High-piezoelectric coefficient potassium-sodium niobate based leadless piezoelectric ceramics and preparation method thereof

A potassium-sodium niobate-based, lead-free piezoelectric technology, applied in the field of high-voltage potassium-sodium niobate-based lead-free piezoelectric ceramics and its preparation, can solve problems such as high-voltage performance, difficulty in obtaining, and complex process , to achieve the effect of increasing the piezoelectric coefficient, shortening the time, and simplifying the process

Inactive Publication Date: 2015-09-02
TONGJI UNIV
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Problems solved by technology

[0004] At present, the preparation of lead-free potassium niobate-based piezoelectric ceramics mainly adopts the traditional solid-state sintering method [Wu J, Peng T, Wang Y, et al. Phase structure and electrical properties of (K 0.48 Na 0.52 )(Nb 0.95 Ta 0.05 )O 3 -LiSbO 3 lead free piezoelctric ceramics.J Am Ceram Soc.,2007,91:319~321], however, using the traditional solid-state sintering method, it is difficult to obtain high piezoelectric properties due to the volatilization of potassium and sodium during high-temperature sintering, thus Limit the application of piezoelectric ceramics
In order to obtain high-performance piezoelectric ceramics, methods of improving the preparation process, such as hot pressing sintering, spark plasma sintering and microwave sintering, etc. [Guo Y.P, Kakimoto K, Ohsato H, Phase transitional behavior and piezoelectric properties of Na 0.5 K 0.5 NbO 3 -LiNbO 3 ceramics,Appl Phys Let.,2004,85:4121~4123.], but the above method requires specific experimental equipment and complex process, it is difficult to realize industrial production, so it is necessary to explore a sintering process with simple process and excellent product performance method

Method used

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  • High-piezoelectric coefficient potassium-sodium niobate based leadless piezoelectric ceramics and preparation method thereof

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Experimental program
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Embodiment 1

[0033] (1) According to (1-a) (K 0.5 Na 0.5 ) 0.95 Li 0.05 Nb 0.93 Sb 0.07 -aCaZrO 3 The stoichiometric ratio of raw material Na 2 CO 3 , K 2 CO 3 , Li 2 CO 3 ,Nb 2 o 5 ,Sb 2 o 5 and CaCO 3 , where a=0.04, put into the ball mill tank and carry out mixing, the ball milling medium is absolute ethanol and zirconia balls, the mass ratio of mixed raw materials and zirconia balls is 1:1.2, and the mass ratio with absolute ethanol is 1: 1.5; The mixed raw materials are ball milled at a speed of 360r / min for 24h, dried at 100°C, put into a corundum crucible, covered, and kept at 850°C for 6h, with a heating rate of 3°C / min;

[0034](2) Grind the powder obtained in step (1) in a mortar, carry out secondary ball milling, the conditions of ball milling and drying are the same as in step (1), and obtain 0.96 (K 0.5 Na 0.5 ) 0.95 Li 0.05 Nb 0.93 Sb 0.07 -0.04CaZrO 3 mixed powder;

[0035] (3) The powder material that step (2) obtains is added the PVA solution that c...

Embodiment 2

[0040] (1) According to (1-a) (K 0.5 Na 0.5 ) 0.95 Li 0.05 Nb 0.93 Sb 0.07 -aCaZrO 3 The stoichiometric ratio of raw material Na 2 CO 3 ,K 2 CO 3 , Li 2 CO 3 ,Nb 2 o 5 ,Sb 2 o 5 and CaCO 3 , wherein a=0.04, put into the ball mill tank and carry out mixing, the ball milling medium is absolute ethanol and zirconia balls, the mass ratio of mixed raw materials and zirconia balls is 1:1.2, and the mass ratio with absolute ethanol is 1: 1.5; The mixed raw materials are ball milled at a speed of 360r / min for 24h, dried at 100°C, put into a corundum crucible, covered, and kept at 850°C for 6h, with a heating rate of 3°C / min;

[0041] (2) Grind the powder obtained in step (1) in a mortar, carry out secondary ball milling, the conditions of ball milling and drying are the same as in step (1), and obtain 0.96 (K 0.5 Na 0.5 ) 0.95 Li 0.05 Nb 0.93 Sb 0.07 -0.04CaZrO 3 mixed powder;

[0042] (3) The powder material that step (2) obtains is added the PVA solution that...

Embodiment 3

[0047] (1) According to (1-a) (K 0.5 Na 0.5 ) 0.95 Li 0.05 Nb 0.93 Sb 0.07 -aCaZrO 3 The stoichiometric ratio of raw material Na 2 CO 3 ,K 2 CO 3 , Li 2 CO 3 ,Nb 2 o 5 ,Sb 2 o 5 and CaCO 3 , wherein a=0.04, put into the ball mill tank and carry out mixing, the ball milling medium is absolute ethanol and zirconia balls, the mass ratio of mixed raw materials and zirconia balls is 1:1.2, and the mass ratio with absolute ethanol is 1: 1.5; The mixed raw materials are ball milled at a speed of 360r / min for 24h, dried at 100°C, put into a corundum crucible, covered, and kept at 850°C for 6h, with a heating rate of 3°C / min;

[0048] (2) Grind the powder obtained in step (1) in a mortar, carry out secondary ball milling, the conditions of ball milling and drying are the same as in step (1), and obtain 0.96 (K 0.5 Na 0.5 ) 0.95 Li 0.05 Nb 0.93 Sb 0.07 -0.04CaZrO 3 mixed powder;

[0049] (3) The powder material that step (2) obtains is added the PVA solution that...

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Abstract

The invention relates to high-piezoelectric coefficient potassium-sodium niobate based leadless piezoelectric ceramics and a preparation method thereof. The raw material composition of the high-piezoelectric coefficient potassium-sodium niobate based leadless piezoelectric ceramics is (1-a)(K0.5Na0.5)-.95Li0.05Nb0.93Sb0.07-aMZrO3, wherein M is Ca, Sr or Ba, and a is within the range of 0.01 to 0.06; the following three-step sintering solid-phase synthesis preparation method is adopted: in the first step, the sintering temperature is within the range of 1100-1120 DEG C and the heat preservation time is 0 minute; in the second step, the sintering temperature is within the range of 1160-1210 DEG C and the heat preservation time is 0-5 minutes; in the third step, the sintering temperature is within the range of 1000-1100 DEG C and the heat preservation time is 2-20 minutes; consequently, a novel leadless piezoelectric ceramic material can be obtained, and the maximum piezoelectric coefficient d33 of the material is 410pC/N, wherein d*33 is 450. The leadless piezoelectric ceramic material is applied to a plurality of fields such as ultrasonic transducers, piezoelectric buzzers, drivers and resonators.

Description

technical field [0001] The invention relates to a piezoelectric ceramic and a preparation method thereof, in particular to a high-voltage electric coefficient potassium sodium niobate-based lead-free piezoelectric ceramic and a preparation method thereof. Background technique [0002] Piezoelectric ceramics are an important class of functional materials, which have been widely used in many fields such as communication, aerospace, nuclear energy, automobile, detection and computer. In 2011, the global market size of ferroelectric, piezoelectric materials and related devices reached USD 300 billion. At present, high-performance piezoelectric materials mainly include lead zirconate titanate (PZT) piezoelectric ceramics and lead magnesium niobate-lead titanate relaxor ferroelectric single crystals, etc., and the proportion of lead oxide contained in them exceeds 60%. Because lead-containing materials will cause serious damage to the environment and human beings in the process o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/495C04B35/622
Inventor 翟继卫张杨沈波
Owner TONGJI UNIV
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