Lead lanthanum zirconate titanate ceramic powder as well as preparation method and application thereof

A technology of lead lanthanum zirconate titanate and ceramic powder, which is applied in the field of lead lanthanum zirconate titanate ceramic powder and its preparation, can solve the problems of low precursor concentration, long reaction time, and easy agglomeration of powder, and achieve powder High purity, uniform crystal grains, and high sintering activity

Pending Publication Date: 2020-02-28

GUANGDONG UNIV OF TECH

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Problems solved by technology

The powder prepared by the sol-gel method has precise composition, easy control of composition, and high purity, but it needs to be calcined at high temperature, and the powder is easy to agglomerate during the calcining pr...

Abstract

The invention belongs to the technical field of inorganic non-metallic materials, and discloses lead lanthanum zirconate titanate ceramic powder as well as a preparation method and application thereof. The molecular formula of the lead lanthanum zirconate titanate ceramic is Pb<x>La<1-x>Zr<y>Ti <1-y>, x is equal to 0.94, and y is equal to 0.52-0.95; the preparation method comprises the following steps: dissolving lead acetate and lanthanum acetate in deionized water to obtain a lead-lanthanum aqueous solution, and dissolving zirconium n-propoxide and tetrabutyl titanate in absolute ethyl alcohol to obtain a zirconium-titanium alcohol solution; adding the zirconium-titanium alcohol solution into the lead-lanthanum aqueous solution, and stirring to obtain a lead lanthanum zirconate titanatemixed solution; under magnetic stirring, adding potassium hydroxide into the lead lanthanum zirconate titanate mixed solution to obtain a lead lanthanum zirconate titanate turbid liquid precursor; andcarrying out hydrothermal reaction on the precursor at 160-180 DEG C to obtain a lead lanthanum zirconate titanate slurry, centrifuging, washing and drying to obtain the lead lanthanum zirconate titanate ceramic powder. The ceramic powder is high in purity, good in dispersity, small and controllable in particle size and high in precursor solution concentration, and can be applied to the fields ofrefrigeration and energy storage.

Technology Topic

Lead acetateLanthanum +12

Image

Examples

Experimental program(3)

Example Embodiment

[0033] Example 1

[0034] 1. Follow Pb 0.94 La 0.06 Zr 0.52 Ti 0.48 Accurate stoichiometric ratio, weigh 17.7390g of lead acetate and 0.8543g of lanthanum acetate, pour into 30ml of deionized water, stir magnetically for 10min under heating in a water bath at 75℃ to prepare a lead lanthanum aqueous solution;

[0035] 2. Weigh 10.9501 g of zirconium n-propoxide and 7.5015 g of tetrabutyl titanate, pour them into 30 ml of absolute ethanol, and stir magnetically for 20 minutes under heating in a water bath at 75°C to prepare a zirconium titanium alcohol solution;

[0036] 3. Pour the zirconium-titanium alcohol solution into the lead-lanthanum aqueous solution, stir it magnetically for 20 minutes under heating in a water bath at 75°C, and cool to room temperature to prepare a lead-lanthanum zirconate titanate mixture;

[0037] 4. In order to make the potassium hydroxide concentration in the prepared precursor solution 2mol/L, weigh 6.2345g potassium hydroxide and pour it into the lead and lanthanum zirconate titanate mixture cooled to room temperature and magnetically stir for 30 minutes to obtain lead zirconate titanate Lanthanum precursor suspension;

[0038] 5. Pour the lead lanthanum zirconate titanate precursor suspension into a hydrothermal kettle with a filling degree of 70-80%, and put it in an oven at 180°C for 10 hours. After the incubation, cool to room temperature, pour the obtained slurry into a centrifuge tube and wash with 36% acetic acid, 3 times with deionized water, 1 time with absolute ethanol, and finally dry at 80°C for 12 hours. The lead lanthanum zirconate titanate ceramic powder was prepared.

[0039] figure 1 In (a) is the XRD pattern of the lead lanthanum zirconate titanate powder prepared in Example 1. From figure 1 It can be seen from (a) that the XRD pattern has no miscellaneous peaks and matches the standard card PDF#70-4060, indicating that a pure tetragonal lead lanthanum zirconate titanate ceramic powder has been prepared. figure 2 This is the SEM photograph of the lead lanthanum zirconate titanate powder obtained in Example 1. From figure 2 It can be seen that the particle morphology of the obtained lead lanthanum zirconate titanate ceramic powder is cubic, the average particle size is about 200 nm, the particle size distribution is uniform, and the powder dispersibility is good.

Example Embodiment

[0040] Example 2

[0041] 1. Follow Pb 0.94 La 0.06 Zr 0.63 Ti 0.37 Weigh 17.7390g of lead acetate and 0.8543g of lanthanum acetate in an accurate stoichiometric ratio, pour into 30ml of deionized water, and stir magnetically for 10 minutes under heating in a water bath at 75°C to prepare an aqueous solution of lead and lanthanum;

[0042] 2. Weigh 13.2665g of zirconium n-propoxide and 5.7824g of tetrabutyl titanate, pour into 30ml of absolute ethanol, stir magnetically under heating in a water bath at 75°C for 20 minutes to obtain a zirconium titanium alcohol solution;

[0043] 3. Pour the zirconium-titanium alcohol solution into the lead-lanthanum aqueous solution, stir it magnetically for 20 minutes under heating in a water bath at 75°C, and cool to room temperature to prepare a lead-lanthanum zirconate titanate mixture;

[0044] 4. In order to make the potassium hydroxide concentration in the prepared precursor solution 3mol/L, weigh 9.3517g potassium hydroxide and pour it into the lead and lanthanum zirconate titanate mixture cooled to room temperature and magnetically stir for 30 minutes to obtain lead zirconate titanate Lanthanum precursor suspension;

[0045] 5. Pour the lead lanthanum zirconate titanate precursor suspension into a hydrothermal kettle with a filling degree of 70-80%, keep it at 160°C for 10 hours, and cool it to room temperature after the heat preservation is complete. The material was poured into a centrifuge tube and washed with 36% acetic acid for 1 time, deionized water for 3 times, and anhydrous ethanol for 1 time, and finally dried at 80°C for 12 hours to prepare lead lanthanum zirconate titanate ceramic powder.

[0046] figure 1 In (b) is the XRD pattern of the lead lanthanum zirconate titanate powder prepared in Example 2. From figure 1 (b) It can be seen that the XRD pattern has no impurity peaks, and it matches the standard card PDF#70-4060, indicating that a pure tetragonal phase lead lanthanum zirconate titanate ceramic powder is prepared; image 3 This is an SEM photograph of the lead lanthanum zirconate titanate powder obtained in Example 2. From image 3 It can be seen that the particle morphology of the obtained lead lanthanum zirconate titanate ceramic powder is cubic, the average particle size is about 500 nm, the particle size distribution is uniform, and the powder dispersibility is good.

Example Embodiment

[0047] Example 3

[0048] 1. Follow Pb 0.94 La 0.06 Zr 0.95 Ti 0.05 Weigh 17.7390g of lead acetate and 0.8543g of lanthanum acetate in an accurate stoichiometric ratio, pour into 30ml of deionized water, and stir magnetically for 10 minutes under heating in a water bath at 75°C to prepare an aqueous solution of lead and lanthanum;

[0049] 2. Weigh 20.0050g of zirconium n-propoxide and 0.7814g of tetrabutyl titanate, pour into 30ml of absolute ethanol, and stir magnetically for 20 minutes under heating in a water bath at 75°C to obtain a zirconium-titanium alcohol solution;

[0050] 3. Pour the zirconium-titanium alcohol solution into the lead-lanthanum aqueous solution, stir it magnetically for 20 minutes under heating in a water bath at 75°C, and cool to room temperature to prepare a lead-lanthanum zirconate titanate mixture;

[0051] 4. In order to make the potassium hydroxide concentration in the prepared precursor solution 3mol/L, weigh 9.3517g potassium hydroxide and pour it into the lead and lanthanum zirconate titanate mixture cooled to room temperature and magnetically stir for 30 minutes to obtain lead zirconate titanate Lanthanum precursor suspension;

[0052] 5. Pour the obtained lead lanthanum zirconate titanate precursor suspension into a hydrothermal kettle with a filling degree of 70-80%, put it in an oven at 180°C for 7 hours, and cool to room temperature after the insulation is complete. The resulting slurry Pour into the centrifuge tube and wash with 36% acetic acid centrifugation once, deionized water centrifugal washing 3 times, absolute ethanol centrifugal washing once, and finally drying in a drying oven at 80°C for 12 hours to prepare lead lanthanum zirconate titanate ceramic powder body.

[0053] figure 1 In (c) is the XRD pattern of the lead lanthanum zirconate titanate powder prepared in Example 3. From figure 1 In (c), it can be seen that the XRD pattern has no miscellaneous peaks, and it matches the standard card PDF#87-0564, indicating that a pure orthogonal phase lead lanthanum zirconate titanate ceramic powder was prepared; Figure 4 This is the SEM photograph of the lead lanthanum zirconate titanate powder obtained in Example 3. From Figure 4 It can be seen that the obtained lead lanthanum zirconate titanate ceramic powder has a cubic morphology, an average particle size of about 800 nm, a uniform particle size distribution, and good powder dispersion.

PUM

Property	Measurement	Unit
Average particle size	200.0	nm
Average particle size	500.0	nm
Average particle size	800.0	nm

Description & Claims & Application Information

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Lead lanthanum zirconate titanate ceramic powder as well as preparation method and application thereof

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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