CN109607615B - B-site high-entropy perovskite oxide and preparation method thereof - Google Patents
B-site high-entropy perovskite oxide and preparation method thereof Download PDFInfo
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- CN109607615B CN109607615B CN201910071218.9A CN201910071218A CN109607615B CN 109607615 B CN109607615 B CN 109607615B CN 201910071218 A CN201910071218 A CN 201910071218A CN 109607615 B CN109607615 B CN 109607615B
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Abstract
The invention discloses a class ratio high-entropy alloy, which is prepared from raw materials of BaCO3, zrO2, snO2, tiO2, hfO2, nb2O5 and Ga2O3 by mixing, wet grinding, drying and presintering, and has the characteristics of convenient operation, strong practicability and convenient popularization and application.
Description
Technical Field
The invention relates to the technical field of perovskite oxides, in particular to a B-site high-entropy perovskite oxide and a preparation method thereof.
Background
The high-entropy alloy is an alloy which is formed by alloying five or more elements according to the principle of equal atomic ratio or near equal atomic ratio, and is a high-entropy solid solution, and the high-entropy alloy has the characteristics of higher thermal stability, high strength, high hardness, good wear resistance, good oxidation resistance, strong corrosion resistance and the like because of higher mixed entropy among all the components, so the high-entropy alloy becomes an emerging material with great development potential, and has great prospect in engineering application.
The perovskite oxide is perovskite BaTiO 3 The perovskite structure of the compound with the same structure can be ABO 3 The cation at the A position is in a 12-coordinate structure and is positioned at 12 vertex positions of the cubic unit cell, the cation at the B position is in a 6-coordinate structure and is positioned at the body center position of the cubic unit cell, and the O ions are positioned at 6 face center positions. Perovskite oxide tolerance factor t value is formulated
Calculation, wherein R A 、R B 、R O Respectively represents the A-position cation radius, the B-position cation radius and the oxygen ion radius. It is known from the literature that the closer t is to 1, the easier it is to form a single-phase perovskite structure.
Disclosure of Invention
The invention designs a novel B-site high-entropy perovskite oxide Ba (Zr) based on high-entropy alloy 1/6 Sn 1/6 Ti 1/ 6 Hf 1/6 Nb 1/6 Ga 1/6 )O 3 At present, no report on the B-site high-entropy perovskite oxide is known.
The invention protectsA B-site high-entropy perovskite oxide has a chemical formula of Ba (Zr) 1/6 Sn 1/6 Ti 1/6 Hf 1/ 6 Nb 1/6 Ga 1/6 )O 3 。
The invention also provides a preparation method of the B-site high-entropy perovskite oxide, which comprises the following steps:
step 1: the raw material BaCO 3 、ZrO 2 、SnO 2 、TiO 2 、HfO 2 、Nb 2 O 5 And Ga 2 O 3 According to the formula Ba (Zr) 1/6 Sn 1/ 6 Ti 1/6 Hf 1/6 Nb 1/6 Ga 1/6 )O 3 Accurately weighing the stoichiometric ratio of the catalyst, then mixing, and mixing Zr in the oxide 4+ Ions, sn 4+ Ions, ti 4+ Ions, hf 4+ Ion, nb 5+ Ions, ga 3+ Mixing ions according to equal atomic ratio, zr 4+ Ion 1/6, sn 4+ Ion 1/6, ti 4+ Ion 1/6, hf 4+ Ion 1/6, nb 5+ Ion 1/6, ga 3+ Ion 1/6;
step 2: grinding the mixed raw materials;
step 3: and (3) drying the ground powder, and presintering for 6-10 h at 1300-1400 ℃ to obtain the B-site high-entropy perovskite oxide.
And further, in the step 2, absolute ethyl alcohol is added into a grinding pot to be subjected to wet grinding for more than 4 hours, and the absolute ethyl alcohol at least needs to be used as a raw material.
Further, in the step 3, the drying temperature is 70 ℃, and the drying time is not less than 24 hours.
Further, in the step 4, the presintering temperature is 1400 ℃, the presintering time is 8 hours, and the heating rate is 3-5 ℃/min.
The preparation method of the B-site high-entropy perovskite oxide disclosed and prepared by the invention has the characteristics of convenience in operation, strong practicability and convenience in popularization and application; the B-site high-entropy perovskite oxide is structurally and firstly realizes solid solution of 6 elements of the B site, has higher solid solubility than a common solid solution, and is convenient to realize performance regulation and control as required by further changing different cation combinations or carrying out fine adjustment on components on the basis of equal atomic ratio.
Drawings
FIG. 1 is an XRD pattern of a B-site high entropy perovskite oxide prepared according to the invention;
FIG. 2 is an EDS spectrum of a B-site high entropy perovskite oxide prepared according to the present invention.
Detailed Description
The invention will be described in further detail with reference to the drawings and the detailed description. The embodiments of the invention have been presented for purposes of illustration and description, and are not intended to be exhaustive or limited to the invention in the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, and to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated.
Example 1
A B-site high entropy perovskite oxide having the chemical composition: ba (Zr) 1/6 Sn 1/6 Ti 1/6 Hf 1/6 Nb 1/6 Ga 1/6 )O 3 The preparation method comprises the following steps:
step 1: the raw material BaCO 3 、ZrO 2 、SnO 2 、TiO 2 、HfO 2 、Nb 2 O 5 And Ga 2 O 3 According to the formula Ba (Zr) 1/6 Sn 1/ 6 Ti 1/6 Hf 1/6 Nb 1/6 Ga 1/6 )O 3 Is precisely measured, in particular BaCO 3 1.2464g, zrO 2 0.1232g of SnO 2 0.1507g of TiO 2 0.0799g, hfO 2 0.2107g, nb 2 O 5 0.1330g and Ga 2 O 3 0.0947g, then mixed;
step 2: placing the mixed raw materials into a grinding pot, adding absolute ethyl alcohol, and carrying out wet grinding for more than 4 hours, wherein the absolute ethyl alcohol at least needs to be used for the raw materials;
step 3: drying the ground powder at 70 ℃ for at least 24 hours; and (3) placing the dried powder into a muffle furnace, and pre-sintering for 8 hours at the temperature of 1400 ℃ at 5 ℃/min to obtain the B-site high-entropy perovskite oxide.
Experimental analysis shows that the B-bit high entropy perovskite oxide Ba (Zr) 1/6 Sn 1/6 Ti 1/6 Hf 1/6 Nb 1/6 Ga 1/6 )O 3 Has the following characteristics:
1. and (3) structural determination: different substances have specific atomic types, atomic arrangement modes and lattice parameters, and under the action of X rays, different crystal faces of the crystal generate respective diffraction to show specific diffraction patterns, so that the structure of a sample is determined by adopting X-ray powder diffraction. The instrument used here is a SmartLab-japan X-ray diffractometer, whose scanning angle range: 2θ=20 to 80 °, the scanning speed is 5 °/min, the step size is 0.01 °, and the obtained powder diffraction result is shown in fig. 1.
2. Morphology determination: observing the B-bit high-entropy perovskite oxide Ba (Zr) by adopting a field emission scanning electron microscope 1/ 6 Sn 1/6 Ti 1/6 Hf 1/6 Nb 1/6 Ga 1/6 )O 3 The EDS surface scan results are shown in FIG. 2, using a field emission scanning electron microscope-energy spectrometer, model 55, zeiss SUPRA, germany.
It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art and which are included in the embodiments of the present invention without the inventive step, are intended to be within the scope of the present invention.
Claims (2)
1. A preparation method of B-site high-entropy perovskite oxide is characterized in that the chemical molecular formula of the B-site high-entropy perovskite oxide is Ba (Zr) 1/6 Sn 1/ 6 Ti 1/6 Hf 1/6 Nb 1/6 Ga 1/6 )O 3 The preparation method comprises the following steps:
step 1: the raw material BaCO 3 、ZrO 2 、SnO 2 、TiO 2 、HfO 2 、Nb 2 O 5 And Ga 2 O 3 According to the formula Ba (Zr) 1/6 Sn 1/6 Ti 1/ 6 Hf 1/6 Nb 1/6 Ga 1/6 )O 3 Accurately weighing the stoichiometric ratio of the components, and then mixing;
step 2: grinding the mixed raw materials, wherein the grinding process is to add absolute ethyl alcohol into a grinding pot for wet grinding for more than 4 hours, and the absolute ethyl alcohol at least needs to be used for the raw materials;
step 3: drying the ground powder, presintering for 8 hours at 1400 ℃ to obtain the B-site high-entropy perovskite oxide, and controlling the heating rate to be 3-5 ℃/min.
2. The method for preparing a B-site high-entropy perovskite oxide according to claim 1, wherein in the step 3, the drying temperature is 70 ℃ and the drying time is not less than 24 hours.
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