CN114621763A - Synthesis method of monodisperse high-entropy metal oxide colloid nanocrystalline with adjustable components - Google Patents
Synthesis method of monodisperse high-entropy metal oxide colloid nanocrystalline with adjustable components Download PDFInfo
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Abstract
The invention provides a universal synthetic method for monodisperse high-entropy metal oxide colloid nanocrystalline, which comprises the following steps: dispersing sodium oleate in mixed solvent of ethanol and water, adding five or more metal cations in equal molar ratio, adding n-hexane 60oC, stirring for one hour, separating and collecting a normal hexane phase; then washing for many times by using a mixed solvent of ethanol and water, and then carrying out rotary evaporation to obtain high-entropy metal oleate; finally, the monodisperse metal oxide colloid nanocrystalline is obtained by high-temperature pyrolysis of a solvent method. The invention can prepare various monodisperse high entropiesThe metal oxide colloid nano particles have adjustable components, can be assembled into various structures, and have good application prospect. The synthesis of the monodisperse colloidal metal oxide nano particles with dispersed organic phase is realized for the first time, the blank that the monodisperse high-entropy metal oxide colloidal nano crystals cannot be synthesized at present is filled, and the invention has good inventive and creative significance.
Description
Technical Field
The invention belongs to the field of materials and inorganic chemistry, in particular to a synthesis method of high-entropy metal oxide colloid nanocrystalline, and especially relates to a synthesis method of monodisperse high-entropy metal oxide colloid nanocrystalline with adjustable components.
Background
High entropy metal oxides are a relatively inexpensive class of catalysts with commercial promise, due to the synergistic effect between multiple metals, which tend to have a beneficial catalytic effect. And because of the difference between the atomic radius and the lattice parameter among various metals, the high-entropy metal oxide lattice often has more defects, derives more oxygen vacancies or metal vacancies, and shows better catalytic property, so the high-entropy metal oxide lattice has good commercial application value, is expected to replace the expensive noble metal catalyst in the current commercial application, greatly reduces the cost of the fuel cell, and promotes the development of new energy source business.
At present, various high-entropy metal oxide synthesis methods are developed, and the high-entropy metal oxide is usually obtained by high-temperature pyrolysis in an air atmosphere of metal cation inorganic salt, and has the advantages of no fixed morphology, large particle size, wide distribution, serious agglomeration, less active site exposure and limited catalytic activity. And thus cannot meet the increasing energy demand.
In summary, the existing synthesis methods of high-entropy metal oxides are single, and one method can only synthesize one high-entropy metal oxide. And the prepared two-dimensional sheet has unadjustable appearance, large size distribution and serious agglomeration. Therefore, it is necessary to develop a method for synthesizing monodisperse high-entropy metal oxide colloid nanocrystals with adjustable components.
Disclosure of Invention
The invention aims to provide a synthesis method of a monodisperse high-entropy metal oxide colloid nanocrystalline with adjustable components.
The invention provides a synthesis method of a monodisperse high-entropy metal oxide colloid nanocrystal with adjustable components, which comprises the following specific steps:
(1) dispersing sodium oleate in a mixed solvent consisting of ethanol and water;
(2) slowly adding a mixed solution consisting of five or more than five metal cations with equal molar ratio into the solution obtained in the step (1), and then adding n-hexane solvent with the same volume to obtain a reaction system; the metal cations are five or more of iron ions, manganese ions, cobalt ions, zinc ions, nickel ions, cerium ions, chromium ions, magnesium ions, ruthenium ions or palladium ions;
(3) stirring the reaction system obtained in the step (2) at 50-70 ℃ for reaction for 50-70 minutes, collecting an n-hexane solvent phase, washing the n-hexane solvent phase for a plurality of times by using a mixed solvent consisting of water and ethanol, and then performing rotary evaporation to remove the n-hexane solvent to obtain high-entropy metal oleate;
(4) pyrolyzing the high-entropy metal oleate obtained in the step (3) in an octadecene solvent at high temperature to obtain monodisperse high-entropy metal oxide colloid nanocrystalline; pyrolysis conditions are N2And pyrolyzing at 300-325 ℃ for 1-4 hours in an atmosphere.
In the invention, the metal ion solution in the step (2) is prepared by mixing the following components in a molar ratio of 1: 1: 1: 1: 1 of ferric chloride, manganese chloride, cobalt chloride, zinc nitrate and nickel nitrate.
In the invention, the metal ion solution in the step (2) is prepared by mixing the following components in a molar ratio of 1: 1: 1: 1: 1 of ferric chloride, manganese chloride, cobalt chloride, zinc nitrate and cerium nitrate.
In the invention, the metal ion solution in the step (2) is prepared by mixing the following components in a molar ratio of 1: 1: 1: 1: 1 of ferric chloride, manganese chloride, cobalt chloride, zinc nitrate and magnesium nitrate.
In the invention, the metal ion solution in the step (2) is prepared by mixing the following components in a molar ratio of 1: 1: 1: 1: 1 of ferric chloride, manganese chloride, cobalt chloride, zinc nitrate and ruthenium nitrate.
In the invention, the metal ion solution in the step (2) is prepared by mixing the following components in a molar ratio of 1: 1: 1: 1: 1: 1 of ferric chloride, manganese chloride, cobalt chloride, zinc nitrate, palladium chloride and cerium nitrate.
In the invention, in the step (4), 0.5-4g of oleic acid, 0.5-4g of oleylamine and 1-12g of sodium oleate are added into 4.5-36g of high-entropy metal oleateThen adding 20-160g of octadecene, and carrying out high-temperature pyrolysis reaction under the reaction atmosphere of N2And the temperature rise condition is that the vacuum filtration is carried out for 2-3 hours at the temperature of 100-325 ℃, the reaction is carried out for 1-3 hours at the temperature of 300-325 ℃, finally n-hexane toluene is taken as a solvent, isopropanol ethanol is taken as an anti-solvent, and the anti-solvent is washed for a plurality of times and then is dispersed in the n-hexane, thus obtaining the monodisperse high-entropy metal oxide colloid nanocrystal.
In the invention, the high-entropy metal oxide nanosheet synthesized in the step (4) has size monodispersity, has oleic acid/oleylamine ligands on the surface, can be dispersed in weak-polarity organic solvents such as n-hexane, toluene, chloroform, tetrahydrofuran and the like, and can be assembled into a specific superstructure by intermolecular force of the surface ligands.
The invention has the beneficial effects that: the invention can prepare various monodisperse high-entropy metal oxide colloid nano crystals. The high-entropy metal oxide synthesized by the existing method has no fixed morphology, large particle size, wide distribution, serious agglomeration, less exposure of active sites and limited catalytic activity. Therefore, the invention realizes the synthesis of organic phase dispersed colloidal metal oxide nano particles for the first time and fills the blank that monodisperse high-entropy metal oxide colloidal nano crystals cannot be synthesized at present.
Drawings
FIG. 1 is a transmission electron microscope image of monodisperse FeCoMnZnNi high-entropy metal oxide colloid nanocrystal prepared in example 1;
FIG. 2 is a transmission electron microscope image of an assembled superstructure of monodisperse FeCoMnZnNi high entropy metal oxide colloid nanocrystals prepared in example 1; wherein; (a) 200nm, (b) 100 nm;
FIG. 3 is a transmission electron micrograph of monodisperse FeCoMnZnCe high-entropy metal oxide colloid nanocrystal prepared in example 2;
FIG. 4 is a transmission electron micrograph of monodisperse FeCoMnZnMg high entropy metal oxide colloid nanocrystal prepared in example 3;
FIG. 5 is a transmission electron micrograph of monodisperse FeCoMnZnRu high entropy metal oxide colloidal nanocrystals prepared in example 4;
FIG. 6 is a transmission electron micrograph of monodisperse FeCoMnZnCePd high entropy metal oxide colloid nanocrystal prepared in example 5.
Detailed Description
The invention is further illustrated by the following examples.
Example 1
(1) Dispersing 30-60g of sodium oleate in a mixed solvent of ethanol and water, and dissolving the sodium oleate by ultrasonic waves;
(2) slowly adding a solution obtained in the step (1) into a reaction kettle according to a molar ratio of 1: 1: 1: 1: 1, adding a mixed solution of ferric chloride, manganese chloride, cobalt chloride, zinc nitrate and nickel nitrate, and then adding an n-hexane solvent with the same volume;
(3) reacting the mixed solvent obtained in the step (2) at 60 ℃ for 1 hour, collecting a n-hexane phase, washing the n-hexane phase for multiple times by using an ethanol-water mixed solvent, and performing rotary evaporation to obtain high-entropy Fe-Co-Mn-Zn-Ni oleate;
(4) 4.5-36g of the high-entropy metal oleate obtained in the step (3), 0.5-4g of oleic acid, 0.5-4g of oleylamine and 1-12g of sodium oleate are dissolved in 20-160g of octadecene, vacuum filtration is carried out at the temperature of 100-120 ℃ for 2-3 hours, reaction is carried out at the temperature of 300-325 ℃ for 1-3 hours in a nitrogen atmosphere, finally n-hexane toluene is taken as a solvent, isopropanol ethanol is taken as a counter solvent, and washing and multi-dispersing are carried out in the n-hexane to obtain the monodisperse high-entropy Fe, Co, Mn, Zn and Ni oxidized colloid nanocrystal.
FIG. 1 is a transmission electron microscope image of the FeCoMnZnNiCuxOxOxNiCuxOxOxNiCuxOxOxOxOxOxOxOxOxOxOyNiCuxOxOxOyNiCuxOxOyGaxOxOyNaxOyNanoTexOyNanoTexOyGaxOyNanoCayNanoTexOyNanoTexOyNanoTexOyEx having a good monodispersity. Fig. 2 is a transmission diagram of grain boundary surface assembly and emulsion assembly of the iron-cobalt-manganese-zinc-nickel high-entropy metal oxide colloid nano-crystalline prepared in example 1, and it is proved that the iron-cobalt-manganese-zinc-nickel high-entropy metal oxide colloid nano-crystalline can be prepared into a super structure due to intermolecular force among surface ligands, and has a good application prospect.
Example 2
(1) Dispersing 30-60g of sodium oleate in a mixed solvent of ethanol and water, and dissolving the sodium oleate by ultrasonic waves;
(2) slowly adding the solution obtained in the step (1) into a reaction kettle in a molar ratio of 1: 1: 1: 1: 1, adding a mixed solution of ferric chloride, manganese chloride, cobalt chloride, zinc nitrate and cerium nitrate, and then adding an n-hexane solvent with the same volume;
(3) reacting the mixed solvent obtained in the step (2) at 60 ℃ for 1 hour, collecting a normal hexane phase, washing the normal hexane phase with an ethanol-water mixed solvent for multiple times, and performing rotary evaporation to obtain high-entropy iron-cobalt-manganese-zinc-cerium oleate;
(4) 4.5-36g of the high-entropy metal oleate obtained in the step (3), 0.5-4g of oleic acid, 0.5-4g of oleylamine and 1-12g of sodium oleate are dissolved in 20-160g of octadecene, vacuum filtration is carried out at the temperature of 100-120 ℃ for 2-3 hours, reaction is carried out at the temperature of 300-325 ℃ for 1-3 hours in a nitrogen atmosphere, finally n-hexane toluene is taken as a solvent, isopropanol ethanol is taken as a counter solvent, and the counter solvent is washed for multiple times and then dispersed in the n-hexane to obtain the monodisperse high-entropy iron, cobalt, manganese, zinc and cerium oxide colloid nanocrystalline.
Fig. 3 is a transmission electron microscope image of the fe-co-mn-zn-ce high-entropy metal oxide colloidal nanocrystal prepared in example 2, and the result shows that the fe-co-mn-zn-ce high-entropy metal oxide colloidal nanocrystal has good monodispersity.
Example 3
(1) Dispersing 30-60g of sodium oleate in a mixed solvent of ethanol and water, and dissolving the sodium oleate by ultrasonic waves;
(2) slowly adding the solution obtained in the step (1) into a reaction kettle in a molar ratio of 1: 1: 1: 1: 1, adding a mixed solution of ferric chloride, manganese chloride, cobalt chloride, zinc nitrate and magnesium chloride into an n-hexane solvent with the same volume;
(3) reacting the mixed solvent obtained in the step (2) at 60 ℃ for 1 hour, collecting a n-hexane phase, washing the n-hexane phase for multiple times by using an ethanol-water mixed solvent, and performing rotary evaporation to obtain high-entropy Fe-Co-Mn-Zn-Mg oleate;
(4) 4.5-36g of the high-entropy metal oleate obtained in the step (3), 0.5-4g of oleic acid, 0.5-4g of oleylamine and 1-12g of sodium oleate are dissolved in 20-160g of octadecene, vacuum filtration is carried out at the temperature of 100-120 ℃ for 2-3 hours, reaction is carried out at the temperature of 300-325 ℃ for 1-3 hours in a nitrogen atmosphere, finally n-hexane toluene is taken as a solvent, isopropanol ethanol is taken as a counter solvent, and the counter solvent is washed for multiple times and then dispersed in the n-hexane to obtain the monodisperse high-entropy iron-cobalt-manganese-zinc-magnesium oxide colloid nanocrystal.
FIG. 4 is a transmission electron microscope image of the FeCoMnZnMgCuAlON colloidal nanocrystal prepared in example 3, and the result shows that the FeCoMnZnMgCuAlON colloidal nanocrystal has good monodispersity.
Example 4
(1) Dispersing 30-60g of sodium oleate in a mixed solvent of ethanol and water, and dissolving the sodium oleate by ultrasonic waves;
(2) slowly adding a solution obtained in the step (1) into a reaction kettle according to a molar ratio of 1: 1: 1: 1: 1, adding a mixed solution of ferric chloride, manganese chloride, cobalt chloride, zinc nitrate and ruthenium chloride into an n-hexane solvent with the same volume;
(3) reacting the mixed solvent obtained in the step (2) at 60 ℃ for 1 hour, collecting a normal hexane phase, washing the normal hexane phase with an ethanol-water mixed solvent for multiple times, and performing rotary evaporation to obtain high-entropy Fe-Co-Mn-Zn-Ru oleate;
(4) dissolving 4.5-36g of the high-entropy metal oleate obtained in the step (3), 0.5-4g of oleic acid, 0.5-4g of oleylamine and 1-12g of sodium oleate in 20-160g of octadecene, performing vacuum filtration at 100-120 ℃ for 2-3 hours, reacting at 300-325 ℃ for 1-3 hours in a nitrogen atmosphere, finally taking n-hexane toluene as a solvent, taking isopropanol ethanol as an anti-solvent, washing for multiple times, and dispersing in the n-hexane to obtain the monodisperse high-entropy Fe-Co-Mn-Zn-Ru-O colloidal oxide nanocrystal.
Fig. 4 is a transmission electron microscope image of the high-entropy metal oxide colloid nanocrystalline containing Fe, Co, Mn, Zn and Ru prepared in example 4, and the result shows that the high-entropy metal oxide colloid nanocrystalline containing Fe, Co, Mn, Zn and Ru has good monodispersity.
Example 5
(1) Dispersing 30-60g of sodium oleate in a mixed solvent of ethanol and water, and dissolving the sodium oleate by ultrasonic waves;
(2) slowly adding the solution obtained in the step (1) into a reaction kettle in a molar ratio of 1: 1: 1: 1: 1: 1, adding a mixed solution of ferric chloride, manganese chloride, cobalt chloride, zinc nitrate, palladium chloride and cerium nitrate, and then adding an n-hexane solvent with the same volume;
(3) reacting the mixed solvent obtained in the step (2) at 60 ℃ for 1 hour, collecting an n-hexane phase, washing the n-hexane phase with the ethanol-water mixed solvent for multiple times, and performing rotary evaporation to obtain high-entropy Fe-Co-Mn-Zn-Pd-Ce oleate;
(4) 4.5-36g of the high-entropy metal oleate obtained in the step (3), 0.5-4g of oleic acid, 0.5-4g of oleylamine and 1-12g of sodium oleate are dissolved in 20-160g of octadecene, vacuum filtration is carried out at the temperature of 100-120 ℃ for 2-3 hours, reaction is carried out at the temperature of 300-325 ℃ for 1-3 hours in a nitrogen atmosphere, finally n-hexane toluene is taken as a solvent, isopropanol ethanol is taken as a counter solvent, and the counter solvent is washed for multiple times and then dispersed in the n-hexane to obtain the monodisperse high-entropy Fe-Co-Mn-Zn-Pd-Ce-O colloidal nanocrystal.
Fig. 6 is a transmission electron microscope image of the fe-co-mn-zn-pd-ce high-entropy metal oxide colloidal nanocrystal prepared in example 5, and the result shows that the fe-co-mn-zn-pd-ce high-entropy metal oxide colloidal nanocrystal has good monodispersity.
Claims (8)
1. A synthesis method of monodisperse high-entropy metal oxide colloid nanocrystalline with adjustable components is characterized by comprising the following specific steps:
(1) dispersing sodium oleate in a mixed solvent consisting of ethanol and water;
(2) slowly adding a mixed solution consisting of five or more than five metal cations with equal molar ratio into the solution obtained in the step (1), and then adding n-hexane solvent with the same volume to obtain a reaction system; the metal cations are five or more of iron ions, manganese ions, cobalt ions, zinc ions, nickel ions, cerium ions, chromium ions, magnesium ions, ruthenium ions or palladium ions;
(3) stirring the reaction system obtained in the step (2) at 50-70 ℃ for reacting for 50-70 minutes, collecting an n-hexane solvent phase, washing the n-hexane solvent phase for a plurality of times by using a mixed solvent consisting of water and ethanol, and then performing rotary evaporation on the n-hexane solvent to obtain high-entropy metal oleate;
(4) pyrolyzing the high-entropy metal oleate obtained in the step (3) in an octadecene solvent at high temperature to obtain monodisperse high-entropy metal oxide colloid nanocrystalline; pyrolysis conditions are N2And pyrolyzing at 300-325 ℃ for 1-4 hours in an atmosphere.
2. The method according to claim 1, wherein the metal ion solution in the step (2) is a solution having a molar ratio of 1: 1: 1: 1: 1 of ferric chloride, manganese chloride, cobalt chloride, zinc nitrate and nickel nitrate.
3. The method according to claim 1, wherein the metal ion solution in the step (2) is a solution having a molar ratio of 1: 1: 1: 1: 1 of ferric chloride, manganese chloride, cobalt chloride, zinc nitrate and cerium nitrate.
4. The method according to claim 1, wherein the metal ion solution in the step (2) is a solution having a molar ratio of 1: 1: 1: 1: 1 of ferric chloride, manganese chloride, cobalt chloride, zinc nitrate and magnesium nitrate.
5. The method according to claim 1, wherein the metal ion solution in the step (2) is a solution having a molar ratio of 1: 1: 1: 1: 1 of ferric chloride, manganese chloride, cobalt chloride, zinc nitrate and ruthenium nitrate.
6. The method according to claim 1, wherein the metal ion solution in the step (2) is a solution having a molar ratio of 1: 1: 1: 1: 1: 1 of ferric chloride, manganese chloride, cobalt chloride, zinc nitrate, palladium chloride and cerium nitrate.
7. The process according to claim 1, wherein in the step (4), 4.5 to 36g of high-entropy metal oleate is added with 0.5 to 4g of oleic acid, 0.5 to 4g of oleylamine and 1 to 12g of sodium oleate, and then 20 to 160g of octadecene to conduct pyrolysis reaction at high temperature in the atmosphere of N2The temperature rise condition is 100-oC vacuum filtration for 2-3 hours, 300-oC, reacting for 1-3 hours, finally, washing for many times by using n-hexane and toluene as solvents and isopropanol and ethanol as anti-solvents, and dispersing in the n-hexane to obtain the monodisperse high-entropy metal oxide colloid nanocrystalline.
8. The method as claimed in claim 1, wherein the high-entropy metal oxide nanosheets synthesized in step (4) have monodispersity in size, have oleic acid/oleylamine ligands on the surface, are dispersible in weakly polar organic solvents such as n-hexane, toluene, chloroform, tetrahydrofuran, etc., and can be assembled into a specific superstructure by intermolecular force of the surface ligands.
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| CN115432740A (en) * | 2022-08-31 | 2022-12-06 | 上海旦元新材料科技有限公司 | Preparation method of high-entropy oxide nanoparticle single-layer superlattice |
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| CN112981279A (en) * | 2021-02-04 | 2021-06-18 | 江苏科技大学 | Quinary high-entropy amorphous alloy based on combination of three ternary amorphous alloy elements and preparation method thereof |
| CN113042744A (en) * | 2021-03-11 | 2021-06-29 | 北京大学 | High-entropy alloy nanobelt and preparation method thereof |
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| CN112981279A (en) * | 2021-02-04 | 2021-06-18 | 江苏科技大学 | Quinary high-entropy amorphous alloy based on combination of three ternary amorphous alloy elements and preparation method thereof |
| CN113042744A (en) * | 2021-03-11 | 2021-06-29 | 北京大学 | High-entropy alloy nanobelt and preparation method thereof |
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| CN115432740A (en) * | 2022-08-31 | 2022-12-06 | 上海旦元新材料科技有限公司 | Preparation method of high-entropy oxide nanoparticle single-layer superlattice |
| CN115432740B (en) * | 2022-08-31 | 2024-03-01 | 上海旦元新材料科技有限公司 | Preparation method of high-entropy oxide nanoparticle monolayer superlattice |
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