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Method for preparing high performance piezoelectric ceramics by reactive solid phase growth

A piezoelectric ceramic, high-performance technology, applied in the field of functional material preparation, can solve the problems of cumbersome production process, difficult preparation of PMNT single crystal, easy introduction of impurities and energy consumption

Active Publication Date: 2016-04-27
江阴智产汇知识产权运营有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Since the early 1960s, people have studied niobate ((K,Na)NbO 3 , NKN)-based lead-free piezoelectric ceramics with perovskite structure; the traditional preparation process of NKN-based ceramics includes two crushing (or ball milling) and two heat treatments of calcination and sintering. The production process is cumbersome, easy to introduce impurities and energy consumption At the same time, because Na and K are volatile, it is generally necessary to adopt methods such as hot pressing and spark plasma sintering to obtain dense NKN-based ceramics; therefore, in order to optimize the preparation process of NKN-based ceramics and improve the pressure of NKN-based ceramics In order to achieve high performance of NKN-based ceramics, it is necessary to develop new ideas
[0004] With Pb(Mg 1 / 3 Nb 2 / 3 )O 3 -PbTiO 3 The successful development of the relaxor ferroelectric single crystal represented by (PMNT) has been called "an exciting breakthrough" in the field of ferroelectricity in the past 50 years; the high performance of PMNT single crystal has guided the new direction of material preparation - pressure The single crystallization of electrical materials is expected to improve the piezoelectric properties of materials; however, due to the complex composition of relaxor ferroelectric single crystals, there is competition between the two phases of perovskite and pyrochlore during melt crystallization, and the high-temperature melt of PbO has great influence on the piezoelectric properties of materials. Pt crucibles will be severely corroded, and the composition segregation, phase transition and domain transition near the best-performing quasi-isomorphic phase boundary (MPB) are more sensitive, making it difficult to prepare large-sized PMNT single crystals

Method used

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  • Method for preparing high performance piezoelectric ceramics by reactive solid phase growth
  • Method for preparing high performance piezoelectric ceramics by reactive solid phase growth
  • Method for preparing high performance piezoelectric ceramics by reactive solid phase growth

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] According to the chemical formula 0.925 (Na 0.48 K 0.52 )NbO 3 -0.05Li(Ta 0.35 Sb 0.65 )O 3 -0.025(Na 1 / 2 Bi 1 / 2 )TiO 3 (NKN-LTS-NBT) Carbonate Na required for metering ratio weighing 2 CO 3 , K 2 CO 3 , Li 2 CO 3 And oxide Nb 2 O 5 , Sb 2 O 3 , Ta 2 O 5 , Bi 2 O 3 Raw materials, the above-mentioned raw materials are uniformly mixed through a traditional wet process, and 1.5 wt% of the total weight of the raw materials is added for granulation of polyvinyl alcohol (PVA).

[0023] Cut with [110] 0.69Pb(Mg 1 / 3 Nb 2 / 3 )O 3 -0.31PbTiO 3 (0.69PMN-0.31PT) The single crystal is used as the template, and the single crystal template is pressed together with the granulated raw material mixture under a pressure of 300MPa to prepare a ceramic blank ( figure 1 ).

[0024] No pre-synthesis process is required. The NKN-LTS-NBT textured lead-free piezoelectric ceramics are prepared by the reactive solid phase growth process. The reactive solid phase growth process conditions depend on the com...

Embodiment 2

[0026] According to chemical formula 1molCuO% doping (CuO doping amount is 0.95(Na 0.5 K 0.5 )NbO 3 -0.05Li(Ta 0.5 Sb 0.5 )O 3 1mol%) 0.95(Na 0.5 K 0.5 )NbO 3 -0.05Li(Ta 0.5 Sb 0.5 )O 3 (NKN-LTS) Carbonate Na required for metering ratio weighing 2 CO 3 , K 2 CO 3 , Li 2 CO 3 And oxide CuO, Nb 2 O 5 , Sb 2 O 3 , Ta 2 O 5 Raw material: [001] cut type 0.69PMN-0.31PT single crystal as template; reaction solid phase growth conditions: air atmosphere, 1020 ℃ reaction solid phase growth for 10 hours, other process conditions are the same as in Example 1.

Embodiment 3

[0028] According to the chemical formula 1wt%Li 2 CO 3 , CeO 2 Or La 2 O 3 Doping (doping amount is 0.75BaTiO 3 -0.15CaTiO 3 -0.1BaZrO 3 1wt% of mass) 0.75BaTiO 3 -0.15CaTiO 3 -0.1BaZrO 3 (BT-CT-BZ) Carbonate BaCO required for metering ratio weighing 3 , CaCO 3 And oxide ZrO 2 , TiO 2 And Li 2 CO 3 , CeO 2 Or La 2 O 3 One of them is used as a raw material; solid-phase reaction conditions: air atmosphere, 1480-1520℃ solid-phase reaction for 2h; because the solid-phase reaction temperature is too high, PMNT single crystal template cannot be used temporarily, and other process conditions are the same as those in Example 1. .

[0029] The NKN-based and BT-based ceramics prepared by reactive solid-phase growth are ground and polished to obtain a smooth and parallel surface; the ceramic structure is determined by XRD, and XRD measurement shows that [110] cut 0.69PMN-0.31PT single crystal is Template, the NKN-LTS-NBT ceramic prepared by reactive solid-phase growth presents a relatively p...

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Abstract

The invention belongs to the technical field of functional material preparation. The single-crystal or textured leadless piezoelectric ceramic is prepared by a reaction solid-phase growth technology, a pre-synthesis process is saved, the formation of pyrochlore phase is suppressed, the ceramic density is increased, and the electrical performance is improved; meanwhile, the problems of difficult growth, high cost and long cycle of a piezoelectric single crystal are solved; and (K, Na)NbO3(NKN)-based leadless piezoelectric ceramic with high density and good electrical performance is obtained.

Description

Technical field [0001] The invention belongs to the technical field of functional material preparation; the single-crystal or textured lead-free piezoelectric ceramics are prepared by a reactive solid phase growth process, so as to omit the pre-synthesis process, inhibit the formation of pyrochlore phase, increase the ceramic density, and improve the electrical properties. Solve the problems of piezoelectric single crystal growth, high cost, and long cycle; obtain (K,Na)NbO with higher density and good electrical properties 3 (NKN)-based lead-free piezoelectric ceramics. Background technique [0002] With the promotion of environmental protection awareness and the deepening of the concept of sustainable development, the development of environmentally compatible, high-performance lead-free piezoelectric materials to replace lead zirconate titanate (PbZrO 3 -PbTiO 3 , PZT)-based piezoelectric ceramics have become a subject of important scientific significance in the field of dielect...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/495C04B35/468C04B35/622
Inventor 方必军钱昆丁建宁罗豪甦
Owner 江阴智产汇知识产权运营有限公司