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Production method of fine-grain high-strength PMN-PZT (lead zirconate titanate) piezoelectric ceramic material

A production method and technology of piezoelectric ceramics, applied in the field of low-temperature sintered fine-grained piezoelectric materials, can solve problems such as unfavorable industrial production, complicated process, and reduced strength of ceramic materials, so as to promote ferroelectric and piezoelectric properties and grain size The effect of uniformity and reduction of synthesis temperature

Active Publication Date: 2013-09-18
SUZHOU VOCATIONAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Usually, the sintering temperature of PMN-PZT ceramic material is 1200-1260°C. Such a high temperature not only increases the volatilization of Pb, but also seriously grows the grains. High temperature sintering and large grains are especially not conducive to the preparation of multilayers with Ag electrodes and low firing. Piezoelectric Ceramics
On the other hand, the brittleness of ceramics is another major bottleneck limiting its use, which mainly comes from the low strength of ceramic grain boundaries
[0003] PMN-PZT has high piezoelectric properties and large electrostrictive properties, but when prepared by the traditional solid-state method, the sintering temperature is as high as 1200 ° C, such a high sintering temperature not only makes the stoichiometric ratio unbalanced, but also leads to crystal High sintering temperature and large grains are not conducive to the preparation of MLCC, and too large grains will seriously reduce the strength of ceramic materials and reduce the life of ceramic devices
Although special preparation techniques (such as high-energy ball milling) can reduce the grain size of ceramic materials, the complex process and high cost are not conducive to industrial production.

Method used

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  • Production method of fine-grain high-strength PMN-PZT (lead zirconate titanate) piezoelectric ceramic material
  • Production method of fine-grain high-strength PMN-PZT (lead zirconate titanate) piezoelectric ceramic material
  • Production method of fine-grain high-strength PMN-PZT (lead zirconate titanate) piezoelectric ceramic material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Ordinary ball milling prepared ceramic materials with intergranular fracture mode. According to (x)Pb(Mg1 / 3Nb2 / 3)O3-(1-x)Pb(TiyZr1-y)O3-(a)Bi2O3-(b)MnO2-(c)Nb2O5-(d)ZnO-(e) SnO2 (x = 0.37, y = 0.50) (a = b = 0.5%, c = 1%, d = e = 0.1%) formula, weigh each oxide powder with an electronic balance, and deionized water As a medium, use a planetary ball mill to mix the raw materials for 24 hours, dry the slurry at 110°C, and then heat the obtained powder at 850°C for 5 hours for pre-calcination. The pre-fired powder is ball milled for the second time, dried again, granulated with 8wt% PVA as a binder, dry-pressed at 300MPa, held at 550°C for 4 hours to debond, and then placed in a programmed temperature-controlled box furnace Carry out sintering, the sintering temperature is 950° C., and the holding time is 5 hours. The obtained ceramic sheet is polished by sandpaper, and XRD and SEM of the cross section are measured.

[0023] figure 1 It is the XRD pattern of the ceramic...

Embodiment 2

[0027] Ceramic materials with partial transgranular fracture mode were prepared by ordinary ball milling. According to (x)Pb(Mg1 / 3Nb2 / 3)O3-(1-x)Pb(TiyZr1-y)O3-(a)Bi2O3-(b)MnO2-(c)Nb2O5-(d)ZnO-(e) SnO2 (x = 0.37, y = 0.50) (a = 1%, b = 0.1%, c = d = e = 0.5%) formula, weigh each oxide powder with an electronic balance, and deionized water As a medium, use a planetary ball mill to mix the raw materials for 24 hours, dry the slurry at 110°C, and then heat the obtained powder at 850°C for 5 hours for pre-calcination. The pre-fired powder is ball-milled twice, dried again, granulated with 8wt% PVA as a binder, dry-pressed at 300MPa, held at 550°C for 4 hours to debond, and then placed in a programmed temperature-controlled box furnace Carry out sintering, the sintering temperature is 950° C., and the holding time is 5 hours. The obtained ceramic sheet is polished by sandpaper, and XRD and SEM of the cross section are measured.

[0028] Figure 4 It is the SEM spectrum of the cro...

Embodiment 3

[0030] Ceramic materials with complete transgranular fracture mode were prepared by ordinary ball milling. According to (x)Pb(Mg1 / 3Nb2 / 3)O3-(1-x)Pb(TiyZr1-y)O3-(a)Bi2O3-(b)MnO2-(c)Nb2O5-(d)ZnO-(e) SnO2 (x = 0.37, y = 0.50) (a = 1%, b = 0.5%, c = 1%, d = e = 0.8%) formula, weigh each oxide powder with an electronic balance, and Deionized water is used as the medium, and the raw materials are mixed with a planetary ball mill for 24 hours, the slurry is dried at 110°C, and then the obtained powder is kept at 850°C for 5 hours for pre-calcination. The pre-fired powder is ball-milled twice, dried again, granulated with 8wt% PVA as a binder, dry-pressed at 300MPa, held at 550°C for 4 hours to debond, and then placed in a programmed temperature-controlled box furnace Carry out sintering, the sintering temperature is 950° C., and the holding time is 5 hours. The obtained ceramic sheet is polished by sandpaper, and XRD and SEM of the cross section are measured.

[0031] Figure 5 It...

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Abstract

The invention discloses a production method of a fine-grain high-strength PMN-PZT (lead zirconate titanate) piezoelectric ceramic material. The production method comprises the following steps of: weighing raw materials including PbO, MgO, Nb2O5, TiO2, ZrO2, Bi2O3 and MnO2 in a stoichiometric ratio of (x)Pb(Mg1 / 3Nb2 / 3)O3-(1-x)Pb(TiyZr(1-y))O3-(a)Bi2O3-(b)MnO2-(c)Nb2O5-(d)ZnO-(e)SnO2, wherein x is 0.35-0.40, y is 0.40-0.70, and a, b, c, d, e are 0-1%; carrying out the process steps of ball milling, calcining, secondary ball milling, pelleting, tabletting, adhesion eliminating, sintering and the like to obtain a product. Therefore, by adopting the production method, the synthesis temperature of PMN-PZ-PT in the prior art can be greatly reduced, the compactness of a ceramic sample is high, the grain is tiny (-2 microns), the grain size is uniform, and a fracture mode realizes conversion from an intergranular fracture mode to a trans-granular fracture mode, namely the grain-boundary strength is greatly improved.

Description

technical field [0001] The invention relates to the field of low-temperature sintered fine-grain piezoelectric materials, in particular to a production method of a fine-grain high-strength PMN-PZT piezoelectric ceramic material. Background technique [0002] Usually, the sintering temperature of PMN-PZT ceramic material is 1200-1260°C. Such a high temperature not only increases the volatilization of Pb, but also seriously grows the grains. High temperature sintering and large grains are especially not conducive to the preparation of multilayers with Ag electrodes and low firing. Piezoelectric Ceramics. On the other hand, the brittleness of ceramics is another bottleneck limiting its use, which mainly comes from the low strength of ceramic grain boundaries. [0003] PMN-PZT has high piezoelectric properties and large electrostrictive properties, but when prepared by the traditional solid-state method, the sintering temperature is as high as 1200 ° C, such a high sintering te...

Claims

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Application Information

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IPC IPC(8): C04B35/493C04B35/453C04B35/495C04B35/622
Inventor 宁海霞
Owner SUZHOU VOCATIONAL UNIV
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