CN105032355A - Preparation method for core-shell structure type carbon-coated magnetic nano particles - Google Patents
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Abstract
The invention discloses a preparation method for core-shell structure type carbon-coated magnetic nano particles. The method comprises the following steps: preparing metal hydroxide or metal oxide nano particles having different morphologies by adopting a hydrothermal method; modifying the surfaces of the particles; coating the nano particles by adopting a similar method (described in the specification) so as to obtain phenolic resin-coated metal oxide or metal hydroxide nano composite particles; and performing calcining and carbonizing on the obtained nano composite particles to obtain the carbon-coated magnetic nano particles. The carbon-coated magnetic nano particles prepared by adopting the method disclosed by the invention are good in dispersibility, uniform in particle size and high in stability, and have graded porous core-shell structures; in the calcining process, the morphologies of the core-shell metal hydroxide or metal oxide nano particles can be kept unchanged; the particle diameters of the nano particles and the coating thickness of a carbon layer can be adjusted according to needs. The core-shell structure type composite particles prepared by adopting the method disclosed by the invention have a superpara magnetism adsorption property, and under the action of an external magnetic field, the fast separation can be realized, so that the core-shell structure type composite particles can be expected to be applied in the fields of magnetic separation and catalyzing.
Description
Technical field
The invention belongs to functional composite material preparation field, relate to the preparation method of a kind of porous, nucleocapsid structure transition metal carbon magnetic nanometer particles, specifically with metal hydroxides or metal oxide for core, surfactant is modified its surface, it is coated to it that carbon source made by phenolic resins, obtains the preparation method of carbon-coated magnetic particle through calcining.
Background technology
Nanoscale Iron, cobalt, nickel powder is as transition metal material, except the small-size effect with nano particle self, quantum tunneling effect, Magic number structure, quantum size effect, outside the physicochemical properties of a series of uniqueness such as skin effect, also there is unique surface characteristic, hydrogenating catalytic, chemical property, microwave-absorbing and ferromagnetism etc., at coating material, catalytic chemistry, electrochemistry, absorbing material, electromagnetic shielding material, the application aspect such as Infrared stealthy materials and magnetic recording material has broad application prospects, it is one of focus of domestic and international New function developing material.But metal nanoparticle is faced with a common issue in actual applications, namely nano metal particles has high specific area and surface energy, and the gathering because Van der Waals force causes easily occurs, and the reunion of metal nanoparticle has a strong impact on its application performance.By carrying out modification to surfaces of metal nanoparticles, particle surface properties is changed can effectively address this problem, namely at other material of coated with uniform one deck of nano particle, the nano particle of the nucleocapsid structure formed after Surface coating, its surface property, stability all can obtain improvement to a certain extent.In addition, the existence of clad can not only stop nano particle oxidation, crystal is grown up, corrodes and reunited, and can also give core-shell particles special performance, widens applications to nanostructures field further.
1993, the reported first such as Rouff research group of the U.S. and the Japanese Tomita structure of the coated La of carbon.After this, carbon-clad metal nano material (Carbonencapsulatedmetalnanoparticles, MC) as a kind of novel metal/carbon composite nano materials, the research of its preparation, performance and application becomes rapidly the study hotspot of carbon science and material science.This carbon-clad metal particle (CEMNP); there is unique physics, chemical property; the coated of carbon-coating has important protective effect to nano metal particles; greatly expand the range of application of this kind of nano-metal particle material, made it have huge potential using value at numerous areas such as chemistry, material, physics.
Up to now, about the preparation method of MC nano particle, mainly comprise arc discharge method (JeyadevanB, SuzukiY, TohjiK, etal.Encapsulationofnanoparticlesbysurfactantreduction [J] .MaterialsScienceandEngineering:A, 1996, 217:54-57), laser method (HayashiT, HironoS, TomitaM, etal.Magneticthinfilmsofcobaltnanocrystalsencapsulatedin graphite-likecarbon [J] .1996), chemical vapour deposition (CVD) (SanoN, AkazawaH, KikuchiT, etal.Separatedsynthesisofiron-includedcarbonnanocapsules andnanotubesbypyrolysisofferroceneinpurehydrogen [J] .Carbon, 2003, 41 (11): 2159-2162), Detonation Process (WuW, ZhuZ, LiuZ, etal.Preparationofcarbon-encapsulatedironcarbidenanopart iclesbyanexplosionmethod [J] .Carbon, 2003, 41 (2): 317-321) etc.All there is certain shortcoming in said method: arc process is because arc temperature is up to 4000K, inevitably there are (as CNT, fullerene and carbon black etc.) with accessory substance in product, the purity of product is caused to reduce, and equipment is comparatively complicated, technological parameter is wayward, power consumption is large, and cost is high, is thus difficult to realize extensive synthesis; Laser method equipment needed thereby costly, makes it be greatly limited in application; The size and distribution of chemical vapour deposition technique gained Carbon-encapsulated Metal Nanoparticles CEMNP is very large by the granular size and distribution influence thereof of reacting the metallic catalyst of front spreading on substrate, generally prepare the particle diameter smaller (20 ~ 80nm) of particle, and in product except CEMNP, also can simultaneously Formed nanotube and unbodied carbon granule, purity is lower; Detonation Process preparation process more complicated, particularly early stage explosive preparation, and process is not easy to operate and control, and there is higher risk, and extensive synthesis is restricted.
Summary of the invention
The problems such as to be solved by this invention is that prior art is being prepared in carbon-clad metal nano material process, and equipment is complicated, process controllability purity that is poor, product is low.
In order to solve the problem, the invention provides a kind of preparation method of nucleocapsid structure carbon-clad metal magnetic nanometer particles, it is characterized in that, specifically implement according to following steps:
Step 1): under room temperature ultrasound condition, joined by alkaline agent in the aqueous solution of the transition metal salt of preparation, 90 ~ 110 DEG C of Water Under thermal responses, prepare the solution of transition metal hydroxide;
Step 2): to step 1) add surfactant polyacrylic acid in the solution that obtains, ultrasonicly carry out finishing, centrifugal washing dispersion;
Step 3): to step 2) add carbon source presoma, ammoniacal liquor successively in the dispersion liquid that obtains, stir, centrifuge washing, in 70 ~ 90 DEG C of oven dry, obtains the nanoparticle of the coated metal oxide of phenolic resins;
Step 4): by step 3) pressed powder that obtains is placed in tube furnace, in 600 ~ 900 DEG C of calcining 2 ~ 3h under atmosphere of inert gases, obtains carbon-coated magnetic nanoparticle.
Preferably, described step 1) in transition metal be any one or a few in Fe, Co and Ni.
Preferably, described step 1) in time of thermal response be 2 hours.
Preferably, described step 2) in time of ultrasonic reaction be 2 hours.
Preferably, described step 2) in surfactant be polyacrylic acid.
Preferably, described step 3) carbon source presoma be phenolic resins.
Preferably, described step 3) in stir design parameter be: at 50 DEG C stir 2 hours.
Preferably, described step 4) in inert gas be argon gas or nitrogen.
Preferably, described step 4) obtained carbon-coated magnetic nanoparticle pattern is any one or a few in nanosphere, nanometer sheet, nanometer rods, nanocube and nanotube, and is regular pattern, monodispersed core-shell structural.
It is core that the present invention proposes a kind of surfactant modified transition metal hydroxide or metal oxide of utilizing, coated to it through carbon source precursor, high-temperature calcination again, the method of the magnetic metal carbon Nano Composite Particles of preparation porous nucleocapsid structure, namely with the metal hydroxides of multiform looks or metal oxide for core, modify through surfactant, with resorcinol and formaldehyde for raw material is through class
method, at its Surface coating continuous print carbon source layer, obtains magnetic Nano composite particles after calcining under an inert atmosphere.The method under the reaction condition of gentleness, can take water as solvent, prepares high stability, single dispersing quickly and easily, has magnetic metal carbon Nano Composite Particles that is classifying porous and nucleocapsid structure.And can according to actual needs, the coated thickness of the particle diameter of flexible modulation stratum nucleare nano particle, pattern and shell carbon structure, specific surface size and carbonizing degree thereof.The preparation method that the present invention adopts is simple and feasible, and favorable reproducibility.
Compared with prior art, beneficial effect of the present invention is:
1, the magnetic adsorptive material that obtains of the inventive method, has classifying porous nucleocapsid structure, Stability Analysis of Structures, good dispersion, uniform particle sizes, and specific surface and at 240m
2/ more than g.
2, the core-shell structure nanometer particle that obtains of the inventive method, because its carbon-coating has graded porous structure, thus has good absorption property.
3, this nucleocapsid structure granule for absorbing has excellent superparamagnetism, can realize quick separating, do not produce secondary pollution under extraneous magnetic fields.
4, this core-shell structure magnetic granule for absorbing, can according to actual needs, coated degree, specific area, the pore size of the pattern of flexible modulation stratum nucleare particle, particle diameter and shell carbon.Both can be applied to the preparation of different-grain diameter M carbon magnetic nanometer particles, also can be applied to the preparation of the magnetic nanometer particles of different shell thickness.
5, compared with the technology of other synthetic kernel shell structure magnetic particles, the controllability that the method prepares core-shell structure particle is strong, simple to operate, and reaction condition is gentle, and favorable reproducibility, cost is low.
Accompanying drawing explanation
Fig. 1 is Ni (OH) in embodiment 1,2
2transmission electron microscope picture;
Fig. 2 is in embodiment 1, Ni (OH)
2the transmission electron microscope picture of RF Nano Composite Particles;
Fig. 3 is in embodiment 1, the transmission electron microscope picture of NiC Nano Composite Particles;
Fig. 4 is in embodiment 2, Ni (OH)
2the transmission electron microscope picture of RF Nano Composite Particles;
Fig. 5 is in embodiment 2, the transmission electron microscope picture of NiC Nano Composite Particles;
Fig. 6 is in embodiment 1, nitrogen adsorption desorption curve (a) of NiC Nano Composite Particles and pore-size distribution (b);
Fig. 7 is in embodiment 1, the XRD figure of NiC Nano Composite Particles;
Fig. 8 is in embodiment 1, the hysteresis curve of NiC Nano Composite Particles.
Detailed description of the invention
For making the present invention become apparent, hereby with preferred embodiment, and accompanying drawing is coordinated to be described in detail below.
Embodiment 1
200mL tri-distilled water, 0.5816g six water nickel nitrate, 0.30mL concentrated ammonia liquor are inserted in 450mL hydrothermal reaction kettle successively, in 90 DEG C of reaction 120min, obtains Ni (OH)
2nanometer sheet.Subsequently, dropwise add 6mL7.2mg/mL polyacrylic acid (PAA) surfactant, ultrasonic disperse 120min, centrifugal washing, is scattered in water.Transmission electron microscope observing shows, the Ni (OH) that hydro-thermal method obtains
2nano particle is monodispersed regular hexagon laminated structure, and diameter is about 90nm, and thickness is about 5nm, as shown in Figure 1.
By 0.5mL0.908mol/L resorcinol (R) solution, 0.07mL formaldehyde (F) solution, 0.4mL weak aqua ammonia joins 60mLNi (OH) successively
2in dispersion liquid, at 50 DEG C, stirring reaction 120min under 400rpm rotating speed.Centrifuge washing, obtains Ni (OH)
2rF Nano Composite Particles.Through transmission electron microscope observing display, particle has obvious nucleocapsid structure, and keeps the regular hexagon sheet-like morphology of original stratum nucleare structure, and coating thickness is 20 ~ 25nm, as shown in Figure 2.
By above-mentioned Ni (OH)
2rF dispersion liquid is placed in the oven dry of 70 DEG C, baking oven, grinds to form solid, powdery, puts it in tube furnace, in the lower 900 DEG C of calcining 120min of nitrogen atmosphere, obtains NiC Nano Composite Particles.Through transmission electron microscope observing display, particle has obvious nucleocapsid structure, and stratum nucleare metal presents loose structure, and shell structurre is continuous whole, and shell thickness is 15 ~ 20nm, as shown in Figure 3.
Embodiment 2
200mL tri-distilled water, 0.5816g six water nickel nitrate, 0.30mL concentrated ammonia liquor are inserted in 450mL hydrothermal reaction kettle successively, in 90 DEG C of reaction 120min, obtains Ni (OH)
2nanometer sheet.Subsequently, dropwise add 6mL7.2mg/mL polyacrylic acid (PAA) surfactant, ultrasonic disperse 120min, centrifugal washing, is scattered in water.Transmission electron microscope observing shows, the Ni (OH) that hydro-thermal method obtains
2nano particle is monodispersed regular hexagon laminated structure, and diameter is about 90nm, and thickness is about 5nm.
By the R solution of 0.25mL0.908mol/L, the F solution of 0.035mL, 0.4mL weak aqua ammonia joins 60mLNi (OH) successively
2in dispersion liquid, at 50 DEG C, stirring reaction 120min under 400rpm rotating speed.Centrifuge washing, obtains Ni (OH)
2rF Nano Composite Particles.Through transmission electron microscope observing display, particle has obvious nucleocapsid structure, and keeps the regular hexagon sheet-like morphology of original stratum nucleare structure, and coating thickness is 10 ~ 15nm, as shown in Figure 4.
By above-mentioned Ni (OH)
2rF dispersion liquid is placed in the oven dry of 70 DEG C, baking oven, grinds to form solid, powdery, puts it in tube furnace, in the lower 900 DEG C of calcining 120min of nitrogen atmosphere, obtains NiC Nano Composite Particles.Through transmission electron microscope observing display, particle has obvious nucleocapsid structure, and stratum nucleare metal presents loose structure, and shell structurre is continuous whole, and shell thickness is 6 ~ 8nm, as shown in Figure 5.
Fe, Co, Ni are period 4 group VIII elements, and its physicochemical properties are similar.The present invention prepares the method for NiC Nano Composite Particles and application is equally applicable to FeC, CoC nanoparticle.At present, different-shape Fe is studied
2o
3or Fe
3o
4, Co (OH)
2the preparation method of nanoparticle is many, and wherein hydro-thermal method is simple to operate due to it, and Application comparison is extensive.In the present invention, preparation Fe, Co hydroxide or oxides nanoparticles method all adopt conventional hydrothermal method route (this technology is prior art); Subsequent preparation process: the coated and carbonization method of Fe, Co, Ni hydroxide or oxides nanoparticles finishing, RF, be technological core of the present invention, its operating process is all identical with NiC method, so the relevant embodiment of unlisted Fe, Co.What in patent, we listed emphatically the NiC Nano Composite Particles of different shell thickness prepares example.
Fig. 6 is NiC adsorption-desorption curve.As seen from the figure, the specific area of this particle is 247.1m
2/ g, and there is classification meso-hole structure, primary aperture is distributed in little mesoporous 3 nanometers and large mesoporous 50 ran.
Analyzed from Fig. 7, the angle of diffraction of 26 ° corresponds to (002) crystal face of graphite-structure, and material with carbon element graphitization is described; Be 45 ° in the angle of diffraction, the diffraction maximum of 52 ° and 76 ° corresponds respectively to (111) of metallic nickel, and the diffraction of (200) and (220) crystal face, shows through carbonisation, β-Ni (OH)
2be transformed into Ni.
Fig. 8 shows, Ni and NiC nanoparticle all has certain superparamagnetic performance.Compared with Ni particle, due to the existence of carbon shell structurre, the saturation magnetization of NiC nanoparticle is down to 6.54emu/g by original 8.55emu/g.Embedding figure shows further, when magnet is near nanoparticle, just can complete adsorption process through the time less than 10 seconds.
Claims (9)
1. a preparation method for nucleocapsid structure carbon-clad metal magnetic nanometer particles, is characterized in that, specifically implements according to following steps:
Step 1): under room temperature ultrasound condition, joined by alkaline agent in the aqueous solution of the transition metal salt of preparation, 90 ~ 110 DEG C of Water Under thermal responses, prepare the solution of transition metal hydroxide;
Step 2): to step 1) add surfactant polyacrylic acid in the solution that obtains, ultrasonicly carry out finishing, centrifugal washing dispersion;
Step 3): to step 2) add carbon source presoma, ammoniacal liquor successively in the dispersion liquid that obtains, stir, centrifuge washing, in 70 ~ 90 DEG C of oven dry, obtains the nanoparticle of the coated metal oxide of phenolic resins;
Step 4): by step 3) pressed powder that obtains is placed in tube furnace, in 600 ~ 900 DEG C of calcining 2 ~ 3h under atmosphere of inert gases, obtains carbon-coated magnetic nanoparticle.
2. the preparation method of nucleocapsid structure carbon-clad metal magnetic nanometer particles as claimed in claim 1, is characterized in that, described step 1) in transition metal be any one or a few in Fe, Co and Ni.
3. the preparation method of nucleocapsid structure carbon-clad metal magnetic nanometer particles as claimed in claim 1 or 2, is characterized in that, described step 1) in time of thermal response be 2 hours.
4. the preparation method of nucleocapsid structure carbon-clad metal magnetic nanometer particles as claimed in claim 1, is characterized in that, described step 2) in time of ultrasonic reaction be 2 hours.
5. the preparation method of nucleocapsid structure carbon-clad metal magnetic nanometer particles as claimed in claim 1, is characterized in that, described step 2) in surfactant be polyacrylic acid.
6. the preparation method of nucleocapsid structure carbon-clad metal magnetic nanometer particles as claimed in claim 1, is characterized in that, described step 3) carbon source presoma be phenolic resins.
7. the preparation method of nucleocapsid structure carbon-clad metal magnetic nanometer particles as claimed in claim 1, is characterized in that, described step 3) in the design parameter that stirs be: stir 2 hours at 50 DEG C.
8. the preparation method of nucleocapsid structure carbon-clad metal magnetic nanometer particles as claimed in claim 1, is characterized in that, described step 4) in inert gas be argon gas or nitrogen.
9. the preparation method of nucleocapsid structure carbon-clad metal magnetic nanometer particles as claimed in claim 1, it is characterized in that, described step 4) obtained carbon-coated magnetic nanoparticle pattern is any one or a few in nanosphere, nanometer sheet, nanometer rods, nanocube and nanotube, and is regular pattern, monodispersed core-shell structural.
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