CN111620681B - Preparation method of high-entropy oxide material - Google Patents
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Abstract
The invention discloses a preparation method of a high-entropy oxide material, which comprises the following steps: 1) dissolving metal nitrate in deionized water, and uniformly stirring; 2) adding a precipitator into the solution obtained in the step 1), and uniformly stirring; 3) carrying out a hydrothermal method on the solution obtained in the step 2) to obtain hydroxide solid powder; 4) and (3) putting the solid powder obtained in the step 3) into a low-temperature plasma reactor for treatment to obtain the high-entropy oxide. The invention adopts liquid-phase ingredients, can ensure that metal elements are uniformly mixed at a molecular level, avoids high-temperature calcination treatment in the synthesis process, obviously reduces energy consumption, has mild reaction conditions, is green and environment-friendly in the reaction process, and hardly causes pollution and waste. The high-entropy oxide material prepared by the invention has uniform appearance, is determined to be a spinel phase according to XRD, and the element content determination shows that the proportion of the contained elements is close to equimolar.
Description
Technical Field
The invention belongs to the technical field of material preparation, and mainly relates to a preparation method of a high-entropy oxide material.
Background
In recent years, high-entropy materials have attracted extensive attention from researchers due to their unique structural and functionally controllable properties. The high-entropy material has an entropy stable crystal structure of more than five metal elements, and the contained elements are almost in equimolar proportion and are uniformly distributed, so that the maximum configuration entropy of a system is ensured. In highly disordered multicomponent systems, high entropy gives rise to attractive properties such as high entropy effects, severe lattice distortion, slow diffusion and cocktail effects, etc. The high-entropy oxide is a novel ceramic material developed based on the concept of high-entropy alloy. In 2015, Rost et al prepared a first example of high entropy oxide (Mg, Ni, Co, Cu, Zn) O by mechanical milling and high temperature calcination, experiments showed that entropy dominates the thermodynamic system and drives reversible solid state transitions between multi-and single-phase (nat. commun., 2015, 6, 8485). However, the preparation method inevitably adopts mechanical grindingThe raw materials are not uniformly mixed, and the designed stoichiometric ratio is difficult to realize; meanwhile, high-temperature calcination has the disadvantage of high energy consumption. Subsequently, Sarkar et al prepared a transition metal high entropy oxide (Co) by spray pyrolysis0.2Cu0.2Mg0.2Ni0.2Zn0.2) And O is applied to the lithium ion battery electrode material, the storage capacity and the charge-discharge cycle stability are remarkably improved (nat. Commun., 2018, 9 and 3400), and the preparation method also has the defect of performing calcination treatment at a high temperature of more than 1000 ℃.
The plasma technology is a method widely applied to material synthesis and modification, and has the advantages of rapid reaction, mild reaction conditions, almost no pollution in the reaction process, waste generation and the like. At present, no report related to the preparation of high-entropy oxide materials by adopting a plasma technology is retrieved.
Disclosure of Invention
Aiming at the defects of the existing high-entropy oxide material preparation technology, the invention provides a method for preparing a high-entropy oxide material by using low-temperature plasma.
The invention provides a preparation method of a high-entropy oxide material, which specifically comprises the following steps:
(1) weighing equimolar metal nitrate, dissolving the metal nitrate in deionized water, and uniformly stirring to obtain a mixed solution of the metal nitrate, wherein the metal nitrate is more than five of ferric nitrate, aluminum nitrate, cobalt nitrate, nickel nitrate, copper nitrate, chromium nitrate and zinc nitrate, and the concentration of the metal nitrate is 0.1-1 mol/L;
(2) weighing a precipitator, adding the precipitator into the mixed solution obtained in the step (1), and uniformly stirring to obtain a mixed solution, wherein the molar ratio of the precipitator to the metal nitrate is 2-5: 1;
(3) transferring the solution obtained in the step (2) to a reaction kettle with a polytetrafluoroethylene lining for heating reaction, cooling to room temperature, then carrying out suction filtration on the reaction solution, and washing with deionized water for 2-4 times to obtain hydroxide solid powder, wherein the temperature of the heating reaction is 100-140 ℃, and the time is 1-2 hours;
(4) and (3) putting the solid powder obtained in the step (3) into a radio frequency plasma reactor for reaction to obtain the high-entropy oxide, wherein the atmosphere of the reaction is oxygen, the radio frequency power is 300-400W, and the reaction time is 20-30 min.
Specifically, the precipitant is one or two of urea, hexamethylenetetramine and arginine.
Compared with the prior art, the invention has the beneficial effects that:
(1) the raw materials are mixed under the condition of liquid phase, so that the metal elements can be uniformly mixed at the molecular level, and the designed stoichiometric ratio of the product is realized;
(2) the prepared high-entropy oxide material is uniform in shape, is determined to be a spinel phase according to XRD, and the element content determination shows that the proportion of the contained elements is close to equimolar;
(3) the synthesis process avoids the use of high-temperature calcination treatment, and the energy consumption is obviously reduced;
(4) the reaction condition is mild, the reaction process is green and environment-friendly, and almost no pollution and waste are generated.
Drawings
FIG. 1 shows (FeAlCoNiZn) prepared in example 13O4XRD pattern of high entropy oxide powder;
FIG. 2 is (FeCrCoNiZn) prepared in example 23O4XRD pattern of high entropy oxide powder;
FIG. 3 is (FeCrCoNiCu) prepared in example 33O4XRD pattern of high entropy oxide powder;
FIG. 4 is (FeCrCoNiCu) prepared in example 33O4SEM image of high entropy oxide powder.
Detailed Description
The invention will be further illustrated by the following examples, which are not intended to limit the scope of the invention
Example 1
2.424 g of Fe (NO) were weighed out3)3·9H2O, 2.25 g of Al (NO)3)3·9H2O, 1.746 g of Co (NO)3)2·6H2O, 1.746 g of Ni (NO)3)2·6H2O, 1.782 g Zn (NO)3)2·6H2Dissolving O in 60 mL of deionized water, and uniformly stirring to obtain a mixed solution of metal salts; then 0.72 g of urea is weighed and added into the mixed solution, and the mixture is stirred uniformly; then transferring the mixed solution into a polytetrafluoroethylene lining reaction kettle, heating to 120 ℃, reacting for 1 h, cooling to room temperature, carrying out suction filtration on the reaction solution, and washing for 3 times by using deionized water to obtain hydroxide solid powder; and finally, putting the solid powder into a low-temperature plasma reactor for reaction for 20 min (the reaction atmosphere is oxygen, and the radio-frequency power is 300W), so as to obtain the high-entropy oxide. XRD spectrum (FIG. 1) shows that (FeAlCoNiZn) is prepared3O4The high entropy oxide is of spinel structure.
Example 2
2.424 g of Fe (NO) were weighed out3)3·9H2O, 2.4 g Cr (NO)3)3·9H2O, 1.746 g of Co (NO)3)2·6H2O, 1.746 g of Ni (NO)3)2·6H2O, 1.782 g Zn (NO)3)2·6H2Dissolving O in 60 mL of deionized water, and uniformly stirring to obtain a mixed solution of metal salts; then 2.52 g of hexamethylenetetramine is weighed and added into the mixed solution, and the mixture is stirred uniformly; then transferring the mixed solution into a polytetrafluoroethylene lining reaction kettle, heating to 140 ℃, reacting for 1 h, cooling to room temperature, carrying out suction filtration on the reaction solution, and washing for 3 times by using deionized water to obtain hydroxide solid powder; and finally, putting the solid powder into a low-temperature plasma reactor for reaction for 20 min (the reaction atmosphere is oxygen, and the radio-frequency power is 400W), so as to obtain the high-entropy oxide. XRD spectrum (FIG. 2) shows that (FeCrCoNiZn) is prepared3O4The high entropy oxide is of spinel structure.
Example 3
2.424 g of Fe (NO) were weighed out3)3·9H2O, 2.4 g Cr (NO)3)3·9H2O, 1.746 g of Co (NO)3)2·6H2O, 1.746 g of Ni (NO)3)2·6H2O、1.45 g of Cu (NO)3)2·6H2Dissolving O in 60 mL of deionized water, and uniformly stirring to obtain a mixed solution of metal salts; then weighing 2.09 g of arginine, adding the arginine into the metal salt mixed solution, and uniformly stirring; then transferring the mixed solution into a polytetrafluoroethylene lining reaction kettle, heating to 100 ℃, reacting for 1 h, cooling to room temperature, carrying out suction filtration on the reaction solution, and washing for 3 times by using deionized water to obtain hydroxide solid powder; and finally, putting the solid powder into a low-temperature plasma reactor for reaction for 20 min (the reaction atmosphere is oxygen, and the radio-frequency power is 400W), so as to obtain the high-entropy oxide. XRD spectrum (FIG. 3) shows that (FeCrCoNiCu) is prepared3O4The high entropy oxide is of spinel structure. SEM picture (FIG. 4) shows that (FeCrCoNiCu) is prepared3O4The high-entropy oxide has uniform appearance. Prepared (FeCrCoNiCu)3O4The ICP-OES test results of the high-entropy oxide metal elements are shown in the table 1;
TABLE 1 preparation of example 3 (FeCrCoNiCu)3O4Content of metal elements in high-entropy oxide
| Element(s) | Content (wt.%) |
| Fe | 5.23 |
| Cr | 5.18 |
| Co | 8.22 |
| Ni | 8.04 |
| Cu | 9.16 |
As shown by the data in Table 1, (FeCrCoNiCu)3O4The molar ratio of metal elements in the high-entropy oxide is Fe: cr: co, Ni, Cu = 0.94, 0.99, 1.39, 1.36, 1.44, contains nearly equimolar proportions of elements, and meets the definition of high entropy materials.
Claims (8)
1. A preparation method of a high-entropy oxide material is characterized by comprising the following steps:
(1) weighing equimolar metal nitrate, dissolving the metal nitrate in deionized water, and uniformly stirring to obtain a mixed solution of metal salts;
(2) weighing a precipitator, adding the precipitator into the solution obtained in the step (1), and uniformly stirring to obtain a mixed solution;
(3) transferring the solution obtained in the step (2) to a reaction kettle with a polytetrafluoroethylene lining for heating reaction, cooling to room temperature, carrying out suction filtration on the reaction solution, and washing to obtain hydroxide solid powder;
(4) and (4) putting the solid powder obtained in the step (3) into a low-temperature plasma reactor for treatment, wherein the reaction atmosphere is oxygen, the radio-frequency power is 300-400W, and the reaction time is 20-30 min, so that the high-entropy oxide is obtained.
2. A method for preparing a high entropy oxide material according to claim 1, wherein in step (1), the metal nitrate is at least five of ferric nitrate, aluminum nitrate, cobalt nitrate, nickel nitrate, copper nitrate, chromium nitrate, and zinc nitrate.
3. A method for preparing a high-entropy oxide material, according to claim 1, wherein in the step (1), the concentration of the metal nitrate is 0.1-1 mol/L.
4. A method for preparing a high entropy oxide material according to claim 1, wherein in step (2), the precipitant is one or two of urea, hexamethylenetetramine and arginine.
5. A method for preparing a high entropy oxide material according to claim 1, wherein in step (2), the molar ratio of the precipitant to the metal nitrate is 2: 1-5: 1.
6. A process for the preparation of a high entropy oxide material according to claim 1, wherein in step (3), the temperature of the heating reaction is 100 to 140 ℃.
7. A process for the preparation of a high entropy oxide material according to claim 1, wherein in step (3), the heating reaction time is 1-2 h.
8. The method for preparing a high-entropy oxide material according to claim 1, wherein in the step (3), the washing is performed 2-4 times by using deionized water.
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| CN112340787B (en) * | 2020-11-09 | 2023-01-24 | 东北大学秦皇岛分校 | Single-phase spinel type high-entropy oxide, preparation method and application |
| CN112599750B (en) * | 2020-12-18 | 2022-02-08 | 安徽工业大学 | Spinel type high-entropy lithium ion negative electrode material containing fluorine-oxygen dianions and preparation method thereof |
| CN113003617B (en) * | 2021-02-26 | 2023-11-14 | 南方科技大学 | Multi-element oxide and preparation method and application thereof |
| CN113149086B (en) * | 2021-04-01 | 2022-03-18 | 南京理工大学 | Two-dimensional high-entropy hydroxide array catalyst and method for synthesizing ammonia by electrocatalysis nitrogen fixation |
| CN113511693B (en) * | 2021-07-19 | 2023-03-14 | 中国科学院兰州化学物理研究所 | Colored spinel type high-entropy oxide (NiFeCrM) 3 O 4 Synthesis method |
| CN113501709B (en) * | 2021-07-19 | 2022-11-01 | 中国科学院兰州化学物理研究所 | Synthesis of spinel-type high-entropy oxide Material (MCoFeCrMn) by hydrothermal method3O4Method (2) |
| CN116692960A (en) * | 2023-04-27 | 2023-09-05 | 江苏大学 | Method for preparing high-entropy hydrotalcite material by utilizing entropy driving chemistry |
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| CN108529689A (en) * | 2018-03-22 | 2018-09-14 | 武汉理工大学 | One kind (CoCrCuNiAl) O entropy stabilizations oxide and its low temperature preparation method |
| CN108933248B (en) * | 2018-07-23 | 2021-02-09 | 安徽工业大学 | Preparation method of spinel-type spherical high-entropy oxide material as negative electrode material of lithium ion battery |
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