A kind of preparation method of micron flaky lead zirconate titanate crystal

A lead zirconate titanate, flake-shaped technology, applied in the field of piezoelectric ceramics, can solve the problems of high success rate and strong stability, and achieve the effect of high orientation degree and large diameter-thickness ratio

Active Publication Date: 2020-10-27
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In summary, the prior art lacks a preparation method of flaky lead zirconate titanate crystals. The preparation process has strong stability and a high success rate, and it can be used as a lead zirconate titanate textured ceramic with a high degree of orientation. seed crystal

Method used

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  • A kind of preparation method of micron flaky lead zirconate titanate crystal
  • A kind of preparation method of micron flaky lead zirconate titanate crystal
  • A kind of preparation method of micron flaky lead zirconate titanate crystal

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Preparation of flake PbBi 4 Ti 4 o 15 Precursor.

[0030] Strictly according to PbO: Bi 2 o 3 : TiO 2 =1:2:4 molar ratio ingredients, weigh PbO (purity: 99.9%) 2.2342g, Bi 2 o 3 (Purity: 99%) 9.4133g, TiO 2 (purity: 99.8%) 3.2024g, dry after ball milling and mixing 12h under dehydrated ethanol medium; Add flux KCl (purity: 99.5%) 14.9245g in the mixed material after drying again, under dehydrated ethanol medium Dry after magnetic stirring for 4 hours; then put the material after the second drying in Al 2 o 3 In the crucible, cover it, keep it warm at 1050°C for 2h, and then lower it to room temperature, with a heating rate of 2°C / min and a cooling rate of 2°C / min; the burnt product after the reaction is repeatedly washed and filtered in hot deionized water until it is used AgNO 3 The reagent detects the filtrate, and Cl cannot be detected in the filtrate - , the washing is completed; finally, the cleaned powder is dried to obtain the required PbBi 4 Ti 4 o...

Embodiment 2

[0033] Preparation of flake PbBi 4 Ti 4 o 15 Precursor.

[0034] Strictly according to PbO: Bi 2 o 3 : TiO 2 =1:2:4 molar ratio ingredients, weigh PbO (purity: 99.9%) 2.2342g, Bi 2 o 3 (Purity: 99%) 9.4133g, TiO 2 (purity: 99.8%) 3.2024g, dry after ball milling and mixing 12h under dehydrated ethanol medium; Add flux KCl (purity: 99.5%) 14.9245g in the mixed material after drying again, under dehydrated ethanol medium Dry after magnetic stirring for 4 hours; then put the material after the second drying in Al 2 o 3 In the crucible, cover it, keep it warm at 1000°C for 2h, and then lower it to room temperature with a heating rate of 2°C / min and a cooling rate of 2°C / min; the burnt product after the reaction is repeatedly washed and filtered in hot deionized water until it is used AgNO 3 The reagent detects the filtrate, and Cl cannot be detected in the filtrate — , the washing is completed; finally, the cleaned powder is dried to obtain the required PbBi 4 Ti 4 o ...

Embodiment 3

[0036] Preparation of flake PbBi 4 Ti 4 o 15 Precursor.

[0037] Strictly according to PbO: Bi 2 o 3 : TiO 2 =1:2:4 molar ratio ingredients, weigh PbO (purity: 99.9%) 2.2342g, Bi 2 o 3 (Purity: 99%) 9.4133g, TiO 2 (purity: 99.8%) 3.2024g, dry after ball milling and mixing 12h under dehydrated ethanol medium; Add flux KCl (purity: 99.5%) 14.9245g in the mixed material after drying again, under dehydrated ethanol medium Dry after magnetic stirring for 4 hours; then put the material after the second drying in Al 2 o 3 In the crucible, cover it, keep it warm at 1100°C for 2h, then lower it to room temperature, the heating rate is 2°C / min, the cooling rate is 2°C / min; the burnt product after the reaction is repeatedly washed and filtered in hot deionized water until it is used AgNO 3 The reagent detects the filtrate, and Cl cannot be detected in the filtrate — , the washing is completed; finally, the cleaned powder is dried to obtain the required PbBi 4 Ti 4 o 15 cry...

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Abstract

The invention discloses a preparation method of micrometer grade thin flaky lead zirconate titanate crystals, and relates to the field of piezoelectric ceramics. A molten salt method is used for preparing lead zirconate titanate crystals with the flaky (001) preferred orientation to be used as precursors; then, through topochemical reaction, mixing the precursor crystals, PbO and ZrO2 according toa mol ratio of 1:(7 to 7.2):4; then, mixing the mixed powder and NaCl according to the mass ratio of (0.5 to 1.5):1; performing heat insulation for 1 to 4 hours at the temperature of 850 to 1050 DEGC; finally performing washing by hot deionized water; performing acid washing; removing NaCl and Bi2O3 in firing articles so as to obtain the micrometer grade thin flaky lead zirconate titanate (Pb(Zr0.5Ti0.5)O3) crystals. The prepared zirconate titanate crystals have perovskite structures; the microcosmic appearance is a thin flaky shape; great diameter-to-thickness ratio and high orientation degree are realized; the preparation process stability is high; the successful rate is high; the crystals can be favorably used as seed crystals of lead zirconate titanate texture ceramics with high orientation degree.

Description

technical field [0001] The invention relates to the field of piezoelectric ceramics, in particular to a method for preparing micron-scale flake-shaped lead zirconate titanate crystals. Background technique [0002] Piezoelectric ceramics are widely used in industrial and national defense fields such as ultrasonic motors, transducers, and filters as sensors, drivers, and frequency converters. At present, lead zirconate titanate and its doping-modified piezoelectric ceramic materials are the most widely used ceramic materials, and the corresponding single crystals have high piezoelectric properties in the <001> direction , piezoelectric coefficient d 33 >1500pC / N. [0003] Due to the random arrangement of grain orientation and no anisotropy of traditional polycrystalline ceramics, its piezoelectric performance is far lower than that of the corresponding single crystal. However, the preparation cost of single crystal is high, the process is complicated, and the moldi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/00B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01G25/006C01P2004/20C01P2004/61C01P2004/62C01P2004/64
Inventor 杨颖孙胜王一平盛云胡悫睿封硕李秀秀
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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