CN101914215B - Method for preparing high-active piezoelectric functional membranes by microwave irradiation - Google Patents
Method for preparing high-active piezoelectric functional membranes by microwave irradiation Download PDFInfo
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- CN101914215B CN101914215B CN2010101925783A CN201010192578A CN101914215B CN 101914215 B CN101914215 B CN 101914215B CN 2010101925783 A CN2010101925783 A CN 2010101925783A CN 201010192578 A CN201010192578 A CN 201010192578A CN 101914215 B CN101914215 B CN 101914215B
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Abstract
The invention discloses a method for preparing high-active piezoelectric functional membranes by microwave irradiation, and relates to a method for preparing high-active piezoelectric functional membranes. The method of the invention comprises the following steps of: soaking polypropylene porous membranes, or COC, PET, FEP, PEN and the like which are available in the market and serve as original membranes into methylenechloride solvent, trichloromethane solvent, acetone solvent, butanone solvent, ethanol solvent and the like which have no response to microwaves for 20 to 30 hours; then taking out from the solvent and irradiating under the microwaves, wherein the irradiation energy is 1.9*10-25-1.99*10-22J, and the irradiation time is 50 to 100 seconds; heating the solvent soaked in membrane pores by using the microwaves to rise the temperature of the solvent and then gasify the solvent in the pores under the action of thermalization so as to achieve the effect of puffing the pores; finally, cooling in ice water at the temperature of 0 zero to obtain the high-active piezoelectric functional membrane which has the pore volume 2 to 3 times that of the original membrane, the thickness improved by over 30 percent, and the density reduced by 10 to 20 percent. The method of the invention has the advantages of simple process, low production cost, low-cost and readily available equipment, and high safety; and the obtained high-active piezoelectric electret membranes are suitable to be used as flexible electromechanical conversion materials.
Description
Technical field
The method of preparing high-active piezoelectric functional membranes by microwave irradiation relates to a kind of making method of high-active piezoelectric functional membranes, specifically is to improve the active method of piezo-electric electret functional membrane by microwave exposure, belongs to the flexible piezoelectric technical field of function materials.
Technical background
With the non-polar polymer material is the microvoid structure film of external phase, by having outstanding piezoelectric effect and the ferroelectric hysteresis loop that is similar to ferroelectric material after the suitable electropolarization processing, being named as piezo-electric electret or ferroelectric eletrect, is the new class energy converting between mechanical material that recent two decades has just grown up.In fields such as sensing, detection, energy acquisition, military affairs and medical science very big application prospect is arranged.
According to theoretical model as can be known, characterize the piezoelectric coefficient d of the active size of piezo-electric electret
33Relevant with the electropolarization ability and the Young's modulus of microporous membrane: the electropolarization ability of film is strong more, and Young's modulus (Young's modulus) is low more, and the piezoelectric activity of acquisition is big more.In order to obtain to suppress electroactive piezo-electric electret film, the method that adopts is " a high pressure gas bulking process " usually.The concrete steps of high pressure gas bulking process are: at first microporous membrane material is placed autoclave, choose suitable gaseous species, set appropriate temperature and gas pressure intensity, allow microporous membrane under the above-mentioned parameter condition, place several hours then, at last when the air pressure of air pressure in the internal capillary of microporous membrane and autoclave setting reaches balance, gas in the extremely short time in the release autoclave is to ambient pressure, since the inner and outer air pressure difference of microporous membrane a pressure difference, so cause the deformation of the inner hole of microporous membrane, thereby optimized the electropolarization performance and the elastic property of microporous membrane, obtained to suppress electrically active films.But the high pressure gas expansion method needs the equipment-autoclave of special higher cost, simultaneously since multiple factor (for example temperature, air pressure, gaseous species etc.) all the modification result to microporous membrane exert an influence, so it is cumbersome to reach the purpose of the electropolarization performance of optimizing microporous membrane and elastic property, technology is difficult to control.
Summary of the invention
The objective of the invention is to disclose a kind of preparation method who suppresses electroactive piezoelectric functional film.Simple and easy to do with method technology of the present invention, facility investment and cost of manufacture are low, safety, and the piezoelectric activity of the porous polymer piezo functional membrane that obtains is big.
In order to achieve the above object, the present invention adopts the method for microwave exposure, at first selecting former film is that commercially available model is the polypropylene porous film of PQ50, or COC (cyclic olefine copolymer), PET (polyethylene terephthalate), FEP (fluorinated ethylene propylene copolymer), PEN (PEN), select that microwave is had the solvent of response is methylene dichloride, trichloromethane, acetone, butanone, ethanol etc. for use, former film is soaked in the solvent, soak time is 20-30h, take out former film from solvent, being placed on irradiation energy is 1.99 * 10
-25～1.99 * 10
-22Irradiation under the J microwave, irradiation time is 50s-100s, immerse solvent in the former fenestra hole by microwave heating, make the temperature of solvent rise, solvent in the hole is heated and flashes to gas, reaches the effect of expanded hole, irradiated former film is placed in 0 ℃ of frozen water or the liquid nitrogen cools off immediately, obtain having the porous-film of high electrode ability and low Young's modulus, and then handle acquisition by suitable electropolarization and suppress electroactive piezo-electric electret functional membrane.
Advantage of the present invention is:
1. because the present invention as long as former film is soaked in the solvent, place irradiation under the microwave then, so technology is simple, cost of manufacture is low.
2. than the high pressure gas bulking process, facility investment of the present invention is cheap to be easy to get.
3. finish under normal pressure owing to technology of the present invention, so security is good.
Description of drawings
Fig. 1 has just immersed the structural representation of the former film of solvent for the present invention.
Fig. 2 soaks the structural representation of former film completely for the present invention.
Fig. 3 has just carried out the structural representation of the former film of microwave exposure for the present invention.
Fig. 4 for microwave exposure of the present invention finish after the structural representation of the piezoelectric functional film that evaporated of solvent.
Fig. 5 is the cross section sem photograph of former film.
Fig. 6 is the cross section sem photograph of the piezoelectric functional film of the embodiment of the invention 1 preparation.
Fig. 7 is the cross section sem photograph of the piezoelectric functional film of the embodiment of the invention 2 preparations.
Fig. 8 is the cross section sem photograph of the piezoelectric functional film of the embodiment of the invention 3 preparations.
Fig. 9 is the cross section sem photograph of the piezoelectric functional film of the embodiment of the invention 4 preparations.
Figure 10 is the cross section sem photograph of the piezoelectric functional film of the embodiment of the invention 5 preparations.
Figure 11 is the piezoelectric functional film of five kinds of embodiment preparations of the present invention and the thickness comparison diagram of former film.
Figure 12 is the piezoelectric functional film of five kinds of embodiment preparations of the present invention and the density comparison diagram of former film.
Figure 13 is a penetron structural representation of the present invention.
1-container among the figure, 2-solvent, 3-film, 4-hole, 5-analytical balance, 6-measuring stand, 7-thin wire, 8-support, 9-tank, 10-V sections silk screen.
Embodiment
With commercially available model is that the polypropylene porous film (pp) of PQ50 cuts into 3cm * 3cm sample and is immersed in as former film commercial reagent level methylene dichloride (CH is housed
2Cl
2) in the container 1 of solvent, 20h is soaked in sealing, former film is made up of film 3 and hole 4, in the hole 4 fully immersion advanced behind the solvent, former film is taken out from solvent 2 puts into culture dish, placing irradiation energy is 1.99 * 10
-25～1.99 * 10
-22Irradiation 50-100s under the microwave of J, microwave heating is risen the temperature of solvent, and the solvent in the hole 4 is heated and flashes to gas, reaches the effect of expanded hole, irradiated former film is placed in 0 ℃ of frozen water cools off immediately, obtains the big piezoelectric functional film of piezoelectric activity.
Just immersed the volume (please see Figure 2) of volume (please see Figure 1) and the hole 4 that soaks 20h of hole 4 of former film of solvent and the volume (please see Figure 3) that just carries out the hole 4 of microwave exposure change little, but the hole after the microwave exposure solvent evaporation 4 has obviously become greatly than the raising of former film 2-3 doubly (please see Figure 4).
Is that 2000 cross section scanning electron microscope detects with obtaining the big piezoelectric functional film of piezoelectric activity by magnification, can see the hole 4 apparent in view increases of the former film of the volume of hole 4 and Fig. 5 (commercially available former film) as Fig. 6.
The present invention is obtained the big piezoelectric functional film sample of piezoelectric activity and former film, and (model: (unit: μ m) find: the thickness of former film is 50 μ m in the thickness contrast that 0-1x30) records through THICKNESS GAUGE FOR THE MEASUREMENT OF THIN FOILS, the sample thickness of embodiment 1 is 66.25 μ m (please see Figure 11), and thickness of the present invention increases by 32.5% than the thickness of former film.
The present invention is obtained the density contrast (unit: g/cm of big piezoelectric functional film sample of piezoelectric activity and former film
3) find: the density of former film is 0.5500g/cm
3, the density of the sample of embodiment 1 is 0.4968g/cm
3(please see Figure 12).
The result of thickness and density show through the sample structure of present embodiment preparation be improved significantly, the porous-film that obtains having high electrode ability and low Young's modulus, and then handle by suitable electropolarization and to obtain to suppress electroactive piezo-electric electret functional membrane.
Except reagent being changed into SILVER REAGENT trichloromethane (CHCl
3) solvent, sealing back soak time is that outer other technologies of 21h are identical with embodiment 1, promptly obtains the big piezoelectric functional film of piezoelectric activity.
By using the measuring method identical with embodiment 1, the volume change trend of cross section scanning electron microscope detection hole 4 is identical with embodiment 1.
The present invention is obtained the thickness contrast of big piezoelectric functional film sample of piezoelectric activity and former film, and (unit: μ m) find: the thickness of former film is 50 μ m, the sample thickness of embodiment 2 is 66.25 μ m (please see Figure 11), and thickness of the present invention increases by 32.5% than the thickness of former film.
The present invention is obtained the density contrast (unit: g/cm of big piezoelectric functional film sample of piezoelectric activity and former film
3) find: the density of former film is 0.5500g/cm
3, the density of the sample of embodiment 2 is 0.5168g/cm
3(please see Figure 12).
The result show through the sample structure of present embodiment preparation also be improved significantly.
Except reagent being changed into commercial reagent grade acetone (CH
3COCH
3) solvent, sealing back soak time is that outer other technologies of 23h are identical with embodiment 1.Promptly obtain the big piezoelectric functional film of piezoelectric activity.
By using the measuring method identical with embodiment 1, the volume change trend of cross section scanning electron microscope detection hole 4 is identical with embodiment 1.
(unit: μ m) find: the thickness of former film is 50 μ m, and the sample thickness of embodiment 3 is 65 μ m (please see Figure 11), and thickness of the present invention increases by 30% than the thickness of former film with the thickness contrast that obtains big piezoelectric functional film sample of piezoelectric activity and former film.
Density contrast (the unit: g/cm of big piezoelectric functional film sample of piezoelectric activity and former film will be obtained
3) find: the density of former film is 0.5500g/cm
3, the density of the sample of embodiment 3 is 0.4673g/cm
3(please see Figure 12).
The result show through the sample structure of present embodiment preparation also be improved significantly.
Except reagent being changed into commercial reagent level butanone (CH
3CH
2COCH
3) solvent, outer other technologies of sealing back immersion 24h are identical with embodiment 1.Promptly obtain the big piezoelectric functional film of piezoelectric activity.
By using the measuring method identical with embodiment 1, the volume change trend of cross section scanning electron microscope detection hole 4 is identical with embodiment 1.
(unit: μ m) find: the thickness of former film is 50 μ m, and the sample thickness of embodiment 4 is 68.5 μ m (please see Figure 11), and thickness of the present invention increases by 37% than the thickness of former film with the thickness contrast that obtains big piezoelectric functional film sample of piezoelectric activity and former film.
Density contrast (the unit: g/cm of big piezoelectric functional film sample of piezoelectric activity and former film will be obtained
3) find: the density of former film is 0.5500g/cm
3, the density of the sample of embodiment 4 is 0.4635g/cm
3(please see Figure 12).
The result show through the sample structure of present embodiment preparation also be improved significantly.
Except reagent being changed into commercial reagent level ethanol (C
2H
5OH) solvent, outer other technologies of sealing back immersion 30h are identical with embodiment 1.Promptly obtain the big piezoelectric functional film of piezoelectric activity.
By using the measuring method identical with embodiment 1, the volume change trend of cross section scanning electron microscope detection hole 4 is identical with embodiment 1.
(unit: μ m) find: the thickness of former film is 50 μ m, and the sample thickness of embodiment 5 is 65 μ m (please see Figure 11), and thickness of the present invention increases by 30% than the thickness of former film with the thickness contrast that obtains big piezoelectric functional film sample of piezoelectric activity and former film.
Density contrast (the unit: g/cm of big piezoelectric functional film sample of piezoelectric activity and former film will be obtained
3) find: the density of former film is 0.5500g/cm
3, the density of the sample of embodiment 5 is 0.4303g/cm
3(please see Figure 12).
The result show through the sample structure of present embodiment preparation also be improved significantly.
Above-mentioned density measuring equipment such as Figure 13 are made up of analytical balance 5, support 8, tank 9, v block silk screen 10, and v block silk screen 10 quality are greater than sample quality.With thin wire analytical balance 5 is connected with v block silk screen 10, v block silk screen 10 is vertically hung also be immersed in the water fully.Measuring process: the analytical balance zeroing, sample is put on the weighbridge 6, weighing sample quality m1 takes out sample.The analytical balance zeroing vertically is put in sample in the v block silk screen 10, and weighing is shown as-m
2Sample rate is
(ρ
Water=1.000g/cm
3).
The sample after process the inventive method is handled and the comparative result of former film: the cross section sem photograph contrast of the sample of five kinds of embodiment and former film, the volume change in various degree of the hole 4 of sample big (shown in Fig. 6-10).All proved the big conclusion of hole change from the density contrast (as shown in figure 12) of the sample of the thickness contrast (as shown in figure 11) of the sample of five kinds of embodiment and former film and five kinds of embodiment and former film.
Claims (1)
1. the method for preparing high-active piezoelectric functional membranes by microwave irradiation, it is characterized in that: commercially available polypropylene porous membrane is immersed in has in SILVER REAGENT methylene dichloride, trichloromethane, acetone, butanone or the alcohol solvent of response microwave earlier, soak time is 20h-30h, then taking out from solvent and placing irradiation under the microwave, irradiation energy is 1.99 * 10
-25～1.99 * 10
-22J, irradiation time is 50s-100s, solvent in the immersion fenestra hole is by microwave heating, the temperature of solvent is risen, and the solvent in the hole is heated and flashes to gas, reaches the effect of expanded hole, be placed on immediately at last in 0 ℃ of frozen water or the liquid nitrogen and cool off, promptly obtain the former film of hole volume ratio and increase 2-3 doubly, thickness increases more than 30% than former film, and density reduces the high-active piezoelectric functional membranes of 10%-20% than former film.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101925783A CN101914215B (en) | 2010-06-04 | 2010-06-04 | Method for preparing high-active piezoelectric functional membranes by microwave irradiation |
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|---|---|---|---|
| CN2010101925783A CN101914215B (en) | 2010-06-04 | 2010-06-04 | Method for preparing high-active piezoelectric functional membranes by microwave irradiation |
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| CN101914215B true CN101914215B (en) | 2011-12-07 |
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| CN104339673B (en) * | 2014-08-06 | 2016-10-05 | 贝骨新材料科技（上海）有限公司 | For increasing the method for microporous polypropylene film thickness, equipment |
| CN112480832B (en) * | 2020-12-04 | 2022-09-30 | 无锡市立帆绝缘材料科技有限公司 | Preparation method of high-voltage-resistance insulating polyester composite film |
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| WO2005069858A2 (en) * | 2004-01-16 | 2005-08-04 | Northern Illinois University | Nano-composite piezoelectric material |
| CN100435371C (en) * | 2006-03-23 | 2008-11-19 | 同济大学 | Method for preparing porous polymer piezo-electric electret thin film |
| CN100505359C (en) * | 2006-10-12 | 2009-06-24 | 同济大学 | Method for producing controllable microhole structural piezoelectric functional film |
| CN101280065B (en) * | 2008-05-29 | 2011-06-29 | 复旦大学 | Polymer film having micropore structure, preparation and application thereof |
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