CN105110314A - Metal oxide hollow nanometer particle-embedded nitrogen-doped nanometer foamy carbon synthesis method - Google Patents
Metal oxide hollow nanometer particle-embedded nitrogen-doped nanometer foamy carbon synthesis method Download PDFInfo
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Abstract
The invention discloses a metal oxide hollow nanometer particle-embedded nitrogen-doped nanometer foamy carbon synthesis method and belongs to the field of novel energy and novel materials. The synthesis method comprises that through high temperature calcining and low temperature oxidation, the metal oxide hollow nanometer particle-embedded nitrogen-doped nanometer foamy carbon is prepared from metal nitrates as metal oxide precursors and foaming agents, and a nitrogen-containing organic molecule as a carbon source and nitrogen source precursor. The synthesis method utilizes the cheap and easily available organic polymer and a plurality of common metal nitrates as precursors to prepare the metal oxide hollow nanometer particle-embedded nitrogen-doped nanometer foamy carbon. The synthesis method has simple processes, is free of a template, realizes accurate adjustment and control of the foamy carbon structure by change of a metal salt/polyvinylpyrrolidone ratio or calcining conditions, is environmentally friendly and can be industrialized easily. The metal oxide hollow nanometer particle-embedded nitrogen-doped nanometer foamy carbon has a wide application prospect in the fields of energy storage, catalysis, photoelectric materials and drug transport.
Description
Technical field
The present invention relates to a kind of synthetic method of nitrogen-doped nanometer foamy carbon of embedded metal oxide compound Hollow Nanoparticles, belongs to new forms of energy and field of new.
Background technology
Foamy carbon is the functional materials of a class excellent combination property, there is good chemical stability, thermostability, electroconductibility, its lighter quality not only given by inner abundant pore texture, be conducive to the transmission of lotus matter simultaneously, be used widely in fields such as new forms of energy battery (as lithium ion battery), ultracapacitors in recent years.But usual foam carbon material chemical constitution is single, pore size at tens of so that hundreds of micron, pore wall thickness in micron dimension, specific surface area is low, greatly limit the energy storage density of its unit volume/quality, be thus difficult to the demand meeting high energy density cells manufacture.
Metal oxide is with low cost, abundance and of a great variety, and showing unique character in magnetic storage, energy storage and the field such as conversion, catalysis, is the study hotspot that functional materials research field does not wane lastingly.In fields such as new forms of energy battery (as lithium ion battery), ultracapacitors, metal oxide, based on polyelectrons redox reaction, shows the stored energy capacitance far above pure carbon material and density.But the most poorly conductive of metal oxide, and in electrochemical reaction process, structural stability is poor, thus needs with carbon material compound to improve its over-all properties.
Summary of the invention
The object of the present invention is to provide a kind of synthetic method of nitrogen-doped nanometer foamy carbon of embedded metal oxide compound Hollow Nanoparticles.Take metal nitrate as metal oxide precursor and whipping agent, nitrogenous organic molecule is carbon source and nitrogenous source presoma, prepares the synthetic method of the nitrogen-doped nanometer foamy carbon of embedded metal oxide compound Hollow Nanoparticles in conjunction with high-temperature calcination and low-temperature oxidation method.
The technical solution used in the present invention is: a kind of synthetic method of nitrogen-doped nanometer foamy carbon of embedded metal oxide compound Hollow Nanoparticles, comprises the steps:
1) by polyvinylpyrrolidone and metal-salt in mass ratio for 1:0.1-20 dissolves in a solvent, be ground to powder after oven dry;
2) powder obtained in step 1) is placed in reactor at ambient pressure, calcines in rare gas element, calcining temperature is 500-1200
oc, calcination time is 0.2-6 hour, and temperature rise rate is 1-20
ocmin
-1, obtain the nitrogen-doped nanometer foamy carbon of embedded metal oxide nano particles; Described rare gas element is nitrogen, argon gas or helium; Described reactor is glass reactor or tube furnace reactor;
3) by step 2) in the nitrogen-doped nanometer foamy carbon of embedded metal oxide nano particles that obtains at ambient pressure, low temperature calcination in air, calcining temperature is 200-350
oc, calcination time is 0.2-6 hour, obtains the nitrogen-doped nanometer foamy carbon of embedded metal oxide compound Hollow Nanoparticles.
The molecular weight of described polyvinylpyrrolidone is 1 thousand to one hundred three ten ten thousand; Described metal-salt is at least one in iron nitrate, nickelous nitrate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, zinc nitrate, magnesium nitrate, aluminum nitrate, chromium nitrate, cupric nitrate, manganous nitrate and hydrate thereof; Described solvent is at least one in water, methyl alcohol, ethanol.
The nitrogen-doped nanometer foamy carbon of gained embedded metal oxide compound Hollow Nanoparticles is mutually through open bore structure, aperture is 1-100 micron, hole wall thick is the nitrogen-doped carbon nanometer sheet of 10-1000 nanometer, the metal oxide hollow nano particle of embedded 1-100 nanometer in described nitrogen-doped carbon nanometer sheet, the hollow cavity of metal oxide hollow nano particle is 1-10 nanometer; In the nitrogen-doped nanometer foamy carbon of described embedded metal oxide compound Hollow Nanoparticles, carbon content is 20-50%, and nitrogen content is 1-3%, and specific surface area is 200-400m
2g
-1.
Adopt above-mentioned technical scheme, the nitrogen-doped nanometer foamy carbon aperture of embedded metal oxide compound Hollow Nanoparticles obtained is about several microns to some tens of pm, hole wall thick in nanometer scale and embedded size approximate number nanometer to the metal oxide hollow nano particle of tens nanometer.Have benefited from organically blending and having complementary functions of metal oxide, hollow nanostructures and nanometer foam carbon, obtain composite material exhibits and go out excellent electrochemical energy storage performance.Need not use external template, simple and easy to do, environmental protection, energy consumption is low, easy to control and have versatility, can be used for large-scale production.
Beneficial effect of the present invention is: the synthetic method of the nitrogen-doped nanometer foamy carbon of this embedded metal oxide compound Hollow Nanoparticles, take metal nitrate as metal oxide precursor and whipping agent, nitrogenous organic molecule is carbon source and nitrogenous source presoma, prepares the nitrogen-doped nanometer foamy carbon of embedded metal oxide compound Hollow Nanoparticles in conjunction with high-temperature calcination and low-temperature oxidation method.The foamy carbon of the method embedded hollow metal oxide nano particle that uses organic polymer cheap and easy to get and multiple common metal nitrate to be precursor power.Technique is simple, and without the need to using template, can carry out finely regulating by the ratio or calcination condition changing metal-salt/polyvinylpyrrolidone to the structure of foamy carbon, process environmental protection, is easy to large-scale production.The foamy carbon of this embedded metal oxide compound Hollow Nanoparticles is with a wide range of applications in fields such as energy storage, catalysis, photoelectric material, drug delivery.
Accompanying drawing explanation
Fig. 1 is the foamy carbon stereoscan photograph of embedded ferric oxide Hollow Nanoparticles prepared by example 1.
Fig. 2 is the foamy carbon stereoscan photograph of embedded nickel oxide Hollow Nanoparticles prepared by example 2.
Fig. 3 is the foamy carbon stereoscan photograph of embedded cobalt oxide Hollow Nanoparticles prepared by example 3.
Fig. 4 is the foamy carbon stereoscan photograph of embedded cobalt-nickel oxide Hollow Nanoparticles prepared by example 4.
Fig. 5 is the foamy carbon low power transmission electron microscope photo of embedded ferric oxide Hollow Nanoparticles prepared by example 1.
Fig. 6 is the high power transmission electron microscope photo of the foamy carbon of embedded ferric oxide Hollow Nanoparticles prepared by example 1.
Embodiment
embodiment 1
(1) by 1.5g nine water iron nitrate and 1g polyvinylpyrrolidone (K30, molecular weight: 40000) be dissolved in 20mL deionized water, by gained mixing solutions in 100
odrying under C, is powder by gained solid abrasive;
(2) powder of preparation in step (1) is heated to 700 in nitrogen gas stream
oc, controlling temperature rise rate is 20
ocmin
-1, calcination time is 1 hour.After reaction terminates, obtain silver gray foamy carbon macroscopic body;
(3) foamy carbon of preparation in step (2) is heated to 290 in atmosphere
oc, calcination time is 3 hours, obtains the foamy carbon of embedded ferric oxide Hollow Nanoparticles.Its macropore diameter is distributed between 5-8 μm, and hole wall is thick is about 50nm, and carbon content is about 22wt.%, and nitrogen content is about 1%, and specific surface area is 230m
2g
-1.
embodiment 2
(1) by 1.5g six water nickelous nitrate and 1g polyvinylpyrrolidone (K30, molecular weight: 40000) be dissolved in 20mL deionized water, by gained mixing solutions in 100
odrying under C, is powder by gained solid abrasive;
(2) powder of preparation in step (1) is heated to 700 in nitrogen gas stream
oc, controlling temperature rise rate is 5
ocmin
-1, calcination time is 1 hour.After reaction terminates, obtain silver gray foamy carbon macroscopic body;
(3) foamy carbon of preparation in step (2) is heated to 290 in atmosphere
oc, calcination time is 3 hours, obtains the foamy carbon of embedded nickel oxide Hollow Nanoparticles.Its macropore diameter is distributed between 5-10 μm, and hole wall is thick is about 60-100nm, and carbon content is about 29wt.%, and nickel oxide Hollow Nanoparticles size is mainly distributed between 10-40nm.
embodiment 3
(1) by 1.5g cobalt nitrate hexahydrate and 1g polyvinylpyrrolidone (K30, molecular weight: 40000) be dissolved in 20mL deionized water, by gained mixing solutions in 100
odrying under C, is powder by gained solid abrasive;
(2) powder of preparation in step (1) is heated to 700 in nitrogen gas stream
oc, controlling temperature rise rate is 5
ocmin
-1, calcination time is 1 hour.After reaction terminates, obtain silver gray foamy carbon macroscopic body;
(3) foamy carbon of preparation in step (2) is heated to 200 in atmosphere
oc, calcination time is 3 hours, obtains the foamy carbon of embedded ferric oxide Hollow Nanoparticles.Its macropore diameter is about 5-9 μm, and hole wall is thick is about about 70nm, and carbon content is about 24wt.%, and nickel oxide content is about 76wt.%, and cobalt oxide Hollow Nanoparticles size is between 5-15nm, and specific surface area is 260m
2g
-1.
embodiment 4
(1) by 0.75g cobalt nitrate hexahydrate, 0.75g six water nickelous nitrate and 1g polyvinylpyrrolidone (K30, molecular weight: 40000) be dissolved in 20mL deionized water, by gained mixing solutions in 100
odrying under C, is powder by gained solid abrasive;
(2) powder of preparation in step (1) is heated to 700 in nitrogen gas stream
oc, controlling temperature rise rate is 5
ocmin
-1, calcination time is 1 hour.After reaction terminates, obtain silver gray foamy carbon macroscopic body;
(3) foamy carbon of preparation in step (2) is heated to 250 in atmosphere
oc, calcination time is 3 hours, obtains the foamy carbon of embedded cobalt acid nickel Hollow Nanoparticles.Its macropore diameter is about 5-9 μm, and hole wall is thick is about 60nm, and cobalt oxide Hollow Nanoparticles size is between 10-25nm, and carbon content about 22%, specific surface area is about 250m
2g
-1.
Claims (3)
1. a synthetic method for the nitrogen-doped nanometer foamy carbon of embedded metal oxide compound Hollow Nanoparticles, is characterized in that: comprise the steps:
1) by polyvinylpyrrolidone and metal-salt in mass ratio for 1:0.1-20 dissolves in a solvent, be ground to powder after oven dry;
2) powder obtained in step 1) is placed in reactor at ambient pressure, calcines in rare gas element, calcining temperature is 500-1200
oc, calcination time is 0.2-6 hour, and temperature rise rate is 1-20
ocmin
-1, obtain the nitrogen-doped nanometer foamy carbon of embedded metal oxide nano particles; Described rare gas element is nitrogen, argon gas or helium; Described reactor is glass reactor or tube furnace reactor;
3) by step 2) in the nitrogen-doped nanometer foamy carbon of embedded metal oxide nano particles that obtains at ambient pressure, low temperature calcination in air, calcining temperature is 200-350
oc, calcination time is 0.2-6 hour, obtains the nitrogen-doped nanometer foamy carbon of embedded metal oxide compound Hollow Nanoparticles.
2. the synthetic method of the nitrogen-doped nanometer foamy carbon of a kind of embedded metal oxide compound Hollow Nanoparticles according to claim 1, is characterized in that: the molecular weight of described polyvinylpyrrolidone is 1 thousand to one hundred three ten ten thousand; Described metal-salt is at least one in iron nitrate, nickelous nitrate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, zinc nitrate, magnesium nitrate, aluminum nitrate, chromium nitrate, cupric nitrate, manganous nitrate and hydrate thereof; Described solvent is at least one in water, methyl alcohol, ethanol.
3. the synthetic method of the nitrogen-doped nanometer foamy carbon of a kind of embedded metal oxide compound Hollow Nanoparticles according to claim 1, it is characterized in that: the nitrogen-doped nanometer foamy carbon of gained embedded metal oxide compound Hollow Nanoparticles is mutually through open bore structure, aperture is 1-100 micron, hole wall thick is the nitrogen-doped carbon nanometer sheet of 10-1000 nanometer, the metal oxide hollow nano particle of embedded 1-100 nanometer in described nitrogen-doped carbon nanometer sheet, the hollow cavity of metal oxide hollow nano particle is 1-10 nanometer; In the nitrogen-doped nanometer foamy carbon of described embedded metal oxide compound Hollow Nanoparticles, carbon content is 20-50%, and nitrogen content is 1-3%, and specific surface area is 200-400m
2g
-1.
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| CN106006549A (en) * | 2016-06-30 | 2016-10-12 | 上海电力学院 | Heteroatom doped hollow carbon sphere material loaded precious metal nano particle and preparation thereof |
| CN106563484A (en) * | 2016-11-03 | 2017-04-19 | 太原理工大学 | Preparation method of mesoporous hollow nitrogen-doped carbon-coated copper nano catalyst |
| CN106587057A (en) * | 2016-12-20 | 2017-04-26 | 上海应用技术大学 | Preparation method of nitrogen doped porous carbon material and application of preparation method in supercapacitor |
| CN106744802A (en) * | 2017-01-06 | 2017-05-31 | 吉林大学 | Compound duct carbon material of the one-dimensional micropore macropore of bio-based and preparation method thereof |
| CN107824797A (en) * | 2017-10-10 | 2018-03-23 | 广州盈思传感科技有限公司 | Nano-particle modified nitrogen-doped carbon nanometer sheet material of a kind of bismuth of porous high-specific surface area and its preparation method and application |
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| CN109516507A (en) * | 2017-09-18 | 2019-03-26 | 浙江工业大学 | A kind of preparation method of porous cobaltosic oxide nano piece |
| CN109850850A (en) * | 2019-01-23 | 2019-06-07 | 复旦大学 | A kind of general preparative methods of carbon, nitrogen co-doped metal oxide nano-sheet |
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