CN102173790A - Lead-free antiferroelectric ceramic material as well as preparation method and application thereof - Google Patents
Lead-free antiferroelectric ceramic material as well as preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910010293 ceramic material Inorganic materials 0.000 title abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 38
- 238000000498 ball milling Methods 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 230000005616 pyroelectricity Effects 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000007858 starting material Substances 0.000 claims 3
- 230000005684 electric field Effects 0.000 abstract description 13
- 239000000919 ceramic Substances 0.000 abstract description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 abstract 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract 2
- 238000002156 mixing Methods 0.000 abstract 2
- 238000003825 pressing Methods 0.000 abstract 1
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract 1
- 235000017550 sodium carbonate Nutrition 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 17
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 239000011734 sodium Substances 0.000 description 7
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 6
- 230000001939 inductive effect Effects 0.000 description 5
- 230000007246 mechanism Effects 0.000 description 5
- 230000009466 transformation Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000002463 transducing effect Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
The invention relates to lead-free antiferroelectric ceramic as a pyroelectric material or a strain driving material as well as a preparation method and application thereof, belonging to the technical field of pyroelectric sensors or strain driving. The preparation method comprises the following steps of: blending and mixing Na2CO3, Bi2O3, BaCO3 and TiO2 as raw materials in proportion, and then carrying out primary ball-milling and precalcination; carrying out secondary ball-milling, then granulating, and pressing to form a blank body; and finally sintering the blank body to obtain a lead-free antiferroelectric ceramic material, wherein the lead-free antiferroelectric ceramic material has the formula of NayBizTi(1-x)O3(1-x)-xBaTiO3. The lead-free antiferroelectric ceramic prepared through the invention has very high pyroelectric current and adjustable peak value temperature of the pyroelectric current and can be used for an infrared pyroelectric detector and a smart device and a smart system; and in addition, the prepared lead-free antiferroelectric ceramic material has huge strain or electrostriction coefficient induced by an electric field and can be used as raw materials of a driver and a driving element inside a high-accuracy sensor.
Description
Technical field
What the present invention relates to is the material and the preparation thereof in a kind of transmitter and Drive technology field, specifically is a kind of lead-free anti-ferroelectric pottery as pyroelectricity material or strain driving material and its production and application.
Background technology
Antiferroelectric materials becomes the focus of domestic and international research owing to the important effect of play more and more in new and high technology.Such as antiferroelectric materials at the high energy storage capacitor, high strain driving mechanism, pyroelectric sensor all has very large using value in quick-fried electric transducer sensor and the electric refrigeration technology.The main at present antiferroelectric materials that uses is the pick lead titanate (PZT) in high pick district, particularly form and be near the PZT base ceramic material of ferroelectric (FE)-antiferroelectric (AFE) phase boundary because of having abundant phase structure, and the spontaneous polarization that causes of outfields such as temperature, stress and electric field changes and produces cholesteric-nematic transition, so near the composition the phase boundary of antiferroelectric phase and ferroelectric phase is the focus of studying always.And be used widely in fields such as transverter, driving mechanism, energy storage capacitor, infrared thermal release electric detections.Such as utilize thermoinducible ferroelectric-antiferroelectric phase transformation can obtain to use in pyroelectricity is surveyed, utilize the electric field inductive antiferroelectric-ferroelectric phase transition can obtain to use in high strain driving mechanism, utilizes stress induced ferroelectric-antiferroelectric phase transformation to be applied in quick-fried electric transducing field.
But plumbous oxide accounts for more than 60% of raw material gross weight in the PZT sill, and we know that plumbous oxide is a kind of severe toxicity and at high temperature volatile material.The volatilization of a large amount of plumbous oxide certainly will cause the pollution of environment in sintering process, directly the health of harm humans.In recent years, along with the demand of environment protection and human social, research and development novel environmental close friend's function ceramics has become one of focus of endeavouring to research and develop in various countries.European Parliament has passed through decree about " limiting objectionable impurities in electrical equipment and the electronics " such as calendar year 2001, and implements due to 2008.For this reason, the research and development about unleaded series piezoelectric ceramic are carried out in the special project verification of the European Economic Community.The U.S., Japan and China have also improved in succession year by year to developing the supporting dynamics of unleaded series piezoelectric ceramic project.
Find that through retrieval antiferroelectric materials can produce huge strain in effect of electric field owing to antiferroelectric-ferroelectric phase transition, but the antiferroelectric materials that can at room temperature use of exploitation is mainly the PZT sill at present to prior art.Antiferroelectric materials can be induced into ferroelectric phase with antiferroelectric phase under effect of electric field in addition, and the inductive ferroelectric phase can comparatively stable existence, therefore can record a very large pyroelectricity electric current when heating up, such as (Pb, La) (Zr, Sn, Ti) O
3(PLZST) its pyroelectric coefficient of pottery can arrive 160 * 10
-8C cm
-2K
-1, it is worth than high two orders of magnitude of general ferroelectric pyroelectricity material.The metastable ferroelectric phase of inductive is transformed into antiferroelectric meeting again and causes the pyroelectricity current peak when temperature raises, this is the coefficient result of electric field and temperature.And present unleaded Na
0.47Bi
0.47Ti
0.94-0.06BaTiO
3Pottery pyroelectric coefficient at room temperature is 3.6 * 10
-8C cm
-2K
-1(seeing the 2357th to 2362 page of Chinese physical volume 53), phase change lead-free pyroelectricity material (Ba, Sr) TiO
3The pyroelectric coefficient of pottery is 70 * 10
-8Ccm
-2K
-1, there is a big difference for the value of its value and lead-containing materials.
(Na
0.5Bi
0.5) TiO
3(NBT) be a kind of ferroelectric piezoelectric with perovskite structure.Wherein NBT is adding BaTiO
3(BT) after, get most of the attention near its piezoelectric constant of pottery d of the component accurate homotype phase boundary owing to having three parts-cubic accurate homotype phase boundary (BT content is 6mol%-10mol%) and can significantly reducing its excessive coercive field
33Can be near 200pC/N, residual polarization P
rCan reach 38 μ C/cm
2There is a umpolarization temperature in this kind ferroelectric material, and is promptly ferroelectric-antiferroelectric transformation temperature.For pure NBT, this umpolarization temperature is about 190 ℃, and near its umpolarization temperature of component the most approaching accurate homotype phase boundary is minimum, be about 100 ℃, along with the increase of BT content, the umpolarization temperature raises then, such as for the NBT-BT85/15 pottery, its umpolarization temperature is about 210 ℃.Its sodium bismuth mol ratio (Na/Bi) of NBT-BT material of research all is 1 at present.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of lead-free anti-ferroelectric pottery and its production and application is provided, its pyroelectric coefficient at room temperature can reach 140 * 10
-8Ccm
-2K
-1Its electric field inductive strain can reach 0.48%, and the electrostriction strain can reach 0.23%.
The present invention is achieved by the following technical solutions:
The present invention relates to a kind of lead-free anti-ferroelectric pottery as pyroelectricity material or strain driving material, its component is Na
yBi
zTi
(1-x)O
3 (1-x)-xBaTiO
3, i.e. N
100yB
100zT
100 (1-x)-BT
x, wherein: the value of x is 0-0.15, and the value of y is 0.30-0.50, and the value of z is 0.40-0.60,1.0≤z/y≤1.25.
The present invention relates to the preparation method of above-mentioned lead-free anti-ferroelectric pottery, by with Na
2CO
3, Bi
2O
3, BaCO
3And TiO
2For raw material carries out ball milling and precalcining according to the above ratio after the batch mixes, granulation compression moulding obtains idiosome behind secondary ball milling, at last idiosome is carried out sintering and obtains the lead-free anti-ferroelectric stupalith.
Described precalcining is meant: the powder of ball milling and oven dry is placed in the alumina crucible 700-900 ℃ of calcining 1-10 hour and naturally cools to room temperature through grinding;
Described secondary ball milling is meant: use ethanol or water to be the powder of medium after with precalcining ball milling 2-24 hour once more;
Described granulating and forming is meant: oven dry back adding additives PVA carries out granulation, uses mould to obtain the cylinder shape idiosome by the press compacting then.
Described sintering is meant: with idiosome as in the middle of the alumina crucible of adding a cover, or directly idiosome is placed the alumina substrate top to carry out sintering, the sintering temperature rise rate is 5 ℃/min-30 ℃/min, sintering temperature is 1100 ℃-1250 ℃, soaking time is 1-10 hour, cools to room temperature at last with the furnace.
The present invention relates to the application method of above-mentioned lead-free anti-ferroelectric pottery, when 1.0≤z/y≤1.15, can be used as pyroelectricity material; When 1.0＜z/y＜1.25, can be used as the strain driving material.
The present invention utilizes traditional solid phase reaction method synthetic, and production technique is simple; The lead-free anti-ferroelectric pottery that makes has the pyroelectric coefficient suitable with leaded antiferroelectric materials at its transformation temperature place, and can by bismuth sodium when the content of barium titanate transformation temperature is regulated, in the application of infrared thermal release electric detector, have vast market prospect.This kind antiferroelectric ceramics material has very big electric field inductive strain or bigger electrostriction strain in addition, can obtain major application in driving mechanism or high accuracy displacement sensor.The discovery of this kind material is to replacing plumbiferous PbZrO
3The based antiferroelectric material is significant.
Description of drawings
Fig. 1 is embodiment 1 a pyroelectric coefficient synoptic diagram.
Fig. 2 is embodiment 1 a pyroelectric coefficient synoptic diagram.
Fig. 3 induces the strained synoptic diagram for embodiment 1 electric field.
Fig. 4 induces the strained synoptic diagram for embodiment 2 electric fields
Embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Its pyroelectric coefficient of pottery by the present invention's preparation at room temperature can reach 140 * 10
-8Ccm
-2K
-1, suitable with the pyroelectric coefficient of plumbiferous PLZST pottery.And its pyroelectric coefficient peak of material of the present invention's preparation can be transferred to 34 ℃, can only be transferred to 50 ℃ and the pyroelectric coefficient peak of PLZST pottery is minimum at present.Its maximum strain of lead-free anti-ferroelectric pottery by the present invention's preparation can reach 0.48%, and is suitable with present leaded antiferroelectric ceramics.
Embodiment 1
Select the Na of AG for use
2CO
3, Bi
2O
3, BaCO
3And nano level TiO
2For raw material is pressed N
yB
zT
94-BT
6Chemical formula is prepared burden, confected materials uses ethanol to use zirconia ball ball milling 24 hours in ball grinder as medium, oven dry is placed in the alumina crucible through grinding, 850 ℃ of calcinings 3 hours, placing ball grinder behind the cool to room temperature again was that medium uses zirconia ball at ball grinder ball milling 12 hours once more with ethanol.Oven dry back adding additives PVA carries out granulation, uses mould to obtain the cylinder shape idiosome of diameter as 13mm by the press compacting then.Place the alumina crucible of adding a cover to be put into stove the cylinder shape idiosome and carry out sintering, temperature rise rate can be controlled in 10 ℃/min.Sintering temperature is 1150 ℃, and soaking time is 2 hours, and stove is chilled to room temperature and obtains ceramics sample then.
Fig. 1 is the N of present embodiment preparation
yB
zT
94-BT
6(z/y=1.04) pyroelectric coefficient of pottery in 20-150 ℃ of scope, it has a pyroelectricity peak at 66 ℃, and its highest pyroelectric coefficient can reach 3270 * 10
-8Ccm
-2K
-1
Fig. 2 is the N of present embodiment preparation
yB
zT
94-BT
6(z/y=1.07) pyroelectric coefficient of pottery in 20-150 ℃ of scope, it has a pyroelectricity peak at 34 ℃, and its highest pyroelectric coefficient can reach 140 * 10
-8Ccm
-2K
-1
Fig. 3 is the N of present embodiment preparation
yB
zT
94-BT
6(z/y=1.09) electric field-strain curve of ceramics sample can obtain huge strain under the electric field action of 70kV/cm, its value can reach 0.48%.Although this strain has bigger hysteresis, after removing electric field, can get back to zero point.The strain that this kind material is huge can obtain important application in driving mechanism.
Embodiment 2
Select the Na of AG for use
2CO
3, Bi
2O
3, BaCO
3And TiO
2For raw material is pressed N
yB
zT
93-BT
7Chemical formula is prepared burden, confected materials uses ethanol to use zirconia ball ball milling 6 hours in ball grinder as medium, oven dry is placed in the alumina crucible through grinding, 750 ℃ of calcinings 2 hours, placing ball grinder behind the cool to room temperature again was that medium uses zirconia ball at ball grinder ball milling 6 hours once more with ethanol.Oven dry back adding additives PVA carries out granulation, uses mould to obtain the cylinder shape idiosome of diameter as 13mm by the press compacting then.Place the alumina crucible of adding a cover to be put into stove the cylinder shape idiosome and carry out sintering, temperature rise rate can be controlled in 10 ℃/min.Sintering temperature is 1150 ℃, and soaking time is 2 hours, and stove is chilled to room temperature and obtains ceramics sample then.
The N of Fig. 4 present embodiment preparation
yB
zT
93-BT
7(z/y=1.09) electric field-strain curve of ceramics sample.Can obtain the less strain curve that lags behind under the electric field action of 70kV/cm, its value can reach 0.23%.At 150 ℃, strain curve does not almost lag behind in addition, and its value still can arrive 0.21%.Show that this kind material strain is mainly the electrostriction strain, can in the high-precision displacement sensor of needs, obtain to use.
Claims (9)
1. lead-free anti-ferroelectric pottery as pyroelectricity material or strain driving material, its component is Na
yBi
zTi
(1-x)O
3 (1-x)-xBaTiO
3, i.e. N
100yB
100zT
100 (1-x)-BT
x, wherein: the value of x is 0-0.15, and the value of y is 0.30-0.50, and the value of z is 0.40-0.60,1.0≤z/y＜1.25.
2. the preparation method of the lead-free anti-ferroelectric pottery as pyroelectricity material according to claim 1 is characterized in that, by with Na
2CO
3, Bi
2O
3, BaCO
3And TiO
2For raw material carries out ball milling and precalcining according to the above ratio after the batch mixes, granulation compression moulding obtains idiosome behind secondary ball milling, at last idiosome is carried out sintering and obtains the lead-free anti-ferroelectric stupalith.
3. the preparation method of the lead-free anti-ferroelectric pottery as pyroelectricity material according to claim 2, it is characterized in that described precalcining is meant: the powder of ball milling and oven dry is placed in the alumina crucible 700-900 ℃ of calcining 1-10 hour and naturally cools to room temperature through grinding.
4. the preparation method of the lead-free anti-ferroelectric pottery as pyroelectricity material according to claim 2 is characterized in that described secondary ball milling is meant: use ethanol or water to be the powder of medium after with precalcining ball milling 2-24 hour once more.
5. the preparation method of the lead-free anti-ferroelectric pottery as pyroelectricity material according to claim 2 is characterized in that described granulating and forming is meant: oven dry back adding additives PVA carries out granulation, uses mould to obtain the cylinder shape idiosome by the press compacting then.
6. the preparation method of the lead-free anti-ferroelectric pottery as pyroelectricity material according to claim 2, it is characterized in that, described sintering is meant: with idiosome as in the middle of the alumina crucible of adding a cover, or directly idiosome is placed the alumina substrate top to carry out sintering, the sintering temperature rise rate is 5 ℃/min-30 ℃/min, sintering temperature is 1100 ℃-1250 ℃, and soaking time is 1-10 hour, cools to room temperature at last with the furnace.
7. the application method according to the described lead-free anti-ferroelectric pottery of above-mentioned arbitrary claim is characterized in that, as the pyroelectricity element of preparation infrared thermal release electric detector or the starting material of strain driver element.
8. application method according to claim 7 is characterized in that, when as the starting material of pyroelectricity element, described lead-free anti-ferroelectric pottery satisfies 1.0≤z/y≤1.15.
9. application method according to claim 7 is characterized in that, when as the starting material of strain driving material, described lead-free anti-ferroelectric pottery satisfies 1.0＜z/y＜1.25.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710172A (en) * | 2015-03-10 | 2015-06-17 | 桂林电子科技大学 | Lead-free anti-ferroelectricity high-energy storage density ceramic medium material and preparation method thereof |
| CN104944943A (en) * | 2015-05-27 | 2015-09-30 | 聊城大学 | BNT-base lead-free electrostriction material with light-emitting characteristic and preparation method thereof |
| CN105439560A (en) * | 2015-12-02 | 2016-03-30 | 陕西科技大学 | High energy density ceramic material and preparation method |
| CN111933786A (en) * | 2020-08-17 | 2020-11-13 | 东莞传晟光电有限公司 | Pyroelectric sensor and manufacturing method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921109A (en) * | 2010-09-27 | 2010-12-22 | 上海交通大学 | Lead-free anti-ferroelectric material and preparation method thereof |
-
2011
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921109A (en) * | 2010-09-27 | 2010-12-22 | 上海交通大学 | Lead-free anti-ferroelectric material and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710172A (en) * | 2015-03-10 | 2015-06-17 | 桂林电子科技大学 | Lead-free anti-ferroelectricity high-energy storage density ceramic medium material and preparation method thereof |
| CN104944943A (en) * | 2015-05-27 | 2015-09-30 | 聊城大学 | BNT-base lead-free electrostriction material with light-emitting characteristic and preparation method thereof |
| CN105439560A (en) * | 2015-12-02 | 2016-03-30 | 陕西科技大学 | High energy density ceramic material and preparation method |
| CN111933786A (en) * | 2020-08-17 | 2020-11-13 | 东莞传晟光电有限公司 | Pyroelectric sensor and manufacturing method thereof |
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