CN108046802A - A kind of preparation method of superelevation Curie temperature piezoceramic material - Google Patents
A kind of preparation method of superelevation Curie temperature piezoceramic material Download PDFInfo
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Abstract
The invention discloses a kind of perovskite-like structure lanthanium titanate La2Ti2O7（LTO）The preparation method of piezoceramic material its main feature is that this method prepares LTO precursor powders using sol-gal process first, reuses ordinary sinter method and prepares LTO piezoelectric ceramics.By sol-gal process and the united mode of ordinary sinter method, the technology of preparing of LTO ceramics is optimized, the sintering temperature of LTO ceramics is not only reduced, also improves the electric property of LTO ceramics to a certain extent, it is made to be expected to play a significant role in superhigh temperature field.
Description
Technical field
The present invention relates to a kind of superelevation Curie temperature perovskite-like structure lanthanium titanate La2Ti2O7（LTO）Piezoceramic material
Preparation method, i.e., first prepare LTO precursor powders with sol-gal process, then be sintered at 1350 ~ 1550 DEG C with ordinary sinter method
6 ~ 12 are made LTO piezoelectric ceramic wafers when small.The invention belongs to Materials Science and Engineering fields.
Background technology
High-temperature piezoelectric sensing technology is in chemistry, material processing, automation, aerospace（Such as the electronics in jet engines
Device needs the service life in the case of bearing 500 ~ 1000 DEG C of high temperature to also need to 100000 more than h）And the row such as oil exploration
Industry has important application.At present, Curie temperatureT c There is LiNbO more than 650 DEG C of material3 (T c = 1150 ℃)、LiTaO3
(T c = 720 ℃)、Aurivillius phases（It is represented as Bi4Ti3O12 ( Tc=675 DEG C), perovskite-like PLS（Generation
Table is Sr2Nb2O7 (T c = 1342 ℃).Due to LiNbO3With LiTaO3Because electrical conductivity is high under its high temperature, can only less than
300 DEG C of uses；The improved Bi stratified materials of Aurivilius phase also can only be used for piezoelectricity application at 500 DEG C.Only PLS
Can be used above at 1000 DEG C, and can be used under high vacuum, strong electron bombardment environment.But perovskite-like PLS materials need
Fine and close polycrystal could be obtained under conditions of high temperature and pressure.In recent years, it is main to the research of PLS high-temperature piezoelectric materials
In terms of concentrating on polycrystalline ceramics, have a certain number of document reports and differently prepare with good piezoelectric performance
PLS materials.Ali Ceylan in 2008 prepare LTO ceramics with hot forging method and its mechanical performance are characterized；2011
Rajesh V. Pai etc. prepare homogeneous sample Nd with gel embedding technology2-xLixTi2O7-δ(x=0,0.1,0.15), 800
The compound of 6 H-shaped Cheng Chun, no piezoelectric property are burnt at DEG C；Aslihan Orum in 2016 etc. prepare La with molten-salt growth method2Ti2O7
Ceramics；N. Zhang in 2015 etc. prepare dielectric constant with solid phase methodε r ~ 57, crystallite dimension ~ 1.8-2.5 μm
La2Ti2O7Ceramics；Z.P. Gao in 2013 etc. prepare piezoelectric ceramics La with solid phase method and SPS methods2−xCexTi2O7 (x =
0.15, 0.25, 0.35)；Chen Chen in 2016 etc. prepare (A with SPS two-step sintering methodsxLa1 – x)2Ti2O7 (A =
Sm and Eu) piezoelectric ceramics, obtain (Sm0.1La0.9)2Ti2O7Piezoelectric constantd 33 =2.8 pC/N；Haixue Yan in 2009
Nd is prepared Deng with solid phase method, coprecipitation combination SPS2Ti2O7、La2Ti2O7Piezoelectric ceramics, piezoelectric constant are respectively 0.6 pC/
N、2.6 pC/N；Ruhollah Talebi in 2016 etc. prepare La with sol-gal process2Ti2O7Nanometer powder.2015
It is about 95 % that Zhipeng Gaoa etc. prepare relative density with molten-salt growth method, TGG methods, slip casting and magnetic field alignment method,
Crystal grain diameter is the LTO ceramics that 4 ~ 5 μ m thicks are 0.5 μm.Due to PLS single crystal preparations are difficult, requirement is high, time-consuming and into
This height, therefore it is more to explore synthesis PLS polycrystalline methods at present：It polymerize replica, urea precipitation method, hydrothermal synthesis method, co-precipitation
Method, metal-organic decomposition method, solution hybrid technology, solid phase method, sol-gal process, plasma spark sintering process (SPS), template
Crystal grain method (TGG), slip casting, magnetic field alignment method, molten-salt growth method, gel embedding technology, epitaxial growth method, hot forging etc..At present
Not useful ordinary sinter forms the report of the LTO ceramic materials with piezoelectric property.
The content of the invention
The present invention relates to a kind of perovskite-like structure lanthanium titanate La of high-curie temperature2Ti2O7（LTO）Piezoceramic material
Preparation method.The technology of preparing of LTO piezoelectric ceramics is the method improve, sintering requirement is not only reduced, also to a certain degree
On improve the electric properties of LTO ceramics.
A kind of perovskite-like structure lanthanium titanate La2Ti2O7（LTO）The sintering method of piezoceramic material is characterized in that system
Standby technique contains following steps：
(1) sol-gal process prepares LTO ceramics precursor powders
Raw material is pressed into La2Ti2O7Molar fraction carry out dispensing, using La (NO3)3、C16H36O4Ti, anhydrous citric acid are raw material,
According to La (NO3)3：C16H36O4Ti：Anhydrous citric acid=1：0.5~2.2：5 ~ 15 are prepared into LTO into colloidal sol, are put into 90 DEG C of baking
Baking obtains LTO gels after 5 ~ 10 days in case, be sintered with ordinary sinter stove at 1000 ~ 1300 DEG C 2 ~ 6 it is small when formation LTO before
Drive body powder.
(2) it is granulated tabletting
It adds in after the poly-vinyl alcohol solution that concentration is 5 ~ 10wt% is sufficiently mixed and is granulated in the powder of above-mentioned drying, then
10 ~ 15 mm of diameter is pressed into the case where pressure is 16 ~ 20 MPa, the LTO ceramic disks that thickness is 0.6 ~ 1.2 mm.
(3) dumping is sintered
By above-mentioned LTO ceramic disks in 700~950 DEG C of 5 ~ 12 h of dumping, then with ordinary sinter method in temperature 1350 ~ 1550
DEG C sintering 6 ~ 12 it is small when LTO ceramic disks are made.
(4) surface metalation and polarization
The LTO ceramic disks surface obtained after above-mentioned sintering is polished to after 0.5 ~ 0.8 mm and paints platinum slurry again, then 900 ~
1100 DEG C sintering 15 minutes after sample is made.Sample is put into 180 ~ 250 DEG C of silicone oil bath and is polarized, Polarization field strength is
Perovskite-like structure lanthanium titanate LTO piezoelectric ceramics is made in 15 ~ 20 kV/mm, dwell time 30min.
Structural characterization and performance test：
1 has carried out phase structure analysis using X-ray diffractometer (XRD, DX-1000) to LTO ceramic disks；
2 carry out refine with Maud softwares to XRD spectrum obtains phase composition different in LTO；
3 draw the cell configuration figure of each phase using Diamond softwares；
4 observe the surface topography of LTO ceramic disks using electron microscope (SEM, JSM-5900)；
5 have obtained the distribution situation of each element in LTO using EDS power spectrums；
6 utilized 33 Piezoelectricity tester (ZJ-3A) tests LTO piezoelectric ceramic wafersd 33 ；
7 use high-temperature resistivity tester（One hundred power wins HRMS-900）Measure the resistivity of LTO piezoelectric ceramics.
Test result is shown in Fig. 1 ~ 7.The result shows that it is pure perovskite using LTO piezoelectric ceramics prepared by the method for the present invention
Structure, monocline coexist with orthorhombic phase；It is imperforate ceramic layered to obtain surface compact, largest grain size reaches 150 μm of left sides
It is right；La, Ti, O being evenly distributed in ceramic LTO, constituent content La:Ti=18.14:18.43, the La with design:Ti=1:More than 1
It is consistent；In the piezoelectric constant of 1495 DEG C or more the LTO being sintered ceramics>2 pC/N, maximum piezoelectric constantd 33 = 2.7 pC/
N；Permittivity εr~ 72, dielectric loss tg<2 %.LTO ceramics at 650 DEG C resistivity up to 1.12 × 107 Ω·cm。
The present invention compared with prior art, has the following advantages that.
1st, the LTO ceramics precursor powder activation energy biggers prepared with sol-gal process reduce the required superelevation of LTO ceramics
Sintering temperature can be used ordinary sinter method and prepare fine and close LTO ceramics.
, with ordinary sinter method prepare LTO piezoelectric ceramics, electric property can with is prepared with SPS sintering process LTO pottery
The performance of porcelain compares favourably.Two-phase coexistent and larger crystallite dimension contribute to the formation of electricdomain in LTO ceramics, have and obtain
The potential of more preferable electric property.
Description of the drawings
Fig. 1 is the X ray diffracting spectrum of perovskite-like structure lanthanium titanate LTO piezoceramic materials.
Fig. 2 is the powder choiceness figure of perovskite-like structure lanthanium titanate LTO piezoceramic materials
Fig. 3 is the crystal structure figure of perovskite-like structure lanthanium titanate LTO piezoceramic materials
Fig. 4 is the stereoscan photograph of perovskite-like structure lanthanium titanate LTO piezoceramic materials（SEM）, left-half is surface
Pattern, right half part are cross-section morphology.
Fig. 5 is the EDS distribution diagram of element of perovskite-like structure lanthanium titanate LTO piezoceramic materials
Fig. 6 is the resistivity map of perovskite-like structure lanthanium titanate LTO piezoceramic materials
Fig. 7 is the dielectric properties of perovskite-like structure lanthanium titanate LTO piezoceramic materials.
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that the present embodiment is served only for
The present invention is further described, it is impossible to be interpreted as limiting the scope of the invention, the person skilled in the art in the field
Some nonessential modifications and adaptations can be made according to the content of the invention described above.
Embodiment
(1) sol-gal process prepares LTO ceramics precursor powders
Raw material is pressed into La2Ti2O7Molar fraction carry out dispensing, using La (NO3)3、C16H36O4Ti, anhydrous citric acid are raw material,
According to La (NO3)3：C16H36O4Ti：Anhydrous citric acid=1：0.5~2.2：5 ~ 15 are prepared into LTO into colloidal sol, are put into 90 DEG C of baking
Baking obtains LTO gels after 5 ~ 10 days in case, be sintered with ordinary sinter stove at 1000 ~ 1300 DEG C 2 ~ 6 it is small when formation LTO before
Drive body powder.
(2) it is granulated tabletting
It adds in after the poly-vinyl alcohol solution that concentration is 5 ~ 10wt% is sufficiently mixed and is granulated in the powder of above-mentioned drying, then
10 ~ 15 mm of diameter is pressed into the case where pressure is 16 ~ 20 MPa, the LTO ceramic disks that thickness is 0.6 ~ 1.2 mm.
(3) dumping is sintered
By above-mentioned LTO ceramic disks in 700~950 DEG C of 5 ~ 12 h of dumping, then with ordinary sinter method in 1515 DEG C of sintering of temperature
6 ~ 12 are made LTO ceramic disks when small.
(4) surface metalation and polarization
The LTO ceramic disks surface obtained after above-mentioned sintering is polished to after 0.5 ~ 0.8 mm and paints platinum slurry again, then 900 ~
1100 DEG C sintering 15 minutes after sample is made.Sample is put into 180 ~ 250 DEG C of silicone oil bath and is polarized, Polarization field strength is
15 ~ 20 kV/mm, dwell time are 30 min, and perovskite-like structure lanthanium titanate LTO piezoelectric ceramics is made.
Claims (6)
1. a kind of perovskite-like structure lanthanium titanate La2Ti2O7（LTO）The preparation method of piezoceramic material, using following steps into
It is prepared by row：
(1) sol-gal process prepares LTO ceramics precursor powders
Raw material is pressed into La2Ti2O7Molar fraction carry out dispensing, using La (NO3)3、C16H36O4Ti, anhydrous citric acid are raw material,
According to La (NO3)3：C16H36O4Ti：Anhydrous citric acid=1：0.5~2.5：5 ~ 15 are prepared into LTO into colloidal sol, are put into 90 DEG C of baking
Baking obtains LTO gels after 5 ~ 10 days in case, be sintered with ordinary sinter stove at 1000 ~ 1300 DEG C 2 ~ 6 it is small when formation LTO before
Drive body powder.
2. (2) it is granulated tabletting
It adds in after the poly-vinyl alcohol solution that concentration is 5 ~ 10 wt% is sufficiently mixed and is granulated in the powder of above-mentioned drying, then
10 ~ 15 mm of diameter is pressed into the case where pressure is 16 ~ 20 MPa, the LTO ceramic disks that thickness is 0.6 ~ 1.2 mm.
3. (3) dumping is sintered
By above-mentioned LTO ceramic disks in 700~950 DEG C of 5 ~ 12 h of dumping, then with ordinary sinter method in temperature 1350 ~ 1550
DEG C sintering 6 ~ 12 it is small when LTO ceramic disks are made.
4. (4) surface metalation and polarization
The LTO ceramic disks surface obtained after above-mentioned sintering is polished to after 0.5 ~ 0.8 mm and paints platinum slurry again, then 900 ~
1200 DEG C sintering 15 minutes after sample is made.
It polarizes 5. sample is put into 180 ~ 250 DEG C of silicone oil bath, Polarization field strength is 15 ~ 20 kV/mm, and the dwell time is
LTO piezoelectric ceramics is made in 30 min.
6. perovskite-like structure lanthanium titanate LTO piezoelectric ceramics as described in claim 1, piezoelectric constant, can up to 2.7 pC/N
Prestige is widely used in superhigh temperature field.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112313808A (en) * | 2018-06-21 | 2021-02-02 | 爱奥尼克斯先进科技有限公司 | Method for annealing polarized ceramics |
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| CN105957958A (en) * | 2016-05-04 | 2016-09-21 | 中国工程物理研究院流体物理研究所 | La2Ti2O7 or solid solution material application in high temperature piezoelectric transducer and prepared transducer |
| CN106518071A (en) * | 2016-09-27 | 2017-03-22 | 四川大学 | High-curie temperature and high-temperature stability piezoceramic material as well as preparation method and application thereof |
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2018
- 2018-01-05 CN CN201810011358.2A patent/CN108046802A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105957958A (en) * | 2016-05-04 | 2016-09-21 | 中国工程物理研究院流体物理研究所 | La2Ti2O7 or solid solution material application in high temperature piezoelectric transducer and prepared transducer |
| CN106518071A (en) * | 2016-09-27 | 2017-03-22 | 四川大学 | High-curie temperature and high-temperature stability piezoceramic material as well as preparation method and application thereof |
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| A. V. PRASADARAO等: "Sol-gel synthesis of Ln2(Ln=La,Nd)Ti2O7", 《JOURNAL OF MATERIALS RESEARCH》 * |
| LI SUN等: "Room-temperature ferromagnetism and ferroelectricity of nanocrystalline La2Ti2O7", 《JOURNAL OR ALLOYS AND COMPOUNDS》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112313808A (en) * | 2018-06-21 | 2021-02-02 | 爱奥尼克斯先进科技有限公司 | Method for annealing polarized ceramics |
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Application publication date: 20180518 |