CN113130161A - Bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticle and preparation method thereof - Google Patents
Bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticle and preparation method thereof Download PDFInfo
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- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/09—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials mixtures of metallic and non-metallic particles; metallic particles having oxide skin
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention relates to a bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticle and a preparation method thereof. The preparation process comprises two steps: by Co2+Synthesizing a precursor of the organic-inorganic hybrid nano-particles with needle-shaped surface and bowknot shape in a solvothermal system under the coordination action of the organic ligand; and then, calcining the mixture in vacuum or inert atmosphere to convert the mixture into bow-tie-shaped nitrogen-doped Co @ C magnetic nanoparticles. The material has large external surface area and good magnetic responsiveness, and can be used as electromagnetic wave absorbent, surface protein imprinting carrier and catalyst carrierBody, etc. has significant advantages when used. Meanwhile, the preparation method is simple in process, easy for large-scale production and has a wide application prospect.
Description
Technical Field
The invention belongs to the field of magnetic carbon materials, and relates to a bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticle and a preparation method thereof.
Background
The magnetic carbon nano-particles are important functional materials and are widely applied as surface protein imprinting carriers, catalyst carriers, electromagnetic wave absorbers and the like. The surface structure of the magnetic carbon nano-particles has important influence on the performance of the magnetic carbon nano-particles, and the surface area of the particles can be increased and a multidirectional reflecting surface can be provided by constructing the convex surface. When the catalyst is used as a surface western blotting carrier and a catalyst carrier material, a larger external surface area can provide more effective sites, and the separation and catalysis efficiency is improved; when the wave absorbing agent is used as a wave absorbing agent, the surface area is increased, the interface polarization capability can be enhanced, meanwhile, the protrusions on the surface can reflect and scatter electromagnetic waves, the propagation path of the electromagnetic waves in the wave absorbing coating is prolonged, and the electromagnetic wave loss capability of the wave absorbing agent is further improved. Therefore, the convex surface is structured to improve the use efficiency of the magnetic carbon nanoparticles.
The general preparation method of the magnetic carbon nano-particles with the convex surfaces is to synthesize a precursor with the convex surfaces and then to perform conversion by high-temperature calcination. At present, the reported preparation methods of the precursor include emulsion polymerization, suspension polymerization, atomization drying self-assembly, liquid-phase electrostatic self-assembly and the like, the surface convex structure mainly takes flower shape, fold shape and raspberry shape, and the whole body takes a spherical shape (201210293149.4, 201811305354.1, 201610566864.9 and 201610239753.7). No relevant work of nitrogen-doped Co @ C magnetic nanoparticles which have acicular convex surfaces and are in a bow-tie shape integrally and a preparation method thereof is seen. Designing and synthesizing the magnetic nano-particles with novel structures and developing a new convex surface construction method have important significance for enriching the types of the magnetic nano-particles with complex surfaces and providing a brand new preparation method thereof.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticle and a preparation method thereof.
Technical scheme
A bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticle is characterized in that: the framework is nitrogen-doped carbon, and the Co nano particles are embedded in the carbon framework, and are in a bowknot shape in overall appearance and have a needle-shaped convex structure on the surface; the radial maximum size of the nano particles is 1-3 mu m, the radial minimum size is 0.5-2.5 mu m, the axial size is 2-5 mu m, and the deviation of the axial size and the radial size among single-kettle products is less than 0.2 mu m; the magnetic content is 30-40%.
A preparation method of the bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticle is characterized by comprising the following steps:
step 1: dissolving nitrilotriacetic acid in N, N' -dimethyl formamide DMF under the assistance of ultrasound to obtain a solution I, wherein the concentration of the nitrilotriacetic acid in the solution I is 0.08-0.2 mol/L;
step 2: dissolving cobalt salt in DMF under the assistance of ultrasound to obtain a solution II, wherein the concentration of the cobalt salt in the solution II is 0.15-0.3 mol/L;
and step 3: adding the solution II into the solution I under magnetic stirring, adding concentrated nitric acid into the solution I, and fully mixing to obtain a mixed solution III; wherein the volume ratio of the solution I to the solution II to the concentrated nitric acid is 1: 0.5-1.5: 0.005-0.015;
and 4, step 4: transferring the solution III into a stainless steel reaction kettle with a polytetrafluoroethylene lining, placing the stainless steel reaction kettle in a blast oven, setting the reaction temperature to be 110-140 ℃, and preserving the heat for 6-12 hours;
and 5: cooling to room temperature after the reaction is finished, performing centrifugal separation, washing with DMF for multiple times, and drying to obtain the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces;
step 6: calcining the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces in a tubular furnace for 2-6h to convert the particles into bowknot-shaped nitrogen-doped Co @ C magnetic nano-particles, wherein the calcining atmosphere is vacuum or inert gas, and the calcining temperature is 550-800 ℃.
The washing with DMF in the step 5 is carried out 3 times.
The cobalt salts include, but are not limited to: cobalt chloride, cobalt acetate, cobalt nitrate, cobalt sulfate and hydrates of the foregoing.
Advantageous effects
The invention provides a bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticle and a preparation method thereof. The preparation process comprises two steps: by Co2+Synthesizing a precursor of the organic-inorganic hybrid nano-particles with needle-shaped surface and bowknot shape in a solvothermal system under the coordination action of the organic ligand; and then, calcining the mixture in vacuum or inert atmosphere to convert the mixture into bow-tie-shaped nitrogen-doped Co @ C magnetic nanoparticles. The material has larger external surface area and good magnetic responsiveness, and has remarkable advantages when being used as an electromagnetic wave absorbent, a surface protein imprinting carrier, a catalyst carrier and the like. Meanwhile, the preparation method is simple in process, easy for large-scale production and has a wide application prospect.
In the complex forming process, the final appearance of the product is determined by the combination mode of the central ions and the ligand molecules. Selecting Co in the invention2+As a central ion, the nitrilotriacetic acid is an organic ligand, and the specific combination mode of the nitrilotriacetic acid and the nitrilotriacetic acid is a precondition for forming a bowtie-shaped organic-inorganic hybrid nanoparticle precursor with a needle-shaped surface. In addition, the solvent is selected to be N, N '-dimethylformamide, and nitric acid with a specific concentration is added into the N, N' -dimethylformamide, so that a proper solution environment is provided while the reaction raw materials are dissolved, and the deprotonation degree of the ligand nitrilotriacetic acid is regulated, which is very important for the formation of a bowtie-shaped structure with a needle-shaped surface. The reaction system adopted by the invention is finally determined through design and repeated verification, is a necessary condition for preparing the precursor of the needle-shaped surface bow-shaped organic-inorganic hybrid nano-particles, and has originality. Moreover, the microstructure of the precursor can be regulated and controlled by properly adjusting the formula and the process, the particle size, the density, the number and the like of the needle-shaped structures can be correspondingly changed according to the application requirements, and the precursor has strong adaptability as shown in the attached drawing 1.
The precursor is calcined in vacuum or inert atmosphere and then converted into the needle-shaped surface bowknot-shaped nitrogen-doped Co @ C magnetic nano-particle, and the unique needle-shaped surface bowknot-shaped structure of the precursor is not reported before and has originality. Compared with the common spherical, square and polyhedral particles, the structure has larger external surface area and has superiority in application scenes of electromagnetic wave absorbers, surface western blot carriers, catalyst carriers and the like.
Drawings
FIG. 1 SEM (A-C) and TEM (D) photographs of a precursor of organic-inorganic hybrid nanoparticles having a needle-like surface and a bowtie shape, wherein A and D correspond to example 3, B corresponds to example 4, and C corresponds to example 6
FIG. 2 is SEM (A) and TEM (B) photographs of bow-tie nitrogen-doped Co @ C magnetic nanoparticles, corresponding to example 3
FIG. 3 shows XRD spectrum (A) and VSM curve (B) of bow-tie-shaped nitrogen-doped Co @ C magnetic nanoparticles, corresponding to example 3
FIG. 4 is an adsorption-desorption isotherm (A) and a pore size distribution curve (B) of a bowtie-shaped nitrogen-doped Co @ C magnetic nanoparticle, wherein the BET surface area is 51.55m2Per g, average pore diameter: 18.73nm, corresponding to example 3
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1: preparation of bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticles
Dissolving 0.65g of nitrilotriacetic acid in 40mL of DMF under the assistance of ultrasound to obtain a solution I, and dissolving 0.52g of cobalt chloride in 20mL of DMF to obtain a solution II; adding the solution II into the solution I under magnetic stirring, adding 0.20mL of concentrated nitric acid into the solution I, and fully mixing to obtain a solution III; transferring the solution III into a stainless steel reaction kettle with a 100mL polytetrafluoroethylene lining, placing the stainless steel reaction kettle in a blast oven, setting the reaction temperature to be 110 ℃, and preserving the heat for 6 hours; after the reaction is finished, cooling to room temperature, centrifugally separating, washing for 3 times by using DMF, and drying to obtain the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces; calcining the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces in a tube furnace at 550 ℃ for 6h in a nitrogen atmosphere, and cooling along with the furnace to obtain the bowknot-shaped nitrogen-doped Co @ C magnetic nano-particles.
Example 2: preparation of bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticles
Dissolving 2.85g of nitrilotriacetic acid in 100mL of DMF with the aid of ultrasound to obtain a solution I, and dissolving 3.95g of cobalt acetate tetrahydrate in 80mL of DMF to obtain a solution II; adding the solution II into the solution I under magnetic stirring, adding 0.75mL of concentrated nitric acid into the solution I, and fully mixing to obtain a solution III; transferring the solution III into a stainless steel reaction kettle with a 250mL polytetrafluoroethylene lining, placing the stainless steel reaction kettle in a blast oven, setting the reaction temperature to be 120 ℃, and preserving the heat for 10 hours; after the reaction is finished, cooling to room temperature, centrifugally separating, washing for 3 times by using DMF, and drying to obtain the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces; calcining the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces in a 800 ℃ tubular furnace for 2h in an argon atmosphere, and cooling along with the furnace to obtain the bowknot-shaped nitrogen-doped Co @ C magnetic nano-particles.
Example 3: preparation of bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticles
Under the assistance of ultrasound, 0.31g of aminotriethoxylate is dissolved in 15mL of DMF to obtain a solution I, and 0.68g of cobalt chloride hexahydrate is dissolved in 15mL of DMF to obtain a solution II; adding the solution II into the solution I under magnetic stirring, adding 0.18mL of concentrated nitric acid into the solution I, and fully mixing to obtain a solution III; transferring the solution III into a 50mL stainless steel reaction kettle with a polytetrafluoroethylene lining, placing the stainless steel reaction kettle in a blast oven, setting the reaction temperature to be 120 ℃, and preserving the heat for 12 hours; after the reaction is finished, cooling to room temperature, centrifugally separating, washing for 3 times by using DMF, and drying to obtain the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces; calcining the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces in a tube furnace at 600 ℃ for 5h in a vacuum atmosphere, and cooling along with the furnace to obtain the bowknot-shaped nitrogen-doped Co @ C magnetic nano-particles.
Example 4: preparation of bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticles
Dissolving 3.69g of nitrilotriacetic acid in 160mL of DMF with the aid of ultrasound to obtain a solution I, and dissolving 7.80g of cobalt chloride hexahydrate in 140mL of DMF to obtain a solution II; adding the solution II into the solution I under magnetic stirring, adding 1.50mL of concentrated nitric acid into the solution I, and fully mixing to obtain a solution III; transferring the solution III into a 500mL stainless steel reaction kettle with a polytetrafluoroethylene lining, placing the stainless steel reaction kettle in a blast oven, setting the reaction temperature to be 120 ℃, and preserving the heat for 12 hours; after the reaction is finished, cooling to room temperature, centrifugally separating, washing for 3 times by using DMF, and drying to obtain the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces; calcining the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces in a 700 ℃ tubular furnace for 4h in a nitrogen atmosphere, and cooling along with the furnace to obtain the bowknot-shaped nitrogen-doped Co @ C magnetic nano-particles.
Example 5: preparation of bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticles
Under the assistance of ultrasound, 1.14g of aminotriethoxylate is dissolved in 30mL of DMF to obtain a solution I, and 1.52g of cobalt sulfate heptahydrate is dissolved in 30mL of DMF to obtain a solution II; adding the solution II into the solution I under magnetic stirring, adding 0.35mL of concentrated nitric acid into the solution I, and fully mixing to obtain a solution III; transferring the solution III into a stainless steel reaction kettle with a 100mL polytetrafluoroethylene lining, placing the stainless steel reaction kettle in a blast oven, setting the reaction temperature to be 135 ℃, and preserving the heat for 8 hours; after the reaction is finished, cooling to room temperature, centrifugally separating, washing for 3 times by using DMF, and drying to obtain the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces; calcining the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces in a tube furnace at 750 ℃ for 2.5h in a vacuum atmosphere, and cooling along with the furnace to obtain the bowknot-shaped nitrogen-doped Co @ C magnetic nano-particles.
Example 6: preparation of bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticles
Dissolving 1.53g of nitrilotriacetic acid in 100mL of DMF with the aid of ultrasound to obtain a solution I, and dissolving 6.75g of cobalt nitrate in 80mL of DMF to obtain a solution II; adding the solution II into the solution I under magnetic stirring, adding 0.70mL of concentrated nitric acid into the solution I, and fully mixing to obtain a solution III; transferring the solution III into a stainless steel reaction kettle with a 250mL polytetrafluoroethylene lining, placing the stainless steel reaction kettle in a blast oven, setting the reaction temperature to be 120 ℃, and preserving the heat for 10 hours; after the reaction is finished, cooling to room temperature, centrifugally separating, washing for 3 times by using DMF, and drying to obtain the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces; calcining the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces in a 650 ℃ tubular furnace for 4h in a nitrogen atmosphere, and cooling along with the furnace to obtain the bowknot-shaped nitrogen-doped Co @ C magnetic nano-particles.
Claims (4)
1. A bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticle is characterized in that: the framework is nitrogen-doped carbon, and the Co nano particles are embedded in the carbon framework, and are in a bowknot shape in overall appearance and have a needle-shaped convex structure on the surface; the radial maximum size of the nano particles is 1-3 mu m, the radial minimum size is 0.5-2.5 mu m, the axial size is 2-5 mu m, and the deviation of the axial size and the radial size among single-kettle products is less than 0.2 mu m; the magnetic content is 30-40%.
2. A method for preparing the bowknot-shaped nitrogen-doped Co @ C magnetic nanoparticles as claimed in claim 1, which is characterized by comprising the following steps:
step 1: dissolving nitrilotriacetic acid in N, N' -dimethyl formamide DMF under the assistance of ultrasound to obtain a solution I, wherein the concentration of the nitrilotriacetic acid in the solution I is 0.08-0.2 mol/L;
step 2: dissolving cobalt salt in DMF under the assistance of ultrasound to obtain a solution II, wherein the concentration of the cobalt salt in the solution II is 0.15-0.3 mol/L;
and step 3: adding the solution II into the solution I under magnetic stirring, adding concentrated nitric acid into the solution I, and fully mixing to obtain a mixed solution III; wherein the volume ratio of the solution I to the solution II to the concentrated nitric acid is 1: 0.5-1.5: 0.005-0.015;
and 4, step 4: transferring the solution III into a stainless steel reaction kettle with a polytetrafluoroethylene lining, placing the stainless steel reaction kettle in a blast oven, setting the reaction temperature to be 110-140 ℃, and preserving the heat for 6-12 hours;
and 5: cooling to room temperature after the reaction is finished, performing centrifugal separation, washing with DMF for multiple times, and drying to obtain the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces;
step 6: calcining the bowknot-shaped organic-inorganic hybrid nano-particles with the needle-shaped surfaces in a tubular furnace for 2-6h to convert the particles into bowknot-shaped nitrogen-doped Co @ C magnetic nano-particles, wherein the calcining atmosphere is vacuum or inert gas, and the calcining temperature is 550-800 ℃.
3. The method of claim 2, wherein: the washing with DMF in the step 5 is carried out 3 times.
4. The method of claim 2, wherein: the cobalt salts include, but are not limited to: cobalt chloride, cobalt acetate, cobalt nitrate, cobalt sulfate and hydrates of the foregoing.
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