high voltage polarization, makes the electric domain orientation in piezoelectricity granule consistent, can obtain
There is the thin film of orientation piezoelectric properties.
A kind of based on Bacterial cellulose with the preparation method of the nano combined piezoelectric generator of piezoelectricity granule.It is characterized in that: its knot
Structure is to be respectively upper electrode layer, nano combined piezoelectric layer, lower electrode layer from top to bottom.Described upper and lower electrode layer is with necessarily
The substrate of the conductive layer of thickness (10～100nm), nano combined piezoelectric layer is based on Bacterial cellulose and the nanometer of piezoelectricity granule
Composite piezoelectric thin films.The construction method of nano generator is as follows:
(1) prepared by electrode.Directly conductive layer can be prepared the upper and lower surface at nano combined piezoelectric membrane, conductive layer can be
(but not limited to): the metals such as platinum, gold, silver, copper, aluminum, or the transparent conductive oxide such as tin indium oxide, Fluorin doped stannum stannum oxide
Or the material with carbon element such as CNT, Graphene, graphite, preparation method includes, but is not limited to: magnetron sputtering, evaporation, atomic layer
Deposition etc..First with same method, conductive layer can also be prepared on substrate, then it is multiple that the substrate with conductive layer is fixed on nanometer
The upper and lower surface of combined pressure conductive film, substrate material includes, but is not limited to: polyethylene terephthalate, poly-naphthalenedicarboxylic acid second
Diol ester, polyimides, polymethyl methacrylate, polydimethylsiloxane, glass etc..
(2) polarization.The purpose of polarization is along direction of an electric field proper alignment by the electricdomain in piezoelectricity granule, makes nano combined piezoelectricity send out
The output that motor obtains reaches optimum performance.Polarization mode is: at 25 to 200 DEG C, according to the thickness of piezoelectric membrane, by upper
Bottom electrode applies the voltage that 50-300kV/cm does not waits, and keeps 24 hours, last cooling with pressure.Temperature needed for polarization, electricity
Pressure, time depend on the thickness of nano combined piezoelectric layer and the kind of piezoelectric.
The invention have the advantages that: the piezoelectricity granule of nanometer (or submicron) yardstick can be evenly distributed to the thin of flexibility easily
In fungin matrix, take full advantage of the high tension electricity coefficient of conventional piezoelectric pottery and the mechanical performance that Bacterial cellulose is good；Carefully
The three-dimensional net structure that nanofiber in fungin is constituted makes piezoelectricity distribution of particles and stress the most uniform, can effectively carry
The piezoelectric property of high-tension electricity thin film；The nano generator output performance built based on this kind of piezoelectric membrane is excellent, and has biology
The compatibility, carries out energy acquisition in can implanting organism；Preparation technology is simple, with low cost, has good application prospect.
Accompanying drawing explanation
Fig. 1 nano combined piezoelectric membrane scanning electron microscope (SEM) photograph.
Detailed description of the invention
Below in conjunction with example, technical scheme is described in detail.Obviously, described example is only schematically,
The full content of the present invention can not be comprised.Those skilled in the art are changed the every other reality obtained under the inspiration of the present invention
Example, broadly falls into the scope of protection of the invention.
Embodiment 1:
(1) bacteria cellulose film through purification process is cut into small pieces soak in deionized water, carries out point with high speed dispersor
Dissipate, obtain the Bacterial cellulose slurry of semigel state.Measuring its density is 0.9675gcm3。
(2) weigh 0.3g barium titanate nano granule (diameter about 100nm) to be dispersed in 20ml deionized water, ultrasonic vibration
20min, obtains uniform Barium metatitanate. suspension.
(3) Bacterial cellulose slurry 40ml prepared in step (1) is measured, with the Barium metatitanate. suspension in step (2)
Mixing, is sufficiently stirred for and ultrasonic vibration 30min, obtains uniform mixed slurry.
(4) sucking filtration is carried out in pouring the mixed slurry in step (3) into Suction filtration device, can shape on filter membrane after liquid filters
Become the thin film of one layer of hygrometric state.
(5) by hygrometric state film-clamp between two pieces of polytetrafluoroethylenes, it is placed in vacuum tank and applies the vertical pressure of 10MPa
Power, is dried 24 hours at 70 DEG C, i.e. obtains Bacterial cellulose and the laminated film of barium titanate nano granule.
(6) Kapton of 125 μ m-thick is cut into 1.5cm × 1cm, by Bacterial cellulose and barium titanate nano granule
Laminated film be cut into 1cm × 1cm.
(7) one layer of gold of magnetron sputtering (Au, thickness 100nm) on polyimides (PI) thin film, and use high speed sol evenning machine
Spin coating PDMS (4000rpm × 20s) on Au layer, heats 3min, at PDMS not yet immediately on the hot plate of 80 DEG C
When being fully cured, the laminated film of the Bacterial cellulose in step (7) and barium titanate nano granule is spread over above, double-layer films
Must be in close contact and not interspace.Heating is continued, until PDMS is fully cured with hot plate.By identical method at laminated film
Another side fix Au electrode, and each draw wire by two electrodes.
(8) connect high voltage power supply by wire, use 100kVcm-1Voltage polarize in the silicone oil of 130 DEG C 24h, its
In last 2 hours be temperature-fall period with pressure.
Embodiment 2:
(1) bacteria cellulose film through purification process is cut into small pieces soak in deionized water, carries out point with high speed dispersor
Dissipate, obtain the Bacterial cellulose slurry of semigel state.Measuring its density is 0.9675gcm3。
(2) weigh 0.2g sodium niobate nano granule (diameter about 1 μm) to be dispersed in 20ml deionized water, ultrasonic vibration 20
Min, obtains uniform sodium niobate suspension.
(3) Bacterial cellulose slurry 40ml prepared in step (1) is measured, with the sodium niobate suspension in step (2)
Mixing, is sufficiently stirred for and ultrasonic vibration 30min, obtains uniform mixed slurry.
(4) sucking filtration is carried out in pouring the mixed slurry in step (3) into Suction filtration device, can shape on filter membrane after liquid filters
Become the thin film of one layer of hygrometric state.
(5) by hygrometric state film-clamp between two pieces of polytetrafluoroethylenes, it is placed in vacuum tank and applies the vertical pressure of 10MPa
Power, is dried 24h at 70 DEG C, i.e. obtains Bacterial cellulose and the laminated film of sodium niobate nano granule.
(6) polyethylene terephthalate (PET) thin film being coated with ITO conductive layer of 100 μ m-thick is cut into
1.5cm × 1cm, is cut into 1cm × 1cm by the laminated film of Bacterial cellulose and sodium niobate nano granule.
(7) high speed sol evenning machine is used to be coated with one side spin coating PDMS (4000rpm × 20s) of ITO conductive layer in PET film,
On the hot plate of 80 DEG C, heat 3min immediately, when PDMS is not yet fully cured the Bacterial cellulose in step (7) and
The laminated film of sodium niobate nano granule spreads over above, and double-layer films must be in close contact and not interspace.Heating is continued with hot plate,
Until PDMS is fully cured.Fix gold electrode by identical method at the another side of laminated film, and pass through two electrodes each
Draw wire.
(8) connect high voltage power supply by wire, use 80kVcm-1Voltage at room temperature polarize 24h.
Embodiment 3:
(1) bacteria cellulose film through purification process is cut into small pieces soak in deionized water, carries out point with high speed dispersor
Dissipate, obtain the Bacterial cellulose slurry of semigel state.Measuring its density is 0.9675gcm3。
(2) weigh 0.1g barium titanate nano granule (diameter about 100nm) to be dispersed in 20ml deionized water, ultrasonic vibration
20min, obtains uniform Barium metatitanate. suspension.
(3) Bacterial cellulose slurry 20ml prepared in step (1) is measured, with the Barium metatitanate. suspension in step (2)
Mixing, is sufficiently stirred for and ultrasonic vibration 30min, obtains uniform mixed slurry.
(4) sucking filtration is carried out in pouring the mixed slurry in step (3) into Suction filtration device, can shape on filter membrane after liquid filters
Become the thin film of one layer of hygrometric state.
(5) by hygrometric state film-clamp between two pieces of polytetrafluoroethylenes, it is placed in vacuum tank and applies the vertical pressure of 10MPa
Power, is dried 24 hours at 70 DEG C, i.e. obtains Bacterial cellulose and the laminated film of barium titanate nano granule.
(6) use high speed sol evenning machine is on nanometer Piezoelectric anisotropy thin film two sides difference spin coating PDMS (4000rpm × 20s), and makes
It is fully cured at 80 DEG C.
(7) on the PDMS layer of two sides, deposit one layer of gold (Au, thickness 100nm) respectively by electron beam evaporation plating, and pass through
Two electrodes each draw wire.
(8) connect high voltage power supply by wire, use the voltage of 100kVcm-1 to polarize in the silicone oil of 130 DEG C 24h, its
In last 2 hours be temperature-fall period with pressure.
Claims (9)
1. the preparation method of a nanometer piezoelectric membrane, it is characterised in that: to have biofacies
Capacitive, Bacterial cellulose with low cost are as matrix, to have nanometer or the Asia of piezoelectric properties
Micron particle is as packing material, and both are combined the thin film obtaining having piezoelectric properties；Specifically
Step is as follows:
(1) first use physical mechanical method or chemolysis method by Bacterial cellulose in liquid phase
In be dispersed into fiber fines, it is thus achieved that Bacterial cellulose slurry；
(2) nanometer or submicron particles with piezoelectric properties are added Bacterial cellulose slurry
In, and be sufficiently mixed, obtain mixed slurry；There is nanometer or the submicron of piezoelectric properties
Grain material includes lead titanate-zirconate, Barium metatitanate., lead magnesio-niobate, sodium niobate, potassium niobate, Lithium metaniobate；
(3) utilize physical method or chemical method that mixed slurry is processed, make Nanowire
Dimension is cross-linked into network structure again, and makes piezoelectricity granule be uniformly distributed therein, and obtains hygrometric state and receives
Rice composite piezoelectric thin films；
(4) piezoelectric membrane nano combined to above-mentioned hygrometric state is dried, and obtains dry state nanometer multiple
Combined pressure conductive film；
(5) piezoelectric membrane nano combined to dry state carries out high voltage polarization, makes in piezoelectricity granule
Electric domain orientation is consistent, obtains the thin film with orientation piezoelectric properties；
Described physical method includes mixed slurry carries out vacuum filtration, solvent evaporation；Describedization
Method includes adding sodium alginate and calcium chloride in mixed slurry, is formed by ionomer
Gel network.
2. the preparation method of nanometer piezoelectric membrane as claimed in claim 1, its feature exists
In: the physical mechanical method described in step (1) refers to natural bacteria fiber by external force
Element film is broken up and is become scattered fiber or fibre bundle；Described chemolysis method is at chemistry
Fiber is made to scatter under the effect of solvent；Physical mechanical and chemolysis method purpose are to make carefully
Fungin is dispersed in liquid phase, forms the Bacterial cellulose slurry of semigel or solution state
Material.
3. the preparation method of nanometer piezoelectric membrane as described in claim 1, its feature exists
In: the nanometer with piezoelectric properties or submicron particles described in step (2) have simultaneously
Piezoelectricity and ferroelectricity, applying voltage can polarize.
4. the preparation method of nanometer piezoelectric membrane as claimed in claim 1, its feature exists
In: every 40ml density is the Bacterial cellulose slurry 0.001-0.01mol of 0.9675g/ml
Piezoelectricity granule mixing；Mixed method is: be first scattered in ethanol by piezoelectricity granule, then
This alcohol dispersion liquid is sufficiently mixed with Bacterial cellulose slurry, obtains uniform mixed slurry.
5. the preparation method of nanometer piezoelectric membrane as claimed in claim 1, its feature exists
In: the physical method described in step (3) refers to remove the liquid component in mixed slurry,
Make nanofiber dehydration and be naturally reunited under hydrogen bond action；Described change
Method refers to be recombined by interpolation cross-linking agent aided nano fiber；Above method
Obtain Bacterial cellulose and hygrometric state thin film that piezoelectricity granule is uniformly combined.
6. the preparation method of nanometer piezoelectric membrane as claimed in claim 1, its feature exists
In: the piezoelectric membrane nano combined to above-mentioned hygrometric state described in step (4) be dried be by
Hygrometric state film-clamp is between the steel plate or polyfluortetraethylene plate of two panels flat smooth, and at vacuum shape
Mechanical compression under state, is dried at 60-90 DEG C, finally gives dried flat and have flexibility
Nano combined piezoelectric membrane, vacuum < 100Pa, mechanical compression pressure 1MPa～10
MPa。
7. the nanometer piezoelectric membrane that a kind uses described in claim 1-6 is prepared nano combined
The method of piezoelectric generator；It is characterized in that: the structure of nano combined piezoelectric generator for from
Top to bottm it is respectively upper electrode layer, nano combined piezoelectric layer, lower electrode layer；Described upper and lower
Electrode layer is the substrate with thickness 10～100nm conductive layer, and nano combined piezoelectric layer is thin
Fungin and the nano combined piezoelectric membrane of piezoelectricity granule.
8. the method preparing nano combined piezoelectric generator as claimed in claim 7, its
It is characterised by: the preparation of upper and lower electrode layer is directly conductive layer to be prepared in nano combined pressure
The upper and lower surface of conductive film, or conductive layer is prepared on substrate, then with conductive layer
Substrate is fixed on the upper and lower surface of nano combined piezoelectric membrane.
9. the method preparing nano combined piezoelectric generator as claimed in claim 8, its
It is characterised by: described nano combined piezoelectric generator needs to reach optimum performance by polarization,
Polarization mode is: at 25 to 200 DEG C, according to the thickness of piezoelectric membrane, by up and down
Electrode applies the voltage that 50-300kV/cm does not waits, and keeps 24 hours, finally band pressure drop
Temperature.
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