CN104695018A - Aluminum gallium tantalum calcium silicate piezoelectric crystal and preparing method thereof - Google Patents

Aluminum gallium tantalum calcium silicate piezoelectric crystal and preparing method thereof Download PDF

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CN104695018A
CN104695018A CN201310655381.2A CN201310655381A CN104695018A CN 104695018 A CN104695018 A CN 104695018A CN 201310655381 A CN201310655381 A CN 201310655381A CN 104695018 A CN104695018 A CN 104695018A
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crystal
piezoquartz
preparation
piezoelectric
tantalum
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熊开南
郑燕青
涂小牛
林全明
李亚乔
施尔畏
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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Priority to PCT/CN2014/082997 priority patent/WO2015081706A1/en
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/34—Silicates
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20—Controlling or regulating
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20—Controlling or regulating
    • C30B15/206—Controlling or regulating the thermal history of growing the ingot

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

An aluminum gallium tantalum calcium silicate piezoelectric crystal and a preparing method thereof are disclosed. The general chemical formula of the crystal is Ca3TaAl<3-x>GaxSi2O14, wherein 0.3<x<2.5. The crystal has a structure the same as the structure of a lanthanum gallium silicate crystal, and belongs to the space group P321 and the point group 32. The piezoelectric crystal is prepared by adoption of a Czochralski method. The piezoelectric crystal has advantages of excellent piezoelectric performance, good crystallization performance, low costs, easy production of large-size crystals, and the like, facilitates wide-range practicability of the crystal, and is expected to achieve large-scale industrial application.

Description

A kind of silicic acid gallium aluminium tantalum calcium piezoquartz and preparation method thereof
Technical field
The present invention relates to a kind of silicic acid gallium aluminium tantalum calcium piezoquartz and preparation method thereof, belong to technical field of piezoelectric materials.
Background technology
Since piezoelectric effect is found, research and the production of piezoelectric achieve great development.Piezoelectric has for wave filter, resonator, sensor device, and they are widely used in the fields such as communication, medical treatment, aerospace, electronics and information industry, detection.
Piezoquartz is the class important materials for making piezoelectric device, and current alpha-quartz relies on its excellent temperature stability, low production cost, ripe production technology and firmly in occupation of most market shares of piezoquartz.But lower (the piezoelectric strain constant d of the piezoelectric activity of alpha-quartz 11for 2.31pC/N) and there is phase transformation at 573 DEG C, so this crystal can not meet the demand for development of the technology such as modern communication and space flight completely.Conventional wave filter, resonator and be used for monitor sound wave, vibration, under the static sensor of noise signal and acoustics sensor piezoelectric device are generally applied to normal temperature condition, along with the development of modern industrial technology, automobile, national defence, the technical fields such as aerospace produce urgent demand to the piezoelectric device worked under hot environment, as to engine interior combustion chamber operational monitoring temperature and the tonometric piezoelectric device be applied in hot environment, higher requirement be it is also proposed to the piezoelectric making piezoelectric device, such as larger piezoelectric activity, phase transformation stability, higher resistivity value, the temperature stability etc. of electromechanical properties.At present conventional piezoquartz still can not meet above-mentioned new demand, thus to explore a kind of New piezoelectric crystal not only having higher pressure electrical property but also can use at relatively high temperatures be the research topic very with practical significance.
At present, LGS class (A 3bC 3d 2o 14) crystal receives and pay close attention to widely.LGS crystalloid belongs to trigonal system, 32 point groups, P321 spacer, the cation crystallographic position that A, B, C, D tetra-kinds is different is comprised in crystalline structure, wherein A position cation-bit is in the decahedron central position be made up of 8 oxonium ions, B position cation-bit is in the octahedra central position be made up of 6 oxonium ions, and C position and D position positively charged ion are in the tetrahedron central position be made up of 4 oxonium ions respectively, and positively charged ion place, D position tetrahedron is slightly less than positively charged ion place, C position tetrahedron.The crystal-like piezo-electric modulus of LGS and electromechanical coupling factor are 2 ~ 3 times of quartz crystal, there is the cut type of zero frequency temperature coefficient, and room temperature to fusing point (being greater than 1300 DEG C) without advantages such as phase transformations.Thus make this crystalloid in acoustic bulk wave and surface acoustic wave device, have bright application prospect.In recent years, this crystalloid reported comprises La 3ga 5siO 14(LGS), La 3nb 0.5ga 5.5o 14(LGN), La 3ta 0.5ga 5.5o 14(LGT), Sr 3nbGa 3si 2o 14(SNGS), Sr 3taGa 3si 2o 14(STGS), Ca 3nbGa 3si 2o 14(CNGS), Ca 3taGa 3si 2o 14(CTGS) etc.
But expensive cost of material seriously limits the crystal-like application of LGS.For exploring performance piezoquartz better with low cost, people have carried out LGS crystalloid and have studied widely.Chinese patent CN101275279A discloses C a3t aal 3si 2o 14(CTAS) crystal, this crystal adopts Al on C case 3+instead of G a 3+, due to Al 2o 3price far below Ga 2o 3, crystal cost is significantly declined, has excellent piezoelectric property simultaneously concurrently, make it in making piezoelectric device, have very strong advantage.But find in crystal growth, CTAS crystal structure is poor, is difficult to obtain non-nuclear density gauge, large-sized single crystal, thus affects promoting the use of of crystal.
Summary of the invention
The problems referred to above existed for prior art and demand, the present invention aims to provide that a kind of not only piezoelectric property is excellent, lower cost and silicic acid gallium aluminium tantalum calcium piezoquartz of crystal property excellence and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of silicic acid gallium aluminium tantalum calcium piezoquartz, its chemical general formula is Ca 3taAl (3-x)ga xsi 2o 14, wherein, 0.3 < x < 2.5(preferably 1≤x≤1.5); Described crystal has and LGS (La 3ga 5siO 14) crystalline structure that crystal is identical, belong to spacer P321, point group 32.
Wherein Ca 2+, Ta 5+, Si 4+occupy A, B, D position respectively, Al 3+and Ga 3+jointly occupy C position at random.By adjustment x value in 0.1 ~ 2.50 scope, the CTAGS crystal of different al/Ga component can be obtained; Concrete x value can be determined for the requirement of related application to crystal property.
In the present invention, when x value is 1.5, the unit cell parameters of described silicic acid gallium aluminium tantalum calcium piezoquartz is be compared to LGS piezoquartz, when piezoelectric property is not affected substantially, the production cost of CTAGS piezoquartz significantly reduces; Compared with CTGS piezoquartz, CTAGS piezoquartz not only piezoelectric property increases, and production cost reduces further; For the CTAS piezoquartz that crystal property is poor, CTAGS piezoquartz embodies the more excellent advantage of its crystal property.When x value is 1.5, the piezoelectric constant d of described silicic acid gallium aluminium tantalum calcium piezoquartz 11for 4.4pC/N, be respectively 6.6 × 10 at the high-temperature resistivity ρ of 500 DEG C, 600 DEG C, 700 DEG C 8Ω cm, 7.6 × 10 7Ω cm, 1.5 × 10 7Ω cm, its resistivity is higher than LGS, CTGS and CTAS crystal under uniform temp, and lg ρ and 1/T is linear, meets Arrhenius experimental formula.
The preparation method of silicic acid gallium aluminium tantalum calcium piezoquartz of the present invention is pulling growth method, comprises following operation steps:
A) by Ca 3taAl (3-x)ga xsi 2o 14stoichiometric ratio take CaCO 3, Ta 2o 5, Al 2o 3, Ga 2o 3and SiO 2each powder, briquetting after mixing, then sinters, obtains Ca at 1200 ~ 1300 DEG C 3taAl (3-x)ga xsi 2o 14polycrystal;
B) by CTGS seed crystal and step a) in the polycrystal that obtains load in crucible, 1300 ~ 1500 DEG C are heated to the temperature rise rate of 150 ~ 250 DEG C/h, after polycrystal fusing, insulation makes melt state stablize, then temperature of sowing is cooled to, start to carry out crystal growth: controlling rotating speed is 2 ~ 20 revs/min, pull rate is 0.1 ~ 5 milli m/h;
C) crystal is departed from melt after terminating by growth, and crystal is cooled to room temperature.
As a kind of preferred version, step b) in heating mode be adopt medium frequency induction power supply heating.
As a kind of preferred version, step b) described in crucible be platinum crucible or iridium crucible.
As a kind of preferred version, step b) in pull rate be 0.1 ~ 1 milli m/h.
As a kind of preferred version, step c) in rate of temperature fall be 20 ~ 100 DEG C/h.
Compared with prior art, silicic acid gallium aluminium tantalum calcium piezoquartz provided by the present invention has excellent piezoelectric property, good crystal property, lower cost concurrently, is easy to the advantages such as growing large-size crystal, be conducive to the extensively practical of crystal, be expected to obtain heavy industrialization application.
Accompanying drawing explanation
Fig. 1 is embodiment 1 gained CTAGS crystallogram;
Fig. 2 is the X-ray rocking curve collection of illustrative plates (X sheet cut type) of embodiment 1 gained CTAGS crystal;
Fig. 3 is the resistivity of embodiment 1 gained CTAGS, CTGS and CTAS crystal and the relation curve comparison diagram of temperature.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.
Embodiment 1
As x=1.5, adopt Czochralski grown crystal Ca 3taAl 1.5ga 1.5si 2o 14,
6CaCO 3+Ta 2O 5+1.5Al 2O 3+1.5Ga 2O 3+4SiO 2=2Ca 3TaAl 1.5Ga 1.5Si 2O 14；
The CaCO that purity is 99.99% is taken by above-mentioned chemical equation 3, Ta 2o 5, Al 2o 3, Ga 2o 3and SiO 2each raw material, is pressed into the nahlock that diameter is 70mm after sufficiently mixing, then sinters 24 hours at 1300 DEG C, obtains Ca 3taAl 1.5ga 1.5si 2o 14polycrystal.
Adopt Frequency Induction Heating lifting furnace to carry out crystal growth, first polycrystal and CTGS seed crystal are placed in Iridium Crucible, with N 2as shielding gas; being warming up to 1460 DEG C through 6 hours makes polycrystal melt; be incubated the temperature of sowing being cooled to 1410 DEG C after making Melt Stability in 5 hours, start to carry out crystal growth, in process of growth; with the rotating speed seeding shouldering of 10rpm to required diameter; turn shoulder after with the pull rate isodiametric growth of 0.5mm/h to 80mm, stop lift, by crystal lift to departing from melt; be down to room temperature by the rate of temperature fall of 40 DEG C/h again, finally obtain Ca 3taAl 1.5ga 1.5si 2o 14crystal.
The photo of gained CTAGS crystal as shown in Figure 1, as seen from Figure 1: plane of crystal is comparatively fine and close.
Fig. 2 is the X-ray rocking curve collection of illustrative plates (X sheet cut type) of gained CTAGS crystal, as seen from Figure 2: gained CTAGS crystal structure quality is better, there is not low angle boundary or twin crystal defect.
Fig. 3 is the resistivity of gained CTAGS, CTGS and CTAS crystal and the relation curve comparison diagram of temperature, as seen from Figure 3: gained CTAGS crystal has excellent temperature stability.
Wherein, preparation method's reference literature of CTGS crystal and CTAS crystal: Solid State Commun.150 (2010) 435-438.
The present embodiment gained Ca 3taAl 1.5ga 1.5si 2o 14the unit cell parameters of crystal, piezoelectric constant and high-temperature resistivity data ginseng is shown in Table 1.
The partial properties parameter of each crystal of table 1
From table 1: gained crystal has the crystalline structure identical with callium-lanthanum silicate crystal.
Embodiment 2
As x=2, adopt Czochralski grown Ca 3taAlGa 2si 2o 14crystal;
6CaCO 3+Ta 2O 5+Al 2O 3+2Ga 2O 3+4SiO 2=2Ca 3TaAlGa 2Si 2O 14；
The CaCO that purity is 99.99% is taken by above-mentioned chemical equation 3, Ta 2o 5, Al 2o 3, Ga 2o 3and SiO 2each raw material, is pressed into the nahlock that diameter is 70mm after sufficiently mixing, then sinters 20 hours at 1300 DEG C, obtains Ca 3taAlGa 2si 2o 14polycrystal.
Adopt Frequency Induction Heating lifting furnace to carry out crystal growth, first polycrystal and CTGS seed crystal are placed in Iridium Crucible, with N 2as shielding gas; being warming up to 1450 DEG C through 6 hours makes polycrystal melt; be incubated the temperature of sowing being cooled to 1400 DEG C after making Melt Stability in 5 hours, start to carry out crystal growth, in process of growth; with the rotating speed seeding shouldering of 8rpm to required diameter; turn shoulder after with the pull rate isodiametric growth of 0.8mm/h to 80mm, stop lift, by crystal lift to departing from melt; be down to room temperature by the rate of temperature fall of 50 DEG C/h again, finally obtain Ca 3taAlGa 2si 2o 14crystal.
Gained crystal has crystalline structure described in embodiment 1 and crystal property and piezoelectric property.
Embodiment 3
As x=0.4, adopt Czochralski grown Ca 3taAl 2.6ga 0.4si 2o 14crystal;
6CaCO 3+Ta 2O 5+2.6Al 2O 3+0.4Ga 2O 3+4SiO 2=2Ca 3TaAl 2.6Ga 0.4Si 2O 14；
The CaCO that purity is 99.99% is taken by above-mentioned chemical equation 3, Ta 2o 5, Al 2o 3, Ga 2o 3and SiO 2each raw material, is pressed into the nahlock that diameter is 70mm after sufficiently mixing, then sinters 30 hours at 1300 DEG C, obtains Ca 3taAl 2.6ga 0.4si 2o 14polycrystal.
Adopt Frequency Induction Heating lifting furnace to carry out crystal growth, first polycrystal and CTGS seed crystal are placed in Iridium Crucible, with N 2as shielding gas; being warming up to 1490 DEG C through 6.5 hours makes polycrystal melt; be incubated the temperature of sowing being cooled to 1450 DEG C after making Melt Stability in 5 hours, start to carry out crystal growth, in process of growth; with the rotating speed seeding shouldering of 6rpm to required diameter; turn shoulder after with the pull rate isodiametric growth of 0.4mm/h to 80mm, stop lift, by crystal lift to departing from melt; be down to room temperature by the rate of temperature fall of 30 DEG C/h again, finally obtain Ca 3taAl 2.6ga 0.4si 2o 14crystal.
Gained crystal has crystalline structure described in embodiment 1 and crystal property and piezoelectric property.
Finally be necessary described herein: above embodiment is only for being described in more detail technical scheme of the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.

Claims (7)

1. a silicic acid gallium aluminium tantalum calcium piezoquartz, is characterized in that: its chemical general formula is Ca 3taAl (3-x)ga xsi 2o 14, wherein, 0.3 < x < 2.5; Described crystal has the crystalline structure identical with callium-lanthanum silicate crystal, belongs to spacer P321, point group 32.
2. silicic acid gallium aluminium tantalum calcium piezoquartz as claimed in claim 1, is characterized in that: 1≤x≤1.5.
3. a preparation method for silicic acid gallium aluminium tantalum calcium piezoquartz as claimed in claim 1 or 2, is characterized in that: be pulling growth method.
4. preparation method as claimed in claim 3, is characterized in that, comprise following operation steps:
A) by Ca 3taAl (3-x)ga xsi 2o 14stoichiometric ratio take CaCO 3, Ta 2o 5, Al 2o 3, Ga 2o 3and SiO 2each powder, briquetting after mixing, then sinters, obtains Ca3TaAl at 1200 ~ 1300 DEG C (3-x)ga xsi 2o 14polycrystal;
B) by CTGS seed crystal and step a) in the polycrystal that obtains load in crucible, 1300 ~ 1500 DEG C are heated to the temperature rise rate of 150 ~ 250 DEG C/h, after polycrystal fusing, insulation makes melt state stablize, then temperature of sowing is cooled to, start to carry out crystal growth: controlling rotating speed is 2 ~ 20 revs/min, pull rate is 0.1 ~ 5 milli m/h;
C) crystal is departed from melt after terminating by growth, and crystal is cooled to room temperature.
5. preparation method as claimed in claim 4, is characterized in that: step b) in heating mode be adopt medium frequency induction power supply heating.
6. preparation method as claimed in claim 4, is characterized in that: step b) described in crucible be platinum crucible or iridium crucible.
7. preparation method as claimed in claim 4, is characterized in that: step c) in rate of temperature fall be 20 ~ 100 DEG C/h.
CN201310655381.2A 2013-12-05 2013-12-05 Aluminum gallium tantalum calcium silicate piezoelectric crystal and preparing method thereof Pending CN104695018A (en)

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PCT/CN2014/082997 WO2015081706A1 (en) 2013-12-05 2014-07-25 Calcium tantalum gallium aluminum silicate piezoelectric crystal and method of preparing same

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CN106480501A (en) * 2015-08-27 2017-03-08 中国科学院上海硅酸盐研究所 A kind of gallium silicate niobium calcium piezo-electric crystal and preparation method thereof
WO2017146244A1 (en) * 2016-02-25 2017-08-31 株式会社Ｃ＆Ａ Crystal material and method for producing same
CN109428257A (en) * 2017-09-01 2019-03-05 中国科学院福建物质结构研究所 The silicate crystal and its 1.5 micron waveband laser devices of erbium ion doping
CN114815222A (en) * 2022-02-25 2022-07-29 上海科技大学 Biaxial micro-reflector based on piezoelectric film
WO2024036655A1 (en) * 2022-08-17 2024-02-22 山东大学 Effective nonlinear optical coefficient optimization method for lanthanum gallium silicate solid solution crystal

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CN114815222A (en) * 2022-02-25 2022-07-29 上海科技大学 Biaxial micro-reflector based on piezoelectric film
CN114815222B (en) * 2022-02-25 2023-09-26 上海科技大学 Double-shaft micro-mirror based on piezoelectric film
WO2024036655A1 (en) * 2022-08-17 2024-02-22 山东大学 Effective nonlinear optical coefficient optimization method for lanthanum gallium silicate solid solution crystal

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