Preparation method for 0-3 compound multiple-ferrite ceramic of cobalt ferrite and lead lanthanum zironate titanate

A technology of lead lanthanum zirconate titanate and multiferroic ceramics is applied in the field of ferroelectric/ferromagnetic composite materials, which can solve the problems of complex processing technology degradation factors, uneven phase dispersion, phase reaction and the like

Active Publication Date: 2012-07-04
山东一开电气设备有限公司
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AI Technical Summary

Problems solved by technology

[0003] Since the late 1950s in Cr 2 o 3 Since the discovery of the magnetoelectric effect in single crystals, the research on magnetoelectric materials has been paid more attention by scientific research institutions in various countries; so far, there have been hundreds of materials with magnetoelectric effects discovered, which can be roughly divided into single and single crystals. There are two types of phase compounds and composite materials; the magnetoelectric coupling coefficient of single-phase ferroelectric / ferromagnetic materials is usually low, and they only have magnetoelectric effects when they are far below room temperature, so they usually cannot meet the requirements of practical applications In addition, the price of some materials is relatively expensive, complex processing technology and degradation factors of magnetoelectric conversion performance under alternating conditions, etc., which makes the progress of the practical application of single-phase ferroelectric / ferromagnetic materials has been little. Applying this difficult problem, people began to study ferroelectric / ferromagnetic composite materials
[0004] The preparation methods of ferroelectric / ferromagnetic composite blocks mainly include Guled laminated, Polymer-based, Solid-state reaction, etc.; Realize the composite on the macro level, so the block has many defects, such as macroscopic mechanical defects, uneven phase dispersion, phase reaction, low magnetoelectric coupling coefficient, etc.
[0005] Ferromagnetic phase powder and ferroelectric phase powder were mixed, and solid phase sintering was carried out at a certain temperature to obtain ferromagnetic / ferroelectric composite materials; Mahajan et al. prepared BaTiO by solid state reaction method 3 / CuFe 2 o 4 structure of ferromagnetic / ferroelectric composites and achieved high magnetoelectric coupling coefficient [1] ; Dai et al. also applied this method to prepare CuFe with different volume ratios 2 o 4 / PbZr 0.53 Ti 0.47 o 4 Ferroelectric / Ferromagnetic Composite Materials [2] The biggest advantage of this method is that the experimental conditions are relatively easy to control, the cost of preparation is low, and the reaction between the two phases is not easy; the sintering time, sintering temperature, heating rate, and cooling rate will directly affect the material microstructure and magnetoelectric effect. , but the density, piezoelectric properties and magnetoelectric conversion properties of the composite materials prepared by this method need to be improved

Method used

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  • Preparation method for 0-3 compound multiple-ferrite ceramic of cobalt ferrite and lead lanthanum zironate titanate

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preparation example Construction

[0023] The preparation method of the high magnetoelectric conversion coefficient composite multiferroic ceramics comprises the following steps:

[0024] (1) Preparation of PLZT powder

[0025] Use analytically pure lead oxide, titanium dioxide, zirconium dioxide, lanthanum trioxide, and niobium pentoxide as raw materials, adopt the traditional mixed oxide sintering process, pre-fire at 850°C for 3 hours after mixing, and pulverize the powder and zirconia balls (diameter 3mm, 5mm, 10mm mass ratio is 4:2:1) into a nylon ball mill jar at a mass ratio of 1:4, and use water as the medium to grind for 2 hours to obtain an average particle size of 0.8- 1.2 micron lead zirconate titanate powder.

[0026] (2) Preparation of CFO powder

[0027] Will Fe 2 o 3 Mixed with CoO at a molar ratio of 1:1, pre-fired at 850°C for 2h, sintered at 1275°C for 2h, CoFe 2 o 4 Put the powder into a stainless steel tank, add 3-4 times the mass of steel balls (the mass ratio of steel balls with dia...

example

[0035] Using analytically pure lead oxide, titanium dioxide, zirconium dioxide, lanthanum trioxide, and niobium pentoxide as raw materials, LiBiO was prepared according to the above steps 3 Doped PLZT and zirconia-coated CFO powders.

[0036] Mix the two powders according to the mass ratio CFO:PLZT=1 / 9, 2 / 8, 3 / 7 and 4 / 6 (volume ratio 14.4 / 85.6, 27.4 / 72.6 and 39.3 / 60.7), and add polyvinyl alcohol (5%) aqueous solution, granulated and pressed to make discs with a diameter of 11 mm and a thickness of 1.5 mm, and sintered at 850-1150 ° C for 15 minutes to obtain composite ceramic discs; for comparison, the quality of all samples is the same as the original size .

Embodiment 1

[0037] Example 1 CFO: PLZT=1 / 9

[0038] (1) Preparation of PLZT powder

[0039] Using analytically pure 127.77g of lead oxide, 20.58g of titanium dioxide, 43.83g of zirconium dioxide, 6.15g of lanthanum trioxide and 1.67g of niobium pentoxide as raw materials, the traditional mixed oxide sintering process was adopted, and the mixture was mixed at 850 Pre-fired at ℃ for 3 hours, crushed powder and zirconia balls (diameter: 3mm, 5mm, 10mm, mass ratio: 4:2:1) were put into nylon ball mill tank according to the mass ratio of 1:4, and water was used as the medium for milling 2 Hours, the lead zirconate titanate powder (Pb 0.91 La 0.06 (Zr 0.58 Ti 0.42 ) 0.975 Nb 0.02 o 3 ).

[0040] (2) Preparation of CFO powder

[0041] Will Fe 2 o 3 Mixed with CoO at a molar ratio of 1:1, pre-fired at 850°C for 2h, sintered at 1275°C for 2h, CoFe 2 o 4 Put the powder into a stainless steel tank, add 3 times the mass of steel balls (the mass ratio of steel balls with diameters of 2mm...

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Abstract

The invention relates to ferroelectric/ferromagnetic compound materials, in particular to a preparation method for 0-3 compound multiple-ferrite ceramic of cobalt ferrite and lead lanthanum zironate titanate, which is characterized in that lead lanthanum zironate titanate is used as a ferroelectric phase in multiple-ferrite ceramic, cobalt ferrite is used as a ferromagnetic phase in the multiple-ferrite ceramic, zirconium oxide sol is wrapped on the surface of the ferrite phase of the cobalt ferrite through sol-gel technology to form a zirconium dioxide coating layer through pyrolysis, 3-8% of LiBiO3 is added into the lead lanthanum zironate titanate to serve as low temperature sintering aid to perform low temperature sintering, the cobalt ferrite wrapped the zirconium dioxide on the surface is mixed with the lead lanthanum zironate titanate sintered at the low temperature according to the mass ratio of 0.1 to 0.5:1, and then mixture of the cobalt ferrite and the lead lanthanum zironate titanate are granulated, pressed and sintered to be prepared into compound ceramic. The preparation method enables CFO and lead lanthanum zironate titanate (PLZT) powder to be compounded and sintered, thereby being simple in process, low in cost and easy to achieve industrialized batch production.

Description

technical field [0001] The invention relates to ferroelectric / ferromagnetic composite materials, in particular to a preparation method of cobalt ferrite and lead lanthanum zirconate titanate 0-3 composite multiferroic ceramics. Background technique [0002] Materials with (anti) ferroelectricity, (anti)ferromagnetism, piezoelectricity and other properties at the same time are called multiferroic materials; this type of material combines electricity, magnetism and force, and can realize the regulation of these parameters. For example, the magnetism of a material can be controlled by an electric field or the electrical polarization of a material can be controlled by a magnetic field, so that this type of material has an important application prospect in new electronic devices; Controllable optical modulators for the refractive index and absorptivity of light; non-volatile multiferroic memories that can be written and read by electric and magnetic fields; magnetic field modulat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/493C04B35/622
Inventor 李坤施东良李政朱尹李金华王雨陈王丽华
Owner 山东一开电气设备有限公司
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