CN108336218A - A kind of road piezo-electricity composite material and preparation method thereof - Google Patents
A kind of road piezo-electricity composite material and preparation method thereof Download PDFInfo
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- CN108336218A CN108336218A CN201810084892.6A CN201810084892A CN108336218A CN 108336218 A CN108336218 A CN 108336218A CN 201810084892 A CN201810084892 A CN 201810084892A CN 108336218 A CN108336218 A CN 108336218A
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- electricity composite
- kynoar
- road
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- 239000002131 composite material Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 60
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 37
- 229910052709 silver Inorganic materials 0.000 claims description 37
- 239000004332 silver Substances 0.000 claims description 37
- 239000011812 mixed powder Substances 0.000 claims description 30
- 230000010287 polarization Effects 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 229910052593 corundum Inorganic materials 0.000 claims description 20
- 239000010431 corundum Substances 0.000 claims description 20
- 230000005684 electric field Effects 0.000 claims description 20
- 238000003760 magnetic stirring Methods 0.000 claims description 19
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 18
- 239000011521 glass Substances 0.000 claims description 18
- 238000000576 coating method Methods 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 12
- 244000137852 Petrea volubilis Species 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000007731 hot pressing Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 238000011068 loading method Methods 0.000 abstract description 5
- 239000002689 soil Substances 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 description 20
- 239000000463 material Substances 0.000 description 10
- 238000001354 calcination Methods 0.000 description 9
- 235000019441 ethanol Nutrition 0.000 description 7
- 230000005611 electricity Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical group FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 230000018199 S phase Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/80—Constructional details
- H10N30/85—Piezoelectric or electrostrictive active materials
- H10N30/852—Composite materials, e.g. having 1-3 or 2-2 type connectivity
-
- E—FIXED CONSTRUCTIONS
- E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
- E01C—CONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
- E01C9/00—Special pavings; Pavings for special parts of roads or airfields
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/09—Forming piezoelectric or electrostrictive materials
- H10N30/092—Forming composite materials
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/80—Constructional details
- H10N30/85—Piezoelectric or electrostrictive active materials
- H10N30/853—Ceramic compositions
- H10N30/8536—Alkaline earth metal based oxides, e.g. barium titanates
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/80—Constructional details
- H10N30/85—Piezoelectric or electrostrictive active materials
- H10N30/857—Macromolecular compositions
Abstract
The invention discloses a kind of road piezo-electricity composite materials and preparation method thereof, by being that 0.6 0.8 parts of barium titanate and 0.2 0.4 parts of Kynoar form by mass fraction, the road has excellent piezoelectricity and dielectric properties with piezo-electricity composite material, anti- traffic loading impact property is preferable simultaneously, and it is smaller on soil environment influence, and preparation method is simple.
Description
Technical field
The invention belongs to the studying technological domain of Load materials, it is related to a kind of road piezo-electricity composite material and its preparation side
Method.
Background technology
With the development of society and economy, along with the continuous exhaustion of non-renewable energy resources, environmental quality constantly declines, such as
What is efficiently collected clean energy resource and can be used in engineering in practice, and the emphasis of collection of energy research is become.It is well known that road
In use, it to undertake hundreds thousand of vehicles to million times every year to roll, the vibrational energy generated is considerable, vehicle
Vibrational energy can not only damage road, also result in the waste of the energy.If vibration energy harvesting is got up, by its turn
The energy that can be for people to use is turned to, can not only bring huge economic benefit and environmental benefit, and road surface can be reduced
Vibration and deformation reduce pavement structure damage etc., have boundless application prospect.
It is both domestic and external at present to study the electricity collection aspect for being concentrated mainly on piezoelectric ceramics, and to being suitable for road generation technology
Piezoelectric material prepare it is very few.When carrying out road energy collection, piezoelectric material will be subjected to Driving Loading repeatedly, and
For a long time in the severe natural environment, should not only have an ability of high resistance environmental disruption effect, should also with compared with
Good piezoelectric property, dielectric properties and piezoelectricity coupling performance.Therefore, the durability of piezoelectric material and piezoelectric property for it in road
Application in the environment of road is most important.
The piezoelectric property and dielectric properties of traditional piezoelectric ceramics are very good, but its hard and crisp characteristic make its molding compared with
For difficulty, and anti-traffic loading impact property is poor；It is multiple that piezoelectricity is made by polymer of the addition with good mechanical properties
Condensation material, although its hard and crisp characteristic is improved, so that the piezoelectric property of composite material and dielectric properties reduce, electricity
Performance is seriously obstructed.In addition, traditional piezoelectric material lead content is higher, it is affected to ecological soil environment.
Invention content
It is an object of the invention to overcome the above-mentioned prior art, provide a kind of road piezo-electricity composite material and its
Preparation method, the road with piezo-electricity composite material have excellent piezoelectricity and dielectric properties, while anti-traffic loading impact property compared with
It is good and smaller on soil environment influence, and preparation method is simple.
In order to achieve the above objectives, road of the present invention with piezo-electricity composite material by being 0.6-0.8 parts by mass fraction
Barium titanate and 0.2-0.4 parts of Kynoar composition.
The fusing point Tm of Kynoar is 167 DEG C, density p 1.75g/cm3~1.78g/cm3, the number of Kynoar is equal
Molecular weight is 825000.
The preparation method of road piezo-electricity composite material of the present invention includes the following steps：
1) barium titanate is placed in corundum crucible, then corundum crucible is subjected to heating heating and is kept the temperature, then be cooled to room temperature；
2) Kynoar is weighed and barium titanate that step 1) obtains；
3) Kynoar and barium titanate are placed into magnetic stirring apparatus, add absolute ethyl alcohol, is then ground,
So that it is uniformly mixed, then be dried, obtains mixed powder；
4) mixed powder that step 3) obtains is placed into hot pressing grinding tool, is kept the temperature after being again heated to 170-190 DEG C,
Then pressure is applied to mixed powder again, and keeps pressure, obtain sample；
5) alundum (Al2O3) solution is taken, then alundum (Al2O3) solution is uniformly coated on glass plate, then puts sample
It is rotated after setting on glass plate, keeps its specimen surface smooth, then cleaned, then dry specimen surface；
6) silver paste is coated in one end of sample, then sample is toasted, then coat silver paste in the other end of sample again,
It is toasted again, is then cooled to room temperature, then polish off the silver paste of specimen surface with sand paper；
7) sample that step 6) obtains is placed in constant temperature oil bath and is heated, then apply high voltage direct current at the both ends of sample
Electric field makes electricdomain inside sample obtain road piezo-electricity composite material along direction of an electric field aligned orderly.
Corundum crucible is subjected to heating heating in step 1) and the concrete operations of heat preservation are：By corundum crucible with 5~15 DEG C/
The speed of min is at the uniform velocity warming up to 850 DEG C -1050 DEG C；And keep the temperature 60~90min.
The concrete operations of step 3) are：Kynoar and barium titanate are placed into magnetic stirring apparatus, then stirred to magnetic force
It mixes and absolute ethyl alcohol is added in device, then grind 10-20min, place into baking oven, and dry 60- at a temperature of 100 DEG C
90min obtains mixed powder.
The time kept the temperature in step 4) is 50-90min, and the time that pressure is kept is 20-40min.
In step 5), sample is first cleaned with clear water, is then cleaned again with absolute ethyl alcohol.
It is in the concrete operations of one end of sample coating silver paste in step 6)：It is primary every 5min coatings in the end of sample
The number of silver paste, coating is 3-5 times.
The concrete operations of step 6) are：Silver paste is coated in one end of sample, sample is then placed into 100 DEG C~120 DEG C
Baking oven in toast 50~90min, then sample the other end coat silver paste, be then placed into 100 DEG C~120 DEG C of baking oven
2-3h is toasted, is then cooled to room temperature, then polish off the silver paste of specimen surface with sand paper；
The concrete operations of step 7) are：The sample that step 6) obtains is placed in thermostatical oil bath and is heated to 80~120 DEG C,
It presses high-voltage dc at the both ends of sample again, wherein the Polarization field strength of high-voltage dc is 3~5kV/mm, when polarization
Between be 30~40min, so that electricdomain inside sample is obtained road piezo-electricity composite material along direction of an electric field aligned orderly.
The invention has the advantages that：
Road of the present invention prepares road piezoelectricity as raw material using barium titanate and Kynoar with piezo-electricity composite material and answers
Condensation material can greatly mitigate conventional piezoelectric materials and be embedded in destruction of the road later to local ecological environment of soil, and meeting can
The Ecological Concept of sustainable development, while in the preparation, the piezo-electricity composite material formed to barium titanate and Kynoar is forged
It burns, relative to the composite material of barium titanate and Kynoar without calcining, piezoelectric property and dielectric properties obtain significantly
It improves.The barium titanate after high-temperature process, activity are excited simultaneously, and electricdomain is turned to and is relatively easy in polarization process, with drop
The surface energy of low barium titanate eliminates the gap on its surface, promotes it to be combined with polymer phase even closer, and polarization is more filled
Point, piezoelectric property is more excellent.In addition, the present invention in preparation process by mixed powder apply pressure, obtain sample, with
The anti-traffic loading impact property of road piezo-electricity composite material is improved, simple process and low cost is honest and clean, and comprehensive performance is more excellent.
Description of the drawings
Fig. 1 is the XRD diagram for the road piezo-electricity composite material that embodiment one is prepared；
Fig. 2 is the XRD diagram for the road piezo-electricity composite material that embodiment two is prepared；
Fig. 3 is the XRD diagram for the road piezo-electricity composite material that embodiment three is prepared；
Fig. 4 is the XRD diagram for the road piezo-electricity composite material that example IV is prepared.
Specific implementation mode
The present invention is described in further detail below in conjunction with the accompanying drawings：
Embodiment one
Road of the present invention is made of with piezo-electricity composite material the barium titanate of 70g and the Kynoar of 32g.
The fusing point Tm of Kynoar is 167 DEG C, density p 1.75g/cm3, the number-average molecular weight of Kynoar is
825000。
The preparation method of road piezo-electricity composite material of the present invention includes the following steps：
1) Kynoar and barium titanate are weighed；
2) Kynoar and barium titanate are placed into magnetic stirring apparatus, then anhydrous second is added into magnetic stirring apparatus
Then alcohol grinds 15min, place into baking oven, and dry 75min at a temperature of 100 DEG C, obtains mixed powder；
3) mixed powder that step 2) obtains is placed into hot pressing grinding tool, 60min is kept the temperature after being again heated to 175 DEG C, so
Pressure is applied to mixed powder again afterwards, and keeps pressure 30min, obtains sample；
4) alundum (Al2O3) solution is taken, then alundum (Al2O3) solution is uniformly coated on glass plate, then puts sample
It is rotated after setting on glass plate, keeps its specimen surface smooth, then sample is first cleaned with clear water, then used again
Absolute ethyl alcohol is cleaned, and specimen surface is subsequently dried；
5) a silver paste is coated every 5min in one end of sample, the number of coating is 3 times, is then placed into sample
60min is toasted in 120 DEG C of baking oven, then coats silver paste in the other end of sample, is then placed into 120 DEG C of baking oven and is toasted
2h is then cooled to room temperature, then the silver paste of specimen surface is polished off with sand paper；
6) sample that step 5) obtains is placed in thermostatical oil bath and is heated to 100 DEG C, then is high in the both ends of sample pressure
Press DC electric field, wherein the Polarization field strength of high-voltage dc is 4kV/mm, polarization time 35min, makes electricdomain inside sample
Along direction of an electric field aligned orderly, road piezo-electricity composite material is obtained.
Embodiment two
Road of the present invention is made of with piezo-electricity composite material the barium titanate of 75g and the Kynoar of 32g；
The fusing point Tm of Kynoar is 167 DEG C, density p 1.77g/cm3, the number-average molecular weight of Kynoar is
825000。
The preparation method of road piezo-electricity composite material of the present invention includes the following steps：
1) barium titanate is placed in corundum crucible, then corundum crucible is at the uniform velocity warming up to 850 DEG C with the speed of 5 DEG C/min；
And 90min is kept the temperature respectively, it is then cooled to room temperature again；
2) Kynoar is weighed and barium titanate that step 1) obtains；
3) Kynoar and barium titanate are placed into magnetic stirring apparatus, then anhydrous second is added into magnetic stirring apparatus
Then alcohol grinds 10min, place into baking oven, and dry 60min at a temperature of 100 DEG C, obtains mixed powder；
4) mixed powder that step 3) obtains is placed into hot pressing grinding tool, 65min is kept the temperature after being again heated to 180 DEG C, so
Pressure is applied to mixed powder again afterwards, and keeps pressure 40min, obtains sample；
5) alundum (Al2O3) solution is taken, then alundum (Al2O3) solution is uniformly coated on glass plate, then puts sample
It is rotated after setting on glass plate, keeps its specimen surface smooth, then sample is first cleaned with clear water, then used again
Absolute ethyl alcohol is cleaned, and specimen surface is subsequently dried；
6) a silver paste is coated every 5min in one end of sample, the number of coating is 5 times, is then placed into sample
90min is toasted in 100 DEG C of baking oven, then coats silver paste in the other end of sample, is then placed into 100 DEG C of baking oven and is toasted
3h is then cooled to room temperature, then the silver paste of specimen surface is polished off with sand paper；
7) sample that step 6) obtains is placed in thermostatical oil bath and is heated to 80 DEG C, then in the both ends of sample pressure high pressure
DC electric field, wherein the Polarization field strength of high-voltage dc is 3kV/mm, polarization time 40min, makes electricdomain edge inside sample
Direction of an electric field aligned orderly obtains road piezo-electricity composite material.
Embodiment three
Road of the present invention is made of with piezo-electricity composite material the barium titanate of 68g and the Kynoar of 29g；
The fusing point Tm of Kynoar is 167 DEG C, density p 1.76g/cm3, the number-average molecular weight of Kynoar is
825000。
The preparation method of road piezo-electricity composite material of the present invention includes the following steps：
1) barium titanate is placed in corundum crucible, then corundum crucible is at the uniform velocity warming up to 950 DEG C with the speed of 10 DEG C/min；
And 75min is kept the temperature respectively, it is then cooled to room temperature again；
2) Kynoar is weighed and barium titanate that step 1) obtains；
3) Kynoar and barium titanate are placed into magnetic stirring apparatus, then anhydrous second is added into magnetic stirring apparatus
Then alcohol grinds 13min, place into baking oven, and dry 70min at a temperature of 100 DEG C, obtains mixed powder；
4) mixed powder that step 3) obtains is placed into hot pressing grinding tool, 50min is kept the temperature after being again heated to 190 DEG C, so
Pressure is applied to mixed powder again afterwards, and keeps pressure 30min, obtains sample；
5) alundum (Al2O3) solution is taken, then alundum (Al2O3) solution is uniformly coated on glass plate, then puts sample
It is rotated after setting on glass plate, keeps its specimen surface smooth, then sample is first cleaned with clear water, then used again
Absolute ethyl alcohol is cleaned, and specimen surface is subsequently dried；
6) a silver paste is coated every 5min in one end of sample, the number of coating is 3 times, is then placed into sample
70min is toasted in 110 DEG C of baking oven, then coats silver paste in the other end of sample, is then placed into 110 DEG C of baking oven and is toasted
2h is then cooled to room temperature, then the silver paste of specimen surface is polished off with sand paper；
7) sample that step 6) obtains is placed in thermostatical oil bath and is heated to 120 DEG C, then is high in the both ends of sample pressure
Press DC electric field, wherein the Polarization field strength of high-voltage dc is 5kV/mm, polarization time 30min, makes electricity inside sample
Farmland obtains road piezo-electricity composite material along direction of an electric field aligned orderly.
Example IV
Road of the present invention is made of with piezo-electricity composite material the barium titanate of 66g and the Kynoar of 28g；
The fusing point Tm of Kynoar is 167 DEG C, density p 1.78g/cm3, the number-average molecular weight of Kynoar is
825000。
The preparation method of road piezo-electricity composite material of the present invention includes the following steps：
1) barium titanate is placed in corundum crucible, then corundum crucible is at the uniform velocity warming up to 1050 DEG C with the speed of 8 DEG C/min；
And 60min is kept the temperature respectively, it is then cooled to room temperature again；
2) Kynoar is weighed and barium titanate that step 1) obtains；
3) Kynoar and barium titanate are placed into magnetic stirring apparatus, then anhydrous second is added into magnetic stirring apparatus
Then alcohol grinds 15min, place into baking oven, and dry 90min at a temperature of 100 DEG C, obtains mixed powder；
4) mixed powder that step 3) obtains is placed into hot pressing grinding tool, 55min is kept the temperature after being again heated to 175 DEG C, so
Pressure is applied to mixed powder again afterwards, and keeps pressure 40min, obtains sample；
5) alundum (Al2O3) solution is taken, then alundum (Al2O3) solution is uniformly coated on glass plate, then puts sample
It is rotated after setting on glass plate, keeps its specimen surface smooth, then sample is first cleaned with clear water, then used again
Absolute ethyl alcohol is cleaned, and specimen surface is subsequently dried；
6) a silver paste is coated every 5min in one end of sample, the number of coating is 3 times, is then placed into sample
60min is toasted in 120 DEG C of baking oven, then coats silver paste in the other end of sample, is then placed into 120 DEG C of baking oven and is toasted
2h is then cooled to room temperature, then the silver paste of specimen surface is polished off with sand paper；
7) sample that step 6) obtains is placed in thermostatical oil bath and is heated to 110 DEG C, then is high in the both ends of sample pressure
Press DC electric field, wherein the Polarization field strength of high-voltage dc is 4kV/mm, polarization time 32min, makes electricity inside sample
Farmland obtains road piezo-electricity composite material along direction of an electric field aligned orderly.
Embodiment five
Road piezo-electricity composite material of the present invention by by mass fraction be 0.6 part barium titanate and 0.4 part it is poly- partially
Vinyl fluoride forms；
The fusing point Tm of Kynoar is 167 DEG C, density p 1.75g/cm3, the number-average molecular weight of Kynoar is
825000。
The preparation method of road piezo-electricity composite material of the present invention includes the following steps：
1) barium titanate is placed in corundum crucible, then corundum crucible is at the uniform velocity warming up to 950 DEG C with the speed of 8 DEG C/min；
And 90min is kept the temperature respectively, it is then cooled to room temperature again；
2) Kynoar is weighed and barium titanate that step 1) obtains；
3) Kynoar and barium titanate are placed into magnetic stirring apparatus, then anhydrous second is added into magnetic stirring apparatus
Then alcohol grinds 20min, place into baking oven, and dry 90min at a temperature of 100 DEG C, obtains mixed powder；
4) mixed powder that step 3) obtains is placed into hot pressing grinding tool, 90min is kept the temperature after being again heated to 170 DEG C, so
Pressure is applied to mixed powder again afterwards, and keeps pressure 35min, obtains sample；
5) alundum (Al2O3) solution is taken, then alundum (Al2O3) solution is uniformly coated on glass plate, then puts sample
It is rotated after setting on glass plate, keeps its specimen surface smooth, then sample is first cleaned with clear water, then used again
Absolute ethyl alcohol is cleaned, and specimen surface is subsequently dried；
6) a silver paste is coated every 5min in one end of sample, the number of coating is 4 times, is then placed into sample
50min is toasted in 110 DEG C of baking oven, then coats silver paste in the other end of sample, is then placed into 110 DEG C of baking oven and is toasted
2.5h is then cooled to room temperature, then the silver paste of specimen surface is polished off with sand paper；
7) sample that step 6) obtains is placed in thermostatical oil bath and is heated to 100 DEG C, then is high in the both ends of sample pressure
Press DC electric field, wherein the Polarization field strength of high-voltage dc is 3.5kV/mm, and polarization time 32min makes inside sample
Electricdomain obtains road piezo-electricity composite material along direction of an electric field aligned orderly.
Embodiment six
Road piezo-electricity composite material of the present invention by by mass fraction be 0.8 part barium titanate and 0.2 part it is poly- partially
Vinyl fluoride forms；
The fusing point Tm of Kynoar is 167 DEG C, density p 1.78g/cm3, the number-average molecular weight of Kynoar is
825000。
The preparation method of road piezo-electricity composite material of the present invention includes the following steps：
1) barium titanate is placed in corundum crucible, then corundum crucible is at the uniform velocity warming up to 850 DEG C with the speed of 15 DEG C/min；
And 60min is kept the temperature respectively, it is then cooled to room temperature again；
2) Kynoar is weighed and barium titanate that step 1) obtains；
3) Kynoar and barium titanate are placed into magnetic stirring apparatus, then anhydrous second is added into magnetic stirring apparatus
Then alcohol grinds 20min, place into baking oven, and dry 90min at a temperature of 100 DEG C, obtains mixed powder；
4) mixed powder that step 3) obtains is placed into hot pressing grinding tool, 90min is kept the temperature after being again heated to 190 DEG C, so
Pressure is applied to mixed powder again afterwards, and keeps pressure 40min, obtains sample；
5) alundum (Al2O3) solution is taken, then alundum (Al2O3) solution is uniformly coated on glass plate, then puts sample
It is rotated after setting on glass plate, keeps its specimen surface smooth, then sample is first cleaned with clear water, then used again
Absolute ethyl alcohol is cleaned, and specimen surface is subsequently dried；
6) a silver paste is coated every 5min in one end of sample, the number of coating is 5 times, is then placed into sample
90min is toasted in 120 DEG C of baking oven, then coats silver paste in the other end of sample, is then placed into 120 DEG C of baking oven and is toasted
3h is then cooled to room temperature, then the silver paste of specimen surface is polished off with sand paper；
7) sample that step 6) obtains is placed in thermostatical oil bath and is heated to 120 DEG C, then is high in the both ends of sample pressure
Press DC electric field, wherein the Polarization field strength of high-voltage dc is 5kV/mm, polarization time 40min, makes electricity inside sample
Farmland obtains road piezo-electricity composite material along direction of an electric field aligned orderly.
Embodiment seven
Road of the present invention is made of with piezo-electricity composite material the barium titanate of 70g and the Kynoar of 32g；
The fusing point Tm of Kynoar is 167 DEG C, density p 1.75g/cm3, the number-average molecular weight of Kynoar is
825000。
The preparation method of road piezo-electricity composite material of the present invention includes the following steps：
1) barium titanate is placed in corundum crucible, then corundum crucible is at the uniform velocity warming up to 950 DEG C with the speed of 15 DEG C/min；
And 90min is kept the temperature respectively, it is then cooled to room temperature again；
2) Kynoar is weighed and barium titanate that step 1) obtains；
3) Kynoar and barium titanate are placed into magnetic stirring apparatus, then anhydrous second is added into magnetic stirring apparatus
Then alcohol grinds 15min, place into baking oven, and dry 75min at a temperature of 100 DEG C, obtains mixed powder；
4) mixed powder that step 3) obtains is placed into hot pressing grinding tool, 60min is kept the temperature after being again heated to 175 DEG C, so
Pressure is applied to mixed powder again afterwards, and keeps pressure 30min, obtains sample；
5) alundum (Al2O3) solution is taken, then alundum (Al2O3) solution is uniformly coated on glass plate, then puts sample
It is rotated after setting on glass plate, keeps its specimen surface smooth, then sample is first cleaned with clear water, then used again
Absolute ethyl alcohol is cleaned, and specimen surface is subsequently dried；
6) a silver paste is coated every 5min in one end of sample, the number of coating is 3 times, is then placed into sample
60min is toasted in 120 DEG C of baking oven, then coats silver paste in the other end of sample, is then placed into 120 DEG C of baking oven and is toasted
2h is then cooled to room temperature, then the silver paste of specimen surface is polished off with sand paper；
7) sample that step 6) obtains is placed in thermostatical oil bath and is heated to 100 DEG C, then is high in the both ends of sample pressure
Press DC electric field, wherein the Polarization field strength of high-voltage dc is 4kV/mm, polarization time 35min, makes electricity inside sample
Farmland obtains road piezo-electricity composite material along direction of an electric field aligned orderly.
XRD is tested
Using XRD test methods to the road piezoelectricity prepared by embodiment one, embodiment two, embodiment three and example IV
The microstructure of composite material is scanned, shown in specific as shown in Figure 1, Figure 2, Fig. 3 and Fig. 4.
The answering by the leadless piezoelectric ceramics of high-temperature calcination (barium titanate)/Kynoar it can be seen from Fig. 1 to Fig. 4
The intensity of the XRD spectrum of condensation material, characteristic peak is enhanced, and the diffraction maximum of (200) is remarkably reinforced compared to Fig. 1 in Fig. 2,
Represented in Fig. 3 tripartite's phase (200) diffraction maximum splitting, go out to represent (002) peak of the tetragonal phase with piezoelectric property, at this time by
In the transformation of the opposite tetragonal phase of tripartite of the composite material of leadless piezoelectric ceramics (barium titanate)/Kynoar, leadless piezoelectric pottery
The piezoelectric property of the composite material of porcelain (barium titanate)/Kynoar significantly improves.With the lasting raising of calcination temperature, when forging
When burning temperature is increased to 1050 DEG C, as shown in figure 4, the intensity at (002) peak starts to die down, so as to cause leadless piezoelectric ceramics (titanium
Sour barium) piezoelectric property of composite material of/Kynoar begins to decline.It follows that leadless piezoelectric ceramics (barium titanate)/poly-
The optimum calcinating temperature of the composite material of vinylidene is 950 DEG C, with this condition, leadless piezoelectric ceramics (barium titanate)/poly- inclined
The piezoelectric property of the composite material of vinyl fluoride reaches maximum value.
Electric property
It uses HP4294A impedance analyzers in the case where test frequency is 1kHz, measures the piezo-electricity composite material of each embodiment
Dielectric loss tan δ；The piezoelectric property of the piezo-electricity composite material of each embodiment is tested using the quasi-static instrument tests of d33, is had
The results are shown in Table 1 for body.
Table 1
From table 1 it follows that embodiment one and the experimental result of embodiment two, embodiment three and example IV compare,
The piezoelectric strain constant of the composite material of leadless piezoelectric ceramics (barium titanate)/Kynoar without calcining, piezoelectric voltage are normal
Number and relative dielectric constant, which are respectively less than, mixes the leadless piezoelectric ceramics (titanium that calcination temperature is respectively 850 DEG C, 950 DEG C and 1050 DEG C
Sour barium)/Kynoar composite material；In addition, leadless piezoelectric ceramics (the barium titanate)/Kynoar that do not calcine is compound
Dielectric material loss is also maximum；When the composite material calcination temperature of leadless piezoelectric ceramics (barium titanate)/Kynoar reaches 950
DEG C when, piezoelectric strain constant value and relative dielectric constant reach maximum value；When temperature reaches 1050 DEG C, piezoelectric strain is normal
Numerical value and relative dielectric constant are begun to decline.Data comparison illustrates, mixes leadless piezoelectric ceramics (barium titanate)/poly- inclined fluorine of calcining
The composite material of ethylene can be obviously improved its piezoelectric property, and the calcination temperature of leadless piezoelectric ceramics (barium titanate) is 950
DEG C when, composition leadless piezoelectric ceramics (barium titanate)/Kynoar composite material piezoelectric property it is best.
To sum up, composite wood of the high-temperature calcination of barium titanate ceramics for leadless piezoelectric ceramics (barium titanate)/Kynoar
The electrical property of material has tremendous influence, and after Overheating Treatment, leadless piezoelectric ceramics (barium titanate) activity is excited, polarization process
Middle electricdomain steering becomes easier to, while heat treatment process reduces the surface energy of leadless piezoelectric ceramics (barium titanate), has eliminated table
The hole in face so that combined with polymer phase it is even closer, polarization it is more abundant, to improve piezoelectric property.But when with
The calcination temperature of leadless piezoelectric ceramics (barium titanate) gradually rises, and piezoelectric property is caused to start to weaken, this is because leadless piezoelectric
Phase transformation has occurred in ceramic (barium titanate).
Claims (10)
1. a kind of road piezo-electricity composite material, which is characterized in that the barium titanate and 0.2-0.4 for being 0.6-0.8 parts by mass fraction
The Kynoar composition of part.
2. road piezo-electricity composite material according to claim 1, which is characterized in that the fusing point Tm of Kynoar is 167
DEG C, density p 1.75g/cm3~1.78g/cm3, the number-average molecular weight of Kynoar is 825000.
3. a kind of preparation method of road piezo-electricity composite material described in claim 1, which is characterized in that include the following steps：
1) barium titanate is placed in corundum crucible, then corundum crucible is subjected to heating heating and is kept the temperature, then be cooled to room temperature；
2) Kynoar is weighed and barium titanate that step 1) obtains；
3) Kynoar and barium titanate are placed into magnetic stirring apparatus, add absolute ethyl alcohol, be then ground, makes it
It is uniformly mixed, then is dried, obtain mixed powder；
4) mixed powder that step 3) obtains is placed into hot pressing grinding tool, is kept the temperature after being again heated to 170-190 DEG C, then
Pressure is applied to mixed powder again, and keeps pressure, obtains sample；
5) alundum (Al2O3) solution is taken, then alundum (Al2O3) solution is uniformly coated on glass plate, is then placed into sample
It is rotated after on glass plate, keeps its specimen surface smooth, then cleaned, then dry specimen surface；
6) silver paste is coated in one end of sample, then sample is toasted, then again in the other end of sample coating silver paste, then into
Row baking, is then cooled to room temperature, then the silver paste of specimen surface is polished off with sand paper；
7) sample that step 6) obtains is placed in constant temperature oil bath and is heated, then apply high voltage direct current at the both ends of sample
, so that electricdomain inside sample is obtained road piezo-electricity composite material along direction of an electric field aligned orderly.
4. the preparation method of road piezo-electricity composite material according to claim 1, which is characterized in that by corundum in step 1)
Crucible carries out heating heating and the concrete operations of heat preservation are：Corundum crucible is at the uniform velocity warming up to 850 with the speed of 5~15 DEG C/min
℃-1050℃；And keep the temperature 60~90min.
5. the preparation method of road piezo-electricity composite material according to claim 1, which is characterized in that the specific behaviour of step 3)
As：Kynoar and barium titanate are placed into magnetic stirring apparatus, then absolute ethyl alcohol is added into magnetic stirring apparatus, then
10-20min is ground, is placed into baking oven, and dry 60-90min at a temperature of 100 DEG C, obtains mixed powder.
6. the preparation method of road piezo-electricity composite material according to claim 1, which is characterized in that kept the temperature in step 4)
Time is 50-90min, and the time that pressure is kept is 20-40min.
7. the preparation method of road piezo-electricity composite material according to claim 1, which is characterized in that in step 5), will try
Sample is first cleaned with clear water, is then cleaned again with absolute ethyl alcohol.
8. the preparation method of road piezo-electricity composite material according to claim 1, which is characterized in that in sample in step 6)
One end coating silver paste concrete operations be：A silver paste is coated every 5min in the end of sample, the number of coating is 3-5
It is secondary.
9. the preparation method of road piezo-electricity composite material according to claim 1, which is characterized in that the specific behaviour of step 6)
As：Silver paste is coated in one end of sample, sample is then placed into 50~90min of baking in 100 DEG C~120 DEG C of baking oven,
Silver paste is coated in the other end of sample again, is then placed into 100 DEG C~120 DEG C of baking oven and toasts 2-3h, be then cooled to room
Temperature, then polish off with sand paper the silver paste of specimen surface.
10. the preparation method of road piezo-electricity composite material according to claim 1, which is characterized in that step 7) it is specific
Operation is：The sample that step 6) obtains is placed in thermostatical oil bath and is heated to 80~120 DEG C, then is high in the both ends of sample pressure
Press DC electric field, wherein the Polarization field strength of high-voltage dc is 3~5kV/mm, and the polarization time is 30~40min, makes sample
Internal electricdomain obtains road piezo-electricity composite material along direction of an electric field aligned orderly.
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