CN111763087A - Series of cubic fluorite type high-entropy cerium oxide nano-powder and preparation method thereof - Google Patents
Series of cubic fluorite type high-entropy cerium oxide nano-powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a series of cubic fluorite type high-entropy cerium oxide nano-powders and a preparation method thereof, wherein the chemical molecular formula of the series of high-entropy oxides is Re2Ce2O7Wherein Re is the equal mole ratio combination of any five rare earth metal elements of La, Er, Nd, Sm, Gd, Dy, Yb, Lu, Sc and Y, and the crystal structure is a cubic fluorite structure. The series of high-entropy oxides are all high-entropy cerium oxides and have uniform single-phase structures. The method has the advantages of simple process, high purity of the prepared product, high yield, suitability for large-scale production and adjustable components. The series of high-entropy cerium oxide nano-powder has the advantages of high purity and good high-temperature stability. In addition, the seriesThe high-entropy cerium oxide can adjust the performance of the high-entropy cerium oxide by regulating and controlling the constituent elements of the high-entropy cerium oxide, is convenient for better coping with different service conditions, fills up the research blank of the high-entropy oxide, enriches a high-entropy material system and expands the application range of the high-entropy ceramic.
Description
Technical Field
The invention belongs to the technical field of high-entropy ceramic material preparation, and relates to a series of cubic fluorite type high-entropy cerium oxide nano-powder and a preparation method thereof.
Background
In recent years, high entropy materials have received much attention because of their special properties. The first reported high entropy material was a high entropy alloy reported in 2004 by professor leonurus. [ document "Nanostructured high-entry electroconductive with multiple primary elements: novel ally design elements and outer monomers [ J ]].Advanced Engineering Materials,2004,6:299-303.”]Along with the discovery of a series of high-entropy alloys, people increasingly know high-entropy materials. In 2015, Rost et al extended the definition of high entropy materials to the field of inorganic non-metals and reported the synthesis of high entropy ceramics for the first time. The method comprises the steps of fully mixing five oxide raw materials (CoO, CuO, MgO, NiO and ZnO) through high-energy ball milling, carrying out heat treatment at 1000 ℃ for 12 hours, and then carrying out quenching treatment to obtain high-entropy oxide (Co) for the first time0.2Cu0.2Mg0.2Ni0.2Zn0.2) O ceramic powder. (literature "control-stabilized oxides [ J ]]Nature Communication,2015,6:8485. ") then, as the research goes in depth, ultra-high temperature high entropy ceramics were gradually discovered. Castle et al synthesized ultra-high temperature ceramic (Hf-Ta-Zr-Nb) C by a method combining high energy ball milling with spark plasma sintering, and studied the mechanical properties thereof. (document "Processing and properties of high entry ultra-high temperature cassettes [ J ]]Scientific Reports,2018,8: 8609'), high-entropy ceramic has excellent properties such as low thermal conductivity, good oxidation resistance, excellent corrosion resistance and sintering resistance, and is expected to replace the traditional ceramic to be applied to the field of ultra-high temperature, thermal protection and thermal insulation.
However, the ultrahigh-temperature high-entropy ceramics synthesized at present generally have low sample purity and are easy to form a second phase. On the other hand, most of the currently synthesized high-entropy ceramics are a single component, and few self-forming systems exist, so that the performance of the high-entropy ceramics is difficult to adjust to different service conditions by regulating and controlling the components of the high-entropy ceramics. Meanwhile, no relevant reports are made on the high-entropy cerium oxide system at present.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a series of cubic fluorite type high-entropy cerium oxide nano-powder and a preparation method thereof, which can overcome the defects of low purity and easy formation of a second phase of the commonly synthesized ultrahigh-temperature high-entropy ceramics at present, and can deal with different service conditions by regulating and controlling the composition components of the ultrahigh-temperature high-entropy ceramics. Meanwhile, the research blank of the high-entropy oxide is filled, a high-entropy material system is enriched, and the application range of the high-entropy ceramic is expanded.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses a series of cubic fluorite type high-entropy cerium oxide nano-powder, and the chemical formula of the high-entropy cerium oxide nano-powder is Re2Ce2O7Wherein Re is the rare earth metal elements La, Nd, Er, Sm, Gd, Dy, Yb and Lu, and any five of Sc and Y are combined in an equimolar way;
the high-entropy cerium oxide nano powder is a multi-component single-phase solid solution, and the crystal structure of the high-entropy cerium oxide nano powder is cubic fluorite.
Preferably, the particle size of the cubic fluorite type high-entropy cerium oxide nano powder is 10-100 nm.
Preferably, the cubic fluorite type high-entropy cerium oxide nanopowder has a single-phase cubic fluorite crystal structure, and each element is uniformly distributed.
The invention also discloses a preparation method of the series of cubic fluorite high-entropy cerium oxide nano-powder, which comprises the following steps:
1) five kinds of Re with equal molar ratio2O3Dissolving in nitric acid solution, and dropwise adding Ce (NO)3)3Obtaining a mixed ionic solution from the solution; wherein, Re is any one of La, Nd, Er, Sm, Gd, Dy, Yb, Lu, Sc and Y;
2) adding citric acid and a solvent into the mixed ionic solution obtained in the step 1), and adjusting the pH value to 6-7 to obtain mixed sol;
3) removing the solvent in the mixed sol obtained in the step 2) to obtain xerogel;
4) and 3) roasting the dried gel obtained in the step 3) in an air atmosphere to obtain a series of cubic fluorite high-entropy cerium oxide nano-powder.
Preferably, in step 1), Ce (NO) is used3)3The amount of substance(s) and Re used2O3Is greater than 10.
Preferably, in step 2), the ratio of the amount of species of citric acid to the amount of total species of ions in the solution is greater than 2.
Preferably, in step 2), the solvent is any one or a mixture of ethanol and ethylene glycol.
Preferably, in the step 4), the sintering temperature is 750-1250 ℃, the sintering time is 1-5 h, and the temperature rise rate is 5-10 ℃/min from the room temperature.
Preferably, the purity of the raw materials used is higher than 99.99%.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a series of cubic fluorite type high-entropy cerium oxide nano-powders, the chemical molecular formula of which is Re2Ce2O7Wherein Re is the equal mole ratio combination of any five rare earth metal elements of La, Er, Nd, Sm, Gd, Dy, Yb, Lu, Sc and Y, and the crystal structure is a cubic fluorite structure. The series of high-entropy oxides are all high-entropy cerium oxides, have single-phase structures, and are uniformly distributed. The series of high-entropy cerium oxide nano-powder has the advantages of high purity and good high-temperature stability, and can overcome the defects of low purity and easy formation of a second phase of the commonly-existing ultrahigh-temperature high-entropy ceramics synthesized at present. The composition elements of the series of high-entropy cerium oxide can be the combination of any five of rare earth metal elements La, Nd, Er, Sm, Gd, Dy, Yb and Lu and Sc and Y, and the final adjustment of the performance of the high-entropy cerium oxide can be realized by adjusting different element combinations, so that different service environments can be more intelligently met. The seriesThe high-entropy cerium oxide nano powder is suitable for the fields of high-temperature thermal barrier coatings, thermal protection materials, catalysis and the like. The series of high-entropy oxides fill the research blank of the high-entropy cerium oxide ceramics, enrich the high-entropy material system and simultaneously expand the application range of the high-entropy ceramics.
The invention also discloses a preparation method of the series of cubic fluorite high-entropy cerium oxide nano-powder, which is characterized in that a ceramic precursor is synthesized by a sol-gel method, and then a series of cubic fluorite high-entropy cerium oxide ceramic nano-powder is successfully synthesized by a high-temperature pyrolysis roasting method. Compared with other preparation methods of ultrahigh-temperature high-entropy ceramics, the method can obviously reduce the preparation temperature, and meanwhile, the particle size of the product can be controlled to be in a nanometer level, thereby laying a foundation for the subsequent functional application of the high-entropy cerium oxide. The method has the advantages of simple process, high purity of the prepared product, high yield, suitability for large-scale production and adjustable components.
Drawings
FIG. 1 is a flow chart of the preparation of a series of cubic fluorite type high-entropy cerium oxide nanopowders of the present invention;
FIG. 2 shows a cubic fluorite type high entropy cerium oxide ceramic (Er, Gd, La, Sm, Y)2Ce2O7A macroscopic morphology picture of the nano powder;
FIG. 3 is a cubic fluorite type high entropy oxide ceramic (Er, Gd, Sm, Y, Yb)2Ce2O7Microscopic morphology of the nano powder;
FIG. 4 is an XRD pattern of several cubic fluorite type high entropy cerium oxide nanopowders prepared;
FIG. 5 shows a cubic fluorite type high entropy cerium oxide ceramic (Gd, La, Nd, Sm, Yb)2Ce2O7A bulk EDS map;
FIG. 6 is a cubic fluorite type high entropy cerium oxide ceramic (Er, La, Lu, Sc, Sm)2Ce2O7TG-DSC curve in air.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
referring to fig. 1, a series of cubic fluorite type high-entropy cerium oxide nanopowders of the present invention is illustrated by combining a process flow diagram, comprising the following steps:
1) five kinds of Re with equal molar ratio2O3Dissolving in nitric acid solution, and dropwise adding Ce (NO)3)3Obtaining a mixed ionic solution from the solution; wherein, Re is any one of La, Nd, Er, Sm, Gd, Dy, Yb, Lu, Sc and Y.
Ce (NO) used3)3The amount of substance(s) and Re used2O3Is greater than 10.
2) Adding a certain amount of citric acid and a proper amount of solvent into the mixed ionic solution obtained in the step 1), and dropwise adding diluted ammonia water to adjust the pH value to 6-7 to obtain mixed sol.
Wherein the ratio of the amount of citric acid to the total amount of ionic substances in the solution is greater than 2, and the solvent can be ethanol or ethylene glycol or their mixture.
3) Removing the solvent in the mixed sol obtained in the step 2) to obtain xerogel.
4) Placing the xerogel obtained in the step 3) in an air atmosphere to be roasted to obtain a series of cubic fluorite type high-entropy cerium oxide nano-powder;
wherein the sintering temperature is 750-1250 ℃, the sintering time is 1-5 h, and the heating rate is 5-10 ℃/min from the room temperature.
Example 1
In this example, a cubic fluorite type high entropy cerium oxide (Dy, Gd, La, Nd, Sm) was prepared at a calcination temperature of 1250 deg.C, a calcination time of 5 hours, and a temperature rise rate of 10 deg.C/min2Ce2O7Ceramic nano-powder.
The method comprises the following specific steps:
the first step is as follows: five kinds of Re with equal molar ratio2O3Dissolving in nitric acid solution, and dropwise adding Ce (NO)3)3Solution of Re to2O3Total amount of material and Ce (NO)3)3The ratio of the ion source to the ion source is 1:10, and mixed ion solution is obtained; wherein, Re is La, Nd, Gd, Dy and Sm;
the second step is that: adding citric acid and ethylene glycol into the mixed ion solution to enable the ratio of the amount of substances of the citric acid to the total amount of ions in the solution to be 2:1, and dropwise adding diluted ammonia water to adjust the pH value to 6-7 to obtain mixed sol;
the third step: removing the solvent in the mixed sol to obtain xerogel;
the fourth step: placing the xerogel in the third step in air atmosphere, roasting for 5h under the conditions that the roasting temperature is 1250 ℃ and the heating rate is 10 ℃/min, and obtaining the cubic fluorite type high-entropy cerium oxide (Dy, Gd, La, Nd, Sm)2Ce2O7Ceramic nano-powder.
Example 2
In this example, the calcination temperature is 750 ℃, the calcination time is 5h, and the temperature rise rate is 10 ℃/minA cubic fluorite type high entropy cerium oxide (Dy, Gd, La, Nd, Sm)2Ce2O7Ceramic nano-powder.
The method comprises the following specific steps:
the first step is as follows: five kinds of Re with equal molar ratio2O3Dissolving in nitric acid solution, and dropwise adding Ce (NO)3)3Solution of Re to2O3Total amount of material and Ce (NO)3)3The ratio of the ion source to the ion source is 1:10, and mixed ion solution is obtained; wherein, Re is La, Nd, Gd, Dy and Sm;
the second step is that: adding citric acid and ethylene glycol into the mixed ion solution to enable the ratio of the amount of substances of the citric acid to the total amount of ions in the solution to be 2:1, and dropwise adding diluted ammonia water to adjust the pH value to 6-7 to obtain mixed sol;
the third step: removing the solvent in the mixed sol to obtain xerogel;
the fourth step: placing the xerogel obtained in the third step in an air atmosphere, roasting for 5 hours at the roasting temperature of 750 ℃ and the heating rate of 10 ℃/min to obtain the cubic fluorite type high-entropy cerium oxide (Dy, Gd, La, Nd, Sm)2Ce2O7Ceramic nano-powder.
Example 3
In this example, a cubic fluorite type high entropy cerium oxide (Dy, Gd, La, Nd, Sm) was prepared under the conditions of a calcination temperature of 1000 deg.C, a calcination time of 3 hours, and a temperature rise rate of 5 deg.C/min2Ce2O7Ceramic nano-powder.
The method comprises the following specific steps:
the first step is as follows: five kinds of Re with equal molar ratio2O3Dissolving in nitric acid solution, and dropwise adding Ce (NO)3)3Solution of Re to2O3Total amount of material and Ce (NO)3)3The ratio of the ion source to the ion source is 1:10, and mixed ion solution is obtained; wherein, Re is La, Nd, Gd, Dy and Sm;
the second step is that: adding citric acid and ethylene glycol into the mixed ion solution to enable the ratio of the amount of substances of the citric acid to the total amount of ions in the solution to be 2:1, and dropwise adding diluted ammonia water to adjust the pH value to 6-7 to obtain mixed sol;
the third step: removing the solvent in the mixed sol to obtain xerogel;
the fourth step: placing the xerogel obtained in the third step in an air atmosphere, roasting for 3 hours at the roasting temperature of 1000 ℃ and the heating rate of 5 ℃/min to obtain the cubic fluorite type high-entropy cerium oxide (Dy, Gd, La, Nd, Sm)2Ce2O7Ceramic nano-powder.
Example 4
In this example, a cubic fluorite type high entropy cerium oxide (Dy, Gd, La, Nd, Sm) was prepared under the conditions of a calcination temperature of 1000 deg.C, a calcination time of 1 hour, and a temperature rise rate of 5 deg.C/min2Ce2O7Ceramic nano-powder.
The method comprises the following specific steps:
the first step is as follows: five kinds of Re with equal molar ratio2O3Dissolving in nitric acid solution, and dropwise adding Ce (NO)3)3Solution of Re to2O3Total amount of material and Ce (NO)3)3The ratio of the ion source to the ion source is 1:10, and mixed ion solution is obtained; wherein, Re is La, Nd, Gd, Dy and Sm;
the second step is that: adding citric acid and ethylene glycol into the mixed ion solution to enable the ratio of the amount of substances of the citric acid to the total amount of ions in the solution to be 2:1, and dropwise adding diluted ammonia water to adjust the pH value to 6-7 to obtain mixed sol;
the third step: removing the solvent in the mixed sol to obtain xerogel;
the fourth step: placing the xerogel obtained in the third step in an air atmosphere, roasting for 1h at the roasting temperature of 1000 ℃ and the heating rate of 5 ℃/min to obtain the cubic fluorite type high-entropy cerium oxide (Dy, Gd, La, Nd, Sm)2Ce2O7Ceramic nano-powder.
Example 5
In this example, a cubic fluorite type high entropy cerium oxide (Dy, Gd, La, Nd, Sm) was prepared under the conditions of a calcination temperature of 1000 deg.C, a calcination time of 5 hours, and a temperature rise rate of 5 deg.C/min2Ce2O7Ceramic nano-powder.
The method comprises the following specific steps:
the first step is as follows: five kinds of Re with equal molar ratio2O3Dissolving in nitric acid solution, and dropwise adding Ce (NO)3)3Solution of Re to2O3Total amount of material and Ce (NO)3)3The ratio of the ion source to the ion source is 1:10, and mixed ion solution is obtained; wherein, Re is La, Nd, Gd, Dy and Sm;
the second step is that: adding citric acid and ethylene glycol into the mixed ion solution to enable the ratio of the amount of substances of the citric acid to the total amount of ions in the solution to be 2:1, and dropwise adding diluted ammonia water to adjust the pH value to 6-7 to obtain mixed sol;
the third step: removing the solvent in the mixed sol to obtain xerogel;
the fourth step: placing the xerogel in the third step in an air atmosphere, roasting for 5 hours at the roasting temperature of 1000 ℃ and the heating rate of 5 ℃/min, and roasting the cubic fluorite type high-entropy cerium oxide (Dy, Gd, La, Nd, Sm)2Ce2O7Ceramic nano-powder.
Example 6
In this example, a cubic fluorite type high entropy cerium oxide (Dy, Gd, La, Nd, Sm) was prepared at a calcination temperature of 1000 ℃ for 3 hours at a temperature rise rate of 10 ℃/min2Ce2O7Ceramic nano-powder.
The method comprises the following specific steps:
the first step is as follows: five kinds of Re with equal molar ratio2O3Dissolving in nitric acid solution, and dropwise adding Ce (NO)3)3Solution of Re to2O3Total amount of material and Ce (NO)3)3The ratio of the ion source to the ion source is 1:10, and mixed ion solution is obtained; wherein, Re is La, Nd, Sm, Gd and Dy;
the second step is that: adding citric acid and ethylene glycol into the mixed ion solution to enable the ratio of the amount of substances of the citric acid to the total amount of ions in the solution to be 2:1, and dropwise adding diluted ammonia water to adjust the pH value to 6-7 to obtain mixed sol;
the third step: removing the solvent in the mixed sol to obtain xerogel;
the fourth step: placing the xerogel obtained in the third step in an air atmosphere, roasting for 5 hours at the roasting temperature of 1000 ℃ and the heating rate of 10 ℃/min to obtain the cubic fluorite type high-entropy cerium oxide (Dy, Gd, La, Nd, Sm)2Ce2O7Ceramic nano-powder.
Example 7
In this example, a cubic fluorite type high entropy cerium oxide (Er, Gd, La, Sm, Y) was prepared under the conditions of a calcination temperature of 1000 deg.C, a calcination time of 3 hours, and a temperature rise rate of 5 deg.C/min2Ce2O7Ceramic nano-powder.
The method comprises the following specific steps:
the first step is as follows: five kinds of Re with equal molar ratio2O3Dissolving in nitric acid solution, and dropwise adding Ce (NO)3)3Solution of Re to2O3Total amount of material and Ce (NO)3)3The ratio of the ion source to the ion source is 1:10, and mixed ion solution is obtained; wherein, Re ═ Er, Gd, La, Sm and Y;
the second step is that: adding citric acid and ethylene glycol into the mixed ion solution to enable the ratio of the amount of substances of the citric acid to the total amount of ions in the solution to be 2:1, and dropwise adding diluted ammonia water to adjust the pH value to 6-7 to obtain mixed sol;
the third step: removing the solvent in the mixed sol to obtain xerogel;
the fourth step: placing the xerogel obtained in the third step in an air atmosphere, roasting for 3 hours at the roasting temperature of 1000 ℃ and the heating rate of 5 ℃/min to obtain the cubic fluorite high-entropy cerium oxide (Er, Gd, La, Sm and Y)2Ce2O7Ceramic nano-powder.
Example 8
In this example, a cubic fluorite type high entropy cerium oxide (Er, La, Sm, Y, Yb) was prepared at a calcination temperature of 1000 deg.C, a calcination time of 3 hours, and a temperature rise rate of 5 deg.C/min2Ce2O7Ceramic nano-powder.
The method comprises the following specific steps:
the first step is as follows: five kinds of Re with equal molar ratio2O3Dissolving in nitric acid solution, and dropwise adding Ce (NO)3)3Solution of Re to2O3Total amount of material and Ce (NO)3)3The ratio of the ion source to the ion source is 1:10, and mixed ion solution is obtained; where Re ═ La, Er, Sm, Yb, and Y;
the second step is that: adding citric acid and ethylene glycol into the mixed ion solution to enable the ratio of the amount of substances of the citric acid to the total amount of ions in the solution to be 2:1, and dropwise adding diluted ammonia water to adjust the pH value to 6-7 to obtain mixed sol;
the third step: removing the solvent in the mixed sol to obtain xerogel;
the fourth step: placing the xerogel in the third step in air atmosphere, roasting for 3h under the conditions that the roasting temperature is 1000 ℃ and the heating rate is 5 ℃/min, and obtaining the cubic fluorite high-entropy cerium oxide (Er, La, Sm, Y and Yb)2Ce2O7Ceramic nano-powder.
Example 9
In this example, a cubic fluorite type high entropy cerium oxide (Er, Gd, La, Sm, Y) was prepared at a calcination temperature of 1000 deg.C, a calcination time of 3 hours, a temperature rise rate of 5 deg.C/min and an ethanol solvent2Ce2O7Ceramic nano-powder. The method comprises the following specific steps:
the first step is as follows: five kinds of Re with equal molar ratio2O3Dissolving in nitric acid solution, and dropwise adding Ce (NO)3)3Solution of Re to2O3Total amount of material and Ce (NO)3)3The ratio of the ion source to the ion source is 1:10, and mixed ion solution is obtained; wherein, Re ═ Er, Gd, La, Sm and Y;
the second step is that: adding citric acid and ethanol into the mixed ion solution to enable the ratio of the amount of substances of the citric acid to the total amount of ions in the solution to be 2:1, and dropwise adding diluted ammonia water to adjust the pH value to 6-7 to obtain mixed sol;
the third step: removing the solvent in the mixed sol to obtain xerogel;
the fourth step: placing the xerogel obtained in the third step in an air atmosphere, roasting for 3 hours at the roasting temperature of 1000 ℃ and the heating rate of 5 ℃/min to obtain the cubic fluorite high-entropy cerium oxide (Er, Gd, La, Sm and Y)2Ce2O7Ceramic nano-powder.
Example 10
Example A cubic fluorite type high entropy cerium oxide (Er, Gd, La, Sm, Y) was prepared under conditions of a firing temperature of 1000 deg.C, a firing time of 3 hours, a temperature rise rate of 5 deg.C/min and a ratio of the amount of citric acid species to the amount of ionic total species in the solution of 4:12Ce2O7Ceramic nano-powder. The method comprises the following specific steps:
the first step is as follows: five kinds of Re with equal molar ratio2O3Dissolving in nitric acid solution, and dropwise adding Ce (NO)3)3Solution of Re to2O3Total amount of material and Ce (NO)3)3The ratio of the ion source to the ion source is 1:10, and mixed ion solution is obtained; wherein, Re ═ Er, Gd, La, Sm and Y;
the second step is that: adding citric acid and ethanol into the mixed ion solution to enable the ratio of the amount of substances of the citric acid to the total amount of ions in the solution to be 4:1, and dropwise adding diluted ammonia water to adjust the pH value to 6-7 to obtain mixed sol;
the third step: removing the solvent in the mixed sol to obtain xerogel;
the fourth step: placing the xerogel obtained in the third step in an air atmosphere, roasting for 3 hours at the roasting temperature of 1000 ℃ and the heating rate of 5 ℃/min to obtain the cubic fluorite high-entropy cerium oxide (Er, Gd, La, Sm and Y)2Ce2O7Ceramic nano-powder.
The performance test results of the cubic fluorite type high-entropy oxide nano powder prepared by the embodiment of the invention are as follows:
FIG. 2 shows the cubic fluorite-type high entropy oxide nanopowder (Er, Gd, La, Sm, Y) prepared in example 2 above2Ce2O7The powder had a pink color and a true density of 6.036g/cm3。
FIG. 3 shows the cubic fluorite type high entropy oxide ceramic powder (Er, Gd, Sm, Y, Yb) prepared in example 3 above2Ce2O7A microscopic scanning photograph of (a).
Fig. 4 is an XRD spectrum of a series of prepared cubic fluorite-type high-entropy oxide ceramic powders, and it can be seen from the XRD spectrum that the high-entropy oxide ceramic powders have nine diffraction peaks in total between 20 ° and 90 °, and no significant diffraction peak is observed at other positions, which are diffraction peaks of a typical cubic fluorite-type crystal structure, and the parameters of the crystal planes are (111), (200), (220), (311), (222), (400), (331), (420), (422), respectively.
FIG. 5 shows a cubic fluorite type high entropy oxide ceramic (Gd, La, Nd, Sm, Yb) prepared in example 4 above2Ce2O7As can be seen from the element surface distribution diagram of the nano powder, six elements (Gd, La, Nd, Sm, Yb and Ce elements) are uniformly distributed, and the phenomenon of local element enrichment or inferiority does not occur, which indicates that all the elements are uniformly and randomly dispersed in the high-entropy ceramic.
FIG. 6 shows cubic fluorite-type high entropy oxide ceramics (Er, La, Lu, Sc, Sm) prepared in example 92Ce2O7The TG-DSC graph of the nano powder has the test temperature of room temperature to 1200 ℃, the heating rate of 10 ℃/min and the atmosphere of air. As can be seen from the figure, when the high-entropy oxide ceramic nano powder is heated from room temperature to 1200 ℃ in the air atmosphere, the mass change is not more than 0.5 percent, and the heat flow curve shows that the sample has no obvious heat absorption/heat release peak in the range of room temperature to 1200 ℃, which shows that the material is very stable in the temperature range of room temperature to 1200 ℃.
In summary, the chemical molecular formula of a series of cubic fluorite type high-entropy oxide nano-powders disclosed by the invention is Re2Ce2O7Wherein Re is the equal mole ratio combination of any five rare earth metal elements of La, Er, Nd, Sm, Gd, Dy, Yb, Lu, Sc and Y, and the crystal structure is a cubic fluorite structure. The method has the advantages of simple process, high purity of the prepared product, high yield, suitability for large-scale production and adjustable components. The series of high-entropy cerium oxideThe compound nano powder has the advantages of high purity and good high-temperature stability. The invention discloses a series of cubic fluorite type high-entropy oxide nano-powder and a preparation method thereof. The discovery of the series of high-entropy oxides fills the research blank of the high-entropy cerium oxide ceramics, and enriches high-entropy material systems.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (9)
1. A series of cubic fluorite type high-entropy cerium oxide nano-powders are characterized in that the chemical formula of the high-entropy cerium oxide nano-powders is Re2Ce2O7Wherein Re is the rare earth metal elements La, Nd, Er, Sm, Gd, Dy, Yb and Lu, and any five of Sc and Y are combined in an equimolar way;
the high-entropy cerium oxide nano powder is a multi-component single-phase solid solution, and the crystal structure of the high-entropy cerium oxide nano powder is cubic fluorite.
2. A series of cubic fluorite type high entropy cerium oxide nanopowders as claimed in claim 1, wherein the cubic fluorite type high entropy cerium oxide nanopowders have a particle size of 10 to 100 nm.
3. A series of cubic fluorite type high entropy cerium oxide nanopowders according to claim 1, wherein the cubic fluorite type high entropy cerium oxide nanopowders all have a single phase cubic fluorite crystal structure with the elements uniformly distributed.
4. The method for preparing a series of cubic fluorite type high-entropy cerium oxide nanopowders according to any one of claims 1 to 3, comprising the steps of:
1) five kinds of Re with equal molar ratio2O3Dissolving in nitric acid solution, and dropwise adding Ce (NO)3)3Obtaining a mixed ionic solution from the solution; wherein, Re is any one of La, Nd, Er, Sm, Gd, Dy, Yb, Lu, Sc and Y;
2) adding citric acid and a solvent into the mixed ionic solution obtained in the step 1), and adjusting the pH value to 6-7 to obtain mixed sol;
3) removing the solvent in the mixed sol obtained in the step 2) to obtain xerogel;
4) and 3) roasting the dried gel obtained in the step 3) in an air atmosphere to obtain a series of cubic fluorite high-entropy cerium oxide nano-powder.
5. The method for preparing a series of cubic fluorite type high-entropy cerium oxide nanopowders according to claim 4, wherein in step 1), Ce (NO) is used3)3The amount of substance(s) and Re used2O3Is greater than 10.
6. The method for preparing a series of cubic fluorite type high entropy cerium oxide nanopowders according to claim 4, wherein in step 2), the ratio of the amount of citric acid species to the total amount of ionic species in the solution is greater than 2.
7. The method for preparing a series of cubic fluorite type high-entropy cerium oxide nanopowders according to claim 4, wherein in the step 2), the solvent is one or a mixture of ethanol and ethylene glycol.
8. The method for preparing a series of cubic fluorite type high-entropy cerium oxide nanopowders according to claim 4, wherein in the step 4), the sintering temperature is 750-1250 ℃, the sintering time is 1-5 h, and the temperature rise rate is 5-10 ℃/min from room temperature.
9. The method for preparing a series of cubic fluorite type high-entropy cerium oxide nanopowders according to claim 4, wherein the purity of the raw materials used is higher than 99.99%.
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