CN102903842A - Polarization system and polarization method of cement-based piezoelectric ceramic composite material - Google Patents
Polarization system and polarization method of cement-based piezoelectric ceramic composite material Download PDFInfo
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Abstract
The invention discloses a polarization system and a polarization method of a cement-based piezoelectric ceramic composite material. The polarization system comprises an adjustable high-voltage DC power supply, a voltmeter, a polarization clamp, a heating tank, and a heating device for heating the heating tank, wherein the wiring terminal of the polarization clamp is connected with the output end of the high-voltage DC power supply; the voltmeter is connected with the wiring terminal of the polarization clamp in parallel; and the polarization clamp is soaked in the heating oil in the heating tank. The system and the method provided by the invention effectively overcome the disadvantages of the conventional polarization method, and can ensure the polarization success rate of the cement-based piezoelectric ceramic composite material as well as the long-term stability of the dielectric and piezoelectric properties of the polarized material.
Description
[technical field]
The present invention relates to the piezoelectric ceramic polarization, relate in particular to a kind of polar system and polarization method of cement base piezoelectric ceramic composite.
[background technology]
The cement base piezoelectric ceramic composite is a kind of novel functional material, and it can be used as piezoelectric transducer, realizes the function of the long-term Real-Time Monitoring of xoncrete structure mechanical property; And this composite material physical/chemical stability that the own water cement-based material is good simultaneously and the outstanding piezoelectric property of piezoelectric ceramic, can effectively solve the consistency problem between traditional intelligence material and the concrete precursor structure material.The cement base piezoelectric ceramic composite not only has perceptional function, and has the driving function; Its preparation technology is simple, and cost is low, is very suitable for the development need of intellectual material in the field of civil engineering.
As a kind of novel piezo-electricity composite material, in order to guarantee the performance of its piezoelectric property, must polarize to piezoelectric.Polarization is basic worker's process of giving the piezoelectric piezoelectric property, and common polarization method comprises and electrically contacts polarization, corona discharge polarization etc.
Electrically contact the polarization be directly to lay metal electrode at polarized material surface, apply direct current or alternative cycle voltage (such as the polarization to the PVDF piezoelectric membrane, such as patent of invention 200310114673.1 description); The corona discharge polarization is a kind of noncontact polarization method, apply high voltage at the relative needle electrode of two rows, form corona ring, polarize to being in film between two row's needle electrodes (such as the polarization to piezoceramic material, such as patent of invention 01143504.6 description).
For the cement base piezoelectric ceramic composite, because the material surface evenness is lower, thickness thicker (0.7mm-32mm), porosity higher (being about 6.5%), water content is higher; In polarization process, also can exist cement matrix to the steric hindrance of piezoelectric ceramic; In common high-temperature gas, polarize, can cause again the temperature stress of cement-based material, thereby destroy the microstructure of composite material; This causes traditional electrically contact the methods such as polarization, corona discharge polarization and all can't effectively polarizing to the cement base piezoelectric ceramic composite.
Existing piezoelectric ceramic polarization method polarizes to the cement base piezoelectric ceramic composite and has following shortcoming:
For electrically contacting polarization, it need to directly lay metal electrode (metal plate electrode) at polarized material surface, applies direct current or alternative cycle voltage; This method is applicable to flexible material, such as the PVDF material; But for the cement base piezoelectric ceramic composite, because surface smoothness is lower; Lay the metal plate electrode at composite material surface, be difficult to the comprehensive engagement between assurance composite material and the metal plate electrode, form easily the microcirculation circuit, affect degree of polarization and uniformity; And the porosity of composite material higher (being about 6.5%), water content is higher, and this also causes the voltage at polarized material two ends not apply, thereby perhaps can't effectively polarize.
For the corona discharge polarization, it is a kind of noncontact polarization method, applies high voltage at the relative needle electrode of two rows, forms corona ring, and the film that is between two row's needle electrodes is polarized; But for the cement base piezoelectric ceramic composite, because thickness is thicker, cement matrix is to the existence of the steric hindrance of piezoelectric ceramic simultaneously, and this causes high-tension electricity halo have no idea effectively the to overturn electricdomain of piezoelectric ceramic; Thereby can't effectively polarize.
For polarization in traditional high-temperature gas, owing to the existence of cement-based material temperature stress, can destroy the microstructure of composite material.
So traditional polarization method all has no idea to realize effective polarization of cement base piezoelectric ceramic composite.
[summary of the invention]
The technical problem to be solved in the present invention provides a kind of polar system that can realize that the cement base piezoelectric ceramic composite effectively polarizes.
The technical problem to be solved in the present invention provides a kind of polarization method that can realize that the cement base piezoelectric ceramic composite effectively polarizes.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is, a kind of polar system of cement base piezoelectric ceramic composite, comprise adjustable high-voltage DC power supply, voltmeter, polarization anchor clamps, heating tank and the heater that heating tank is heated, the terminals of polarization anchor clamps are connected with the output of high-voltage DC power supply, voltmeter also connects with the terminals of polarization anchor clamps, and described polarization anchor clamps are immersed in the heating oil in the heating tank.
The polar system of above-described cement base piezoelectric ceramic composite comprises current-limiting resistance, and described current-limiting resistance is serially connected between high-voltage DC power supply and the polarization anchor clamps; Described heating tank is glassware, and described heater is the digital display type heater, and glassware places on the digital display type heater; Described heating oil is silicone oil, and described voltmeter is digital display type high-voltage dc voltage table.
The polar system of above-described cement base piezoelectric ceramic composite, described polarization anchor clamps comprise frame and two thimbles of high-temperature resistance plastice, described frame comprise base and with two blocks of side plates of base one, described thimble is installed on the side plate, thimble comprises conical needle point, and the needle point of two thimbles is relative; Have at least one to be movable thimble in two thimbles, movable thimble by tailstock barrel and spring fitting on side plate; Described tailstock barrel is fixed in the thimble trepanning of side plate, and movable thimble passes tailstock barrel, and the shank of movable thimble and the endoporus of tailstock barrel are slidingly matched; The rear end of movable thimble needle point comprises spring fastening, and described spring housing is on shank, and an end of spring is against on the spring fastening, the other end be against on the side plate or the end face of tailstock barrel on.
The polar system of above-described cement base piezoelectric ceramic composite, the cone angle of needle point are 25-35 °; The material of frame is polyimides, polysulfones, polyphenylene sulfide, polyether-ether-ketone or polyether sulfone; The material of tailstock barrel is stainless steel.
The polar system of above-described cement base piezoelectric ceramic composite, described current-limiting resistance are bar-shaped glass glaze film resistance, resistance value 80-120 megaohm.
A kind of cement base piezoelectric ceramic composite polarization method based on said system, the relative dielectric constant of cement base piezoelectric composite material is 100-800, thickness 0.7mm-32mm; The polarization temperature is at 90-160 ° of C, polarizing voltage 1KV-15KV; Polarization time-20min-140min.
The above cement base piezoelectric ceramic composite polarization method, the cement base piezoelectric ceramic composite is heated to the stage of polarization temperature for preheating the stage from room temperature, pre-warmed programming rate be 2-4 ° C/ minute, when being warmed up to 87-93 ° of C, be stabilized in this temperature range, remove the moisture in the cement base piezoelectric ceramic composite hole; Cement base piezoelectric ceramic composite surface is warming up to the polarization temperature after no longer including Bubble formation again.
The above cement base piezoelectric ceramic composite polarization method, cement base piezoelectric ceramic composite are opened the adjustable high-voltage DC power supply after reaching the polarization temperature, regulate electric current to the 0.8-1.2 milliampere; After current stabilization, slowly improve voltage to the voltage that polarizes with 80-120V/ minute speed.
The above cement base piezoelectric ceramic composite polarization method, in slowly putting forward high-tension process, greater than 100V, the voltage of then keeping this moment is constant such as the reading fluctuating range of voltmeter, until the reading fluctuation less than behind the 10V, continues to improve voltage.
The above cement base piezoelectric ceramic composite polarization method, in polarization process, the reading of voltmeter slowly reduced with 10V/ minute, showed that polarization process finishes; After confirming that polarization process is finished, progressively reduce the voltage that applies, until voltage is zero.
The present invention is directed to the cement base piezoelectric ceramic composite, designed new type high temperature polar system and method, efficiently solve the drawback of conventional polar method, guaranteed the dielectric property that is polarized to power and polarized material of cement base piezoelectric ceramic composite and the long-time stability of piezoelectric property.
[description of drawings]
The present invention is further detailed explanation below in conjunction with the drawings and specific embodiments.
Fig. 1 is embodiment of the invention cement base piezoelectric ceramic composite polar system structural representation.
Fig. 2 is embodiment of the invention cement base piezoelectric ceramic composite polar system polarization anchor clamps schematic diagrames.
Fig. 3 is the variation diagram of polarization method cement base piezoelectric ceramic composite electromechanical coupling factor of the present invention with the polarization time.
Fig. 4 is that polarization method cement base piezoelectric ceramic composite electromechanical coupling factor of the present invention is with the variation diagram of polarization temperature.
Fig. 5 is that polarization method cement base piezoelectric ceramic composite electromechanical coupling factor of the present invention is with the variation diagram of polarization sample thickness.
Fig. 6 is the flow chart of polarization method cement base piezoelectric ceramic composite polarization method of the present invention.
[embodiment]
In Fig. 1, embodiment of the invention cement base piezoelectric ceramic composite polar system shown in Figure 2, comprise with lower device:
1: adjustable high-voltage DC power supply (High Voltage Regulated DC Power Supply, model: ES30): GAMMA High Voltage Research Inc, USA.
The current-limiting resistance of 2:100M Ω (the bar-shaped glass glaze film resistance of high pressure, model: RI80 series): moral bonding electron Industries, Inc, Taiwan.
3: digital display type high-voltage dc voltage table (High Voltage Digital Voltmeter, model: 4600): Valhalla Scientfic Inc, USA.
4: the pyroceram vessel: hold silicone oil, can be used to place the polarization anchor clamps
5: polarization anchor clamps (seeing accompanying drawing 2):
5-1 stainless steel thimble: two thimbles all are movable thimbles, and movable thimble 5-1 is installed on the side plate 5-2 by stainless steel sleeve pipe 5-7 and spring 5-6; The front end of two thimble 5-1 is conical needle point, and the needle point of two thimbles is relative.The endoporus of the shank of movable thimble 5-1 and tailstock barrel 5-7 is slidingly matched; There is spring fastening the rear end of movable thimble 5-1 needle point, and spring housing 5-6 is on the shank of movable thimble 5-1, and the end of spring 5-6 supports on the spring fastening of rear end of needle point, and the other end is against on the end face of the upper or tailstock barrel 5-7 of side plate 5-2.
The cone angle of conical needle point is 30 °, and (30 ° cone angle can guarantee that anchor clamps fixedly reach optimum efficiency to sample.
5-2 heat-resistant polymer side plate: can select the materials (but being not limited to above-mentioned listed material) such as polyimides (PI), polysulfones (PSF), polyphenylene sulfide (PPS), polyether-ether-ketone (PEEK) and polyether sulfone (PES).
5-3 heat-resistant polymer base: can select the materials (but being not limited to above-mentioned listed material) such as polyimides (PI), polysulfones (PSF), polyphenylene sulfide (PPS), polyether-ether-ketone (PEEK) and polyether sulfone (PES).
5-4 fixed screw: be used for connecting lateral plate and base.
5-6 spring: can be used for the fixedly polarized material of different-thickness.
5-7 stainless steel top needle guard; Be fixed on the thimble trepanning of side plate, be used for the guiding of movable thimble 5-1.
Stainless steel sleeve pipe 5-7 is fixed in the 5-2 heat-resistant polymer side plate, guarantees not slide; Stainless steel movable thimble 5-1 is positioned among the stainless steel sleeve pipe 5-7, can be free to slide; 5-6 regulating spring one end bearing is on the end face of stainless steel sleeve pipe 5-7, and an other end bearing is on the spring base of stainless steel thimble 5-1; Utilize the elastic force of spring to guarantee that stainless steel thimble 5-1 is to the clamping force of cement base piezoelectric ceramic composite sample 7.
6: digital display type heater (Digital Hot Plate, model: PMC DataPlate 730 series): BARNSTEAD THERMOLYNE CORPORATION, USA.
7: cement base piezoelectric ceramic composite sample.
As shown in Figure 6, the polarization of cement base piezoelectric ceramic composite sample may further comprise the steps:
(1) according to the order of connection of accompanying drawing 1, with electric wire connect successively protective resistance 2, the polarization anchor clamps 5 of adjustable high-voltage DC power supply 1,100M Ω, polarization anchor clamps two ends digital display type high-voltage dc voltage in parallel table 3.Check whether the polarization circuit is complete, avoid occurring the phenomenon that opens circuit, opens circuit; Whether special survey adjustable high-voltage DC power supply 1 and digital display type high-voltage dc voltage table 3 be working properly.
(2) cement base piezoelectric ceramic composite sample 7 is fixed (thickness of material (sample 7) can change) by polarization anchor clamps 5 between 0.7mm-32mm; Anchor clamps 5 are placed in the pyroceram vessel 4 that fill silicone oil (select that the reason of silicone oil is that silicone oil has that the sticking coefficient of temperature is little, high-low temperature resistant, anti-oxidant, flash-point is high, volatility is little, good insulating, surface tension are little, to metal without characteristics such as burn into are nontoxic).
(3) glassware 4 is placed on the digital display type heater (6); Slowly heat (2 ° C-4 ° C/ minute) to 90 ° of C, stablize this temperature about 10 minutes, guarantee that the moisture in the cement base piezoelectric ceramic composite hole is thoroughly removed (generation of observable material surface bubble is not until there is Bubble formation); Be warming up to again polarization temperature (the polarization temperature is adjustable between 90 ° of C-160 ° C);
(4) open adjustable high-voltage DC power supply 1, regulate electric current (A) to 1 milliampere; After current stabilization, slowly apply polarizing voltage (100V/ minute), the reading of the explicit high-voltage dc voltage of observed number table 3 (if the reading fluctuating range is very large, as 100V, can keep first the polarizing voltage that this point applies, until the reading fluctuating range stable till); Be continuously applied polarizing voltage, until the reading of high-voltage dc voltage table 3 constant till (fluctuating range＜10V);
(5) stablize this polarizing voltage, observe the reading of high-voltage dc voltage table 3; Slowly diminish if there is reading, such as＜10V/ minute; Show that polarization process finishes;
(6) after the affirmation polarization process is finished, gradually reduce the polarizing voltage (voltage reduces speed＜200V/ minute) that applies, until voltage drops to zero; Close adjustable high-voltage DC power supply 1, close digital display type heater 6; By the time the silicone oil drop in temperature in the pyroceram vessel 4 takes out cement base piezoelectric ceramic composite sample 7 to room temperature; After blotting the remaining silicone oil of material surface with lens wiping paper, with electric property, the dielectric property of the accurate electric impedance analyzer test of HP4294A cement base piezoelectric ceramic composite material sample; Piezoelectric property with quasistatic d33 analyzer test cement base piezoelectric ceramic composite material.
The relative dielectric constant of employed cement base piezoelectric composite material is generally 100-800 in the polarization method that the present invention relates to, and piezoelectric coefficient d 33 is 5 * 10-12C/N-90 * 10-12C/N after the polarization, thickness 0.7mm-32mm.
The polarization method that the present invention relates to, generally between 90 ° of C-160 ° of C, the polarizing voltage that applies is relevant with the thickness of polarized material, is generally 1KV-15KV for the polarization temperature; Polarization time is between 20min-140min (above-mentioned steps (5) duration) generally.
Below in conjunction with embodiment the polarization method that the present invention relates to is described in detail, but not as limitation of the present invention.
Embodiment 1:
Adopting polarization method involved in the present invention, is that the cement base piezoelectric ceramic composite of 1mm polarizes to thickness, and the polarization temperature is 130 ° of C, and the polarization time is from 20min-140min; Polarizing voltage adopts respectively (1KV, 3KV, 5KV, 6.5KV); After polarization is finished, behind cement base piezoelectric ceramic composite cool to room temperature, blot the remaining silicone oil of material surface with lens wiping paper; Electric property with the accurate electric impedance analyzer test of HP4294A cement base piezoelectric ceramic composite material; Utilize electromechanical coupling factor (electromechanical coupling coefficient) kt to characterize degree of polarization.5 groups of each test points of parallel polarization completion rate 100%(are got 5 samples, are 1 group; If the mean deviation of the electromechanical coupling factor of 5 samples all in 10%, thinks that then this group polarization completion rate is 100%; If have 1 beyond 10%, the completion rate that then polarizes is 80%; By that analogy), test data is seen Fig. 3.By this polar system the polarization completion rate of cement base piezoelectric ceramic composite is all reached 100%; Validity and the reasonability of polar system of the present invention have been described.
Embodiment 2:
Adopting polarization method involved in the present invention, is that the cement base piezoelectric ceramic composite of 1mm polarizes to thickness, and polarizing voltage is 5.5KV, and the polarization time is from 20min-140min; The polarization temperature adopts respectively that (figure of 20oC adds, Fig. 4); 90 ° of C, 130 ° of C, 160 ° of C); After polarization is finished, behind cement base piezoelectric ceramic composite cool to room temperature, blot the remaining silicone oil of material surface with lens wiping paper; Electric property with the accurate electric impedance analyzer test of HP4294A cement base piezoelectric ceramic composite material; Utilize electromechanical coupling factor (electromechanical coupling coefficient) kt to characterize degree of polarization, the implication of electromechanical coupling factor (Kt) is: piezoelectric vibrator is in vibration processes, change mechanical energy into electric energy, or changing electric energy into mechanical energy, the degree of the mutual conversion of this expression energy represents with electromechanical coupling factor.Below respectively organize parallel polarization completion rate 100%, test data is seen Fig. 4.
Embodiment 3:
Adopt polarization method involved in the present invention, the cement base piezoelectric ceramic composite sample of 0.8mm-3.2mm different-thickness is polarized, the polarization temperature is 130 ° of C; Do not limit the polarization time saturated polarization voltage condition that observation post applies.Each organizes parallel polarization completion rate 100%, and polarization data is seen Fig. 5.
The present invention is to electrically contact polarization method as the basis, in conjunction with the advantage of corona discharge polarization method; Adopt DC power supply to apply polarizing voltage, realize the fixing and polarization process of cement base piezoelectric ceramic composite with the needle-like anchor clamps; Degree of polarization and polarization uniformity have been guaranteed; Cement base piezoelectric ceramic composite specimen surface brushing silver slurry, to form plate electrode, it is even, stable to have guaranteed to act on polarized lip-deep electric field; Cement base piezoelectric ceramic composite sample is fixed with the needle-like anchor clamps, and be positioned in the container that fills silicone oil, by polarize temperature control of the constent temperature heater with temperature regulating device, protective resistance on polarized circuit is connected may with what avoid puncturing in the polarization process; High-voltage dc voltage table in parallel at needle-like anchor clamps two ends is to realize the monitoring of polarizing voltage.
Polarization condition of the present invention is simple, and is easy to operate, avoids polarization to puncture; Controllable poles parameter (comprising polarizing voltage, polarization current, polarization time, polarized material thickness etc.); The polarization process good stability, the dielectric property of polarized material and the stability of piezoelectric property are guaranteed; Can successfully realize the polarization of cement base piezoelectric ceramic composite.
Claims (10)
1. the polar system of a cement base piezoelectric ceramic composite, comprise adjustable high-voltage DC power supply, voltmeter and polarization anchor clamps, the terminals of polarization anchor clamps are connected with the output of high-voltage DC power supply, the terminals of voltmeter and polarization anchor clamps also connect, it is characterized in that, comprise heating tank and the heater that heating tank is heated, described polarization anchor clamps are immersed in the heating oil in the heating tank.
2. the polar system of cement base piezoelectric ceramic composite according to claim 1 is characterized in that, comprises current-limiting resistance, and described current-limiting resistance is serially connected between high-voltage DC power supply and the polarization anchor clamps; Described heating tank is glassware, and described heater is the digital display type heater, and glassware places on the digital display type heater; Described heating oil is silicone oil, and described voltmeter is digital display type high-voltage dc voltage table.
3. the polar system of cement base piezoelectric ceramic composite according to claim 1, it is characterized in that, described polarization anchor clamps comprise frame and two thimbles of high-temperature resistance plastice, described frame comprise base and with two blocks of side plates of base one, described thimble is installed on the side plate, thimble comprises conical needle point, and the needle point of two thimbles is relative; Have at least one to be movable thimble in two thimbles, movable thimble by tailstock barrel and spring fitting on side plate; Described tailstock barrel is fixed in the thimble trepanning of side plate, and movable thimble passes tailstock barrel, and the shank of movable thimble and the endoporus of tailstock barrel are slidingly matched; The rear end of movable thimble needle point comprises spring fastening, and described spring housing is on shank, and an end of spring is against on the spring fastening, the other end be against on the side plate or the end face of tailstock barrel on.
4. the polar system of cement base piezoelectric ceramic composite according to claim 3 is characterized in that, the cone angle of needle point is 25-35 °; The material of frame is polyimides, polysulfones, polyphenylene sulfide, polyether-ether-ketone or polyether sulfone; The material of tailstock barrel is stainless steel.
5. the polar system of cement base piezoelectric ceramic composite according to claim 2 is characterized in that, described current-limiting resistance is bar-shaped glass glaze film resistance, resistance value 80-120 megaohm.
6. the cement base piezoelectric ceramic composite polarization method based on the described system of claim 1 is characterized in that the relative dielectric constant of cement base piezoelectric composite material is 100-800, thickness 0.7mm-32mm; The polarization temperature is at 90-160 ° of C, polarizing voltage 1KV-15KV; Polarization time-20min-140min.
7. described cement base piezoelectric ceramic composite polarization method according to claim 6, it is characterized in that, the cement base piezoelectric ceramic composite is heated to the stage of polarization temperature for preheating the stage from room temperature, pre-warmed programming rate be 2-4 ° C/ minute, when being warmed up to 87-93 ° of C, be stabilized in this temperature range, remove the moisture in the cement base piezoelectric ceramic composite hole; Cement base piezoelectric ceramic composite surface is warming up to the polarization temperature after no longer including Bubble formation again.
8. described cement base piezoelectric ceramic composite polarization method according to claim 6 is characterized in that, the cement base piezoelectric ceramic composite is opened the adjustable high-voltage DC power supply after reaching the polarization temperature, regulates electric current to the 0.8-1.2 milliampere; After current stabilization, slowly improve voltage to the voltage that polarizes with 80-120V/ minute speed.
9. described cement base piezoelectric ceramic composite polarization method according to claim 8 is characterized in that, in slowly putting forward high-tension process, such as the reading fluctuating range of voltmeter greater than 100V, the voltage of then keeping this moment is constant, until the reading fluctuation less than behind the 10V, continues to improve voltage.
10. described cement base piezoelectric ceramic composite polarization method according to claim 6 is characterized in that, in polarization process, the reading of voltmeter slowly reduced with 10V/ minute, shows that polarization process finishes; After confirming that polarization process is finished, progressively reduce the voltage that applies, until voltage is zero.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104183695A (en) * | 2014-09-02 | 2014-12-03 | 济南大学 | Polarization system and method of large-length-diameter-ratio piezoelectric ceramic transistor |
| CN106771407A (en) * | 2017-01-22 | 2017-05-31 | 长安大学 | A kind of pluggable piezoelectric polarization device high temperature test fixture |
| CN111554804A (en) * | 2020-05-26 | 2020-08-18 | 大连理工大学 | Synchronous polarization method for partitioned piezoelectric elements |
| CN111883650A (en) * | 2020-07-20 | 2020-11-03 | 清华大学深圳国际研究生院 | Preparation method of flexible multilayer composite piezoelectric film and flexible multilayer composite piezoelectric film |
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| CN111554804A (en) * | 2020-05-26 | 2020-08-18 | 大连理工大学 | Synchronous polarization method for partitioned piezoelectric elements |
| CN111554804B (en) * | 2020-05-26 | 2021-09-24 | 大连理工大学 | Synchronous polarization method for partitioned piezoelectric elements |
| CN111883650A (en) * | 2020-07-20 | 2020-11-03 | 清华大学深圳国际研究生院 | Preparation method of flexible multilayer composite piezoelectric film and flexible multilayer composite piezoelectric film |
| CN111883650B (en) * | 2020-07-20 | 2023-09-15 | 清华大学深圳国际研究生院 | Preparation method of flexible multilayer composite piezoelectric film and flexible multilayer composite piezoelectric film |
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