CN101176915B - Method for preparing nano metallic nickel granular material coating with carbon - Google Patents
Method for preparing nano metallic nickel granular material coating with carbon Download PDFInfo
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- CN101176915B CN101176915B CN200610097443A CN200610097443A CN101176915B CN 101176915 B CN101176915 B CN 101176915B CN 200610097443 A CN200610097443 A CN 200610097443A CN 200610097443 A CN200610097443 A CN 200610097443A CN 101176915 B CN101176915 B CN 101176915B
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Abstract
The invention relates to a preparation method for carbon-coated nano-metal nickel grain, which comprises the following steps: nickel precursor and macromolecule resin are respectively dissolved in organic solvent in proportion; the two solutions are mixed and 5% mass of auxiliary reagent is added in; the mixed solution is diffused uniformly via ultrasonic; the solvent is vaporized till approximately dry, and then the remainder is dried for 4 hours at 100 DEG C; the sample is crushed and then is solidified in inert or reducing gas and then carbonized to obtain the carbon-coated oxidation resisting nano-metal nickel. The grain size of the nano-metal nickel grain obtained with the method is about 40 to 80nm and the grain is coated with 5 to 10nm carbon layer outside. The metal content can be controlled in a range of 1 to 90% with single phase. The material has the advantages of stability in air, oxidation resistance, simple preparation technology and easy realization of mass production, which is hopefully applied in sensors, magnetic storage medium, magnetic fluid, electromagnetic shielding and other fields.
Description
One, technical field
The present invention relates to the preparation method of the nano metallic nickel granular material that a kind of carbon coats, is that compound with nickel mixes with macromolecule resin after prepare after the solvent evaporation, curing, charing.
Two, technical background
Nano material causes extensive concern owing to its special structure and physicochemical property and potential huge applications are worth.Found C from 1985
60Since, the carbon nano science has obtained continuous development, the material with carbon element of various forms such as CNT, carbon nano-fiber, nano-sized carbon hollow ball, nano metal filled-type carbon pipe and particle etc. are produced out in succession, have opened up brand-new scientific research and technical applications.
The nano metal that carbon coats is a kind of novel nano functional material, its metallic size below 100nm, the outside carbon-coating that coats, medium-term and long-term stable at air, Heat stability is good has solved nano metal oxidation and problem of unstable easily in air.Such material is extensively paid close attention to, and is with a wide range of applications.Changing metal species, carbonization temperature and tenor can the different material of preparation property, can be used as electronic material (as sensor, electrode etc.), magnetic material (as magnetic, electromagnetic shielding, suction ripple, magnetic recording material etc.) and hydrogenation catalyst.The activated material with carbon element that can also prepare Controlled Pore Structure of the composite of low-metal content, being expected to has special purposes in fields such as adsorbent, carrier, molecular sieve.
The preparation method of carbon-coated nano metal generally has arc discharge method, chemical vapour deposition technique (CVD), pyrolysismethod, liquid impregnation charring and explosion method etc. (Huo Jun equality, chemistry circular, 68 (2005) 23-29).Arc discharge method comprises two kinds of direct-current arc and plasma discharges, similarly method also has sputtering method, irradiation and evaporation etc., these a few class preparation method's temperature height (＞2000 ℃), impurity in products many (association carbon pipe and carbon granules), equipment complexity, cost height, (Saito yields poorly, Carbon, 33 (1995) 979-988).The productive rate of chemical vapour deposition technique is than the arc discharge method height, and equipment is simpler, but the product complexity, purity is low, association carbon fiber and carbon pipe, base material and product not easily separated (Nolan et al., Carbon, 33 (1995) 79-85).In the product of liquid impregnation charring preparation, between carbon-coating and the metal hole is arranged, in conjunction with not tight, and productive rate very low (Harris et al., Chem.Phys.Lett., 295 (1998) 53-58).The explosion method preparation process is complicated, dangerous and control is difficult, mass preparation limited (Wu et al., Carbon, 41 (2003) 317-321).
Pyrolysismethod be with source metal with after carbon source is fully mixed, pyrolysis charring in inertia or reducing atmosphere obtains the nano-metal particle material that carbon base body coats through subsequent treatment.(J.Mat.Sci.26 (1991) 1363-1367 such as Yogo; J.Mat.Sci.24 (1989) 2115-2119) reported that in the 125Mpa aqueous medium thermal cracking polymer manufacture metal Fe and Pt are dispersed in the method for the composite in the carbon base body, the surface area of preparation gained material is respectively 120m
2/ g and 154m
2/ g.Patent CN200510012512.0 has narrated the method for the nano metal material that catalytic pyrolysis ferrocene formulations prepared from solutions onion shape carbon coats under high temperature (1000-1200 ℃).Van der Wal etc. has reported catalytic pyrolysis C
2H
2Gas prepares the method for carbon-clad metal particle, and adds thiophene and chlorobenzene in cracked gas, prepares the metal Ni particle (J.Phys.Chem.B, 104 (2000) 11606-11611) that carbon pipe and graphite coat.Song etc. have reported under 6-8Mpa pressure crack refinement petroleum slag and ferrocene mixture, have prepared the method for carbon-clad metal Fe particle through extraction and charing, and metal Fe content is less than 20wt% (Carbon, 41 (2003) 3029-3038) in the material that makes.Song etc. have also reported with similar charring altogether and have prepared FeC and Fe granular materials (Chem.Phys.Lett., 374 (2003) 400-404 that carbon coats; Carbon, 42 (2004) 3177-3182).Paraskevas etc. have reported that catalytic cracking methane and benzene prepare the method for the nano metal FeNi particle of carbon coating, wherein tenor (Carbon, 44 (2006) 820-823) about about 10wt%.Patent CN 200310119200.0 has reported that starch coats ferric hydroxide precipitate, and drying, charing prepare the method for carbon-clad metal particle.Comprehensive literature finds that pyrolysismethod technology is simple, and cost is low, and the yield height is easy to realize large-scale production, has application prospect.But all there is the improved place of needs in these methods of having reported as being actually used in production, and are less as the tenor controlled range, complex operation, and temperature is higher, and preparative-scale is little etc.
Three, summary of the invention
The present invention adopts pyrolysismethod to prepare the nano metal nickel particle that carbon coats, purpose is to disclose the technical method of the nano metallic nickel granular material that but a kind of mass preparation thing is mutually single, content is controlled carbon coats on a large scale, this method is simple to operate, and condition is easy to control.
Technical scheme of the present invention:
The preparation method of the nano metal nickel particle that a kind of carbon coats comprises following two processes: the one, the charing predecessor is the preparation of macromolecule and nickel compound compound, the 2nd, predecessor at a certain temperature inertia or reducing atmosphere in charing.Concrete steps are as follows:
1, with the nickel compound of metering, be dissolved in the organic solvent, concentration is 6-8g/100ml, fully stirs, and mixes, and gets solution A.
2, with the macromolecule resin of metering, be dissolved in the organic solvent, mix with above-mentioned A solution, stir, add the auxiliary reagent of mixed solution quality about 5%, the water-bath evaporating solvent is done near, pulverize the back at 100 ℃ of dry 4h, must contain the polymeric solid of metal precursor.
3, get the polymeric solid 10g that contains metal precursor, place the porcelain container, solidify and carbonization in tube furnace, carburizing atmosphere is inertia or reducibility gas, and flow is 40ml/min, and heating rate is 1-10 ℃/min.At first be warming up to the solidification temperature of macromolecule resin, solidify 1h, be warming up to 300-1000 ℃ then, carbonization insulation 1-4h.
4, charing finishes back maintenance gas flow, naturally cools to room temperature, obtains the nano metallic nickel granular material that carbon coats.
Described metallic nickel compound for can be dissolved in nickel nitrate, nickel acetylacetonate, dicyclopentadienyl nickel, nickel acetate, nickel oxalate in the organic solvent a kind of or several;
Described macromolecule resin is for being dissolved in a kind of of thermosetting epoxy resin, thermoset phenolic resin, low molecular weight polyethylene base resin or styrene base resin in the organic solvent or several;
Described auxiliary reagent is polyethylene glycol, methylcellulose or both mixtures;
Described inertia or reducibility gas are H
2, N
2, He, Ar or its mist.
The present invention prepares the method for carbon-coated nano metallic nickel particle, advantage is: in organic solvent, the big molecule forming composite of nickel compound and resin, through solvent evaporated and curing, nickel compound is evenly dispersed in the macromolecule matrix, and in carbonisation subsequently, macromolecule decomposes, carbonization, the reducing atmosphere that produces when it decomposes can be reduced to metallic state from oxidation state with nickel, thereby obtains being coated on the nano metal nickel particle in the carbon base body.This method is simple, is easy to realize mass preparation, and metallic particles is even in the gained composite, thing mutually single (being impurity such as metallic nickel, nickeliferous hardly oxide and carbide), and content is adjustable on a large scale, and is stable in the air.Solved the difficult problem of the more little easy more oxidation in air of nano-metal particle.
The nano metallic nickel granular material that the carbon for preparing by the present invention coats has magnetic and electric conductivity preferably, can be used for electronic material (as sensor, electrode material etc.), magnetic material (as magnetic, electromagnetic shielding, suction ripple, magnetic recording material etc.) and catalytic hydrogenation material etc., the activated material with carbon element that can also prepare Controlled Pore Structure of the composite of low-metal content, being expected to has specific use in various fields such as adsorbent, carrier, molecular sieve.
Description of drawings:
Transmission electron microscope (TEM) photo of the nano metallic nickel granular material that the typical carbon of Fig. 1 coats
Transmission electron microscope (TEM) photo of the nano metallic nickel granular material that the typical carbon of Fig. 2 coats
X-ray diffraction (XRD) spectrogram of the nano metallic nickel granular material that the typical carbon of Fig. 3 coats
Four, the specific embodiment:
For the present invention is described better, attached embodiment is as follows.It is emphasized that embodiment and do not mean that scope of the present invention is limited in the condition of embodiment narration, the purpose of embodiment is further to set forth content of the present invention and feasibility thereof.
Embodiment 1
Take by weighing the 7.5g Nickelous nitrate hexahydrate, be dissolved in about 100ml ethanol, fully stir solution A.Take by weighing thermosetting epoxy resin 6.5g, be dissolved in the 50ml ethanol, mix with aforementioned A solution behind the adding polyethylene glycol 0.7g, stir, place 80 ℃ of water-bath evaporating solvents to do, behind 100 ℃ of dry 4h, pulverize then, must contain the polymeric solid of metal precursor near.Get this solid 10g in the porcelain container, place quartz ampoule central authorities in the tube furnace, at H
2Heat up H in the air-flow
2Flow is 40ml/min, and heating rate is 1 ℃/min, is warming up to 150 ℃, solidifies 1h, then continues to be warming up to 400 ℃, constant temperature 4h charing.Charing finishes the back and keeps gas flow, naturally cools to room temperature, gets powder sample, is the nano metallic nickel granular material that carbon coats, wherein the about 30wt% of metallic nickel content.
Embodiment 2
Take by weighing the 0.62g dicyclopentadienyl nickel, be dissolved in the 20ml acetone, fully stir, mix.Take by weighing molecular weight and be 3000 polyvinyl resin 34.3g, be dissolved in the 150ml acetone, mix with aforementioned solution after adding methylcellulose 1.75g, stir, 80 ℃ of water-bath evaporating solvents are done near, pulverize behind 100 ℃ of dry about 4h, must contain the polymeric solid of metal precursor.Get this solid 10g in the porcelain container, place quartz ampoule central authorities in the tube furnace, at N
2Heat up in the air-flow, flow is 40ml/min, and heating rate is 1 ℃/min, is warming up to 130 ℃, solidifies 1h, then continues to be warming up to 600 ℃, constant temperature 4h charing.Charing finishes the back and keeps gas flow, naturally cools to room temperature, takes out powder sample, is the nano metallic nickel granular material that carbon coats, wherein the about 1wt% of metallic nickel content.
Embodiment 3
Take by weighing the 6.4g nickel acetylacetonate, be dissolved in about 100ml ethylene glycol, fully stir, mix.Take by weighing molecular weight and be 5000 styrene resin 31.2g, be dissolved in the 130ml ethylene glycol, mix with aforementioned solution after adding methylcellulose 1.87g, stir, 80 ℃ of water-bath evaporating solvents are done near, pulverize behind 100 ℃ of dry about 4h, must contain the polymeric solid of metal precursor.Get this solid 10g in the porcelain container, place quartz ampoule central authorities in the tube furnace, heat up in the He air-flow, flow is 40ml/min, and heating rate is 1 ℃/min, is warming up to 140 ℃, solidifies 1h, then continues to be warming up to 800 ℃, constant temperature 4h charing.Charing finishes the back and keeps gas flow, naturally cools to room temperature, takes out powder sample, is the nano metallic nickel granular material that carbon coats, wherein the about 5wt% of metallic nickel content.
Embodiment 4
Take by weighing 45.24g two oxalic acid hydrate nickel, be dissolved in about 400ml propyl alcohol, stir.Take by weighing thermoset phenolic resin 2.3g, be dissolved in the 30ml propyl alcohol, add 2.38g polyethylene glycol 800 backs and mix with aforementioned solution, stir, 80 ℃ of water-bath evaporating solvents are done near, pulverize behind 100 ℃ of dry about 4h, must contain the polymeric solid of metal precursor.Get this solid 10g in the porcelain container, place quartz ampoule central authorities in the tube furnace, heat up in the Ar air-flow, flow is 40ml/min, and heating rate is 10 ℃/min, is warming up to 170 ℃, solidifies 1h, then continues to be warming up to 1000 ℃, constant temperature 1h charing.Charing finishes the back and keeps gas flow, naturally cools to room temperature, takes out powder sample, is the nano metallic nickel granular material that carbon coats, wherein the about 90wt% of metallic nickel content.
Embodiment 5
Take by weighing 18.12g four hydration nickel acetates, be dissolved in about 200ml ether, stir.Take by weighing thermoset phenolic resin 4.3g, be dissolved in the 40ml ether, mix with aforementioned solution behind the adding polyethylene glycol 1.12g, stir, 80 ℃ of water-bath evaporating solvents are done near, pulverize behind 100 ℃ of dry about 4h, must contain the polymeric solid of metal precursor.Get this solid 10g in the porcelain container, place quartz ampoule central authorities in the tube furnace, heat up in the Ar air-flow, the Ar flow is 40ml/min, and heating rate is that 10 ℃/min is warming up to 170 ℃, solidifies 1h, then continues to be warming up to 300 ℃, constant temperature 4h charing.Charing finishes the back and keeps gas flow, naturally cools to room temperature, takes out powder sample, is the nano metallic nickel granular material that carbon coats, wherein the about 50wt% of metallic nickel content.
Embodiment 6
Take by weighing 7.11g four hydration nickel acetates, be dissolved in (V/V=1/1) in 200ml ether and the acetone mixed solvent, stir.Take by weighing thermoset phenolic resin 5.0g, be dissolved in (V/V=1/1) in 40ml ether and the acetone mixed solvent, mix with aforementioned solution after adding polyethylene glycol 0.6g, stir, 80 ℃ of water-bath evaporating solvents are done near, pulverize behind 100 ℃ of dry about 4h, must contain the polymeric solid of metal precursor.Get this solid 10g and be put in the porcelain container, place quartz ampoule central authorities in the tube furnace, heat up in the Ar air-flow, the Ar throughput is 40ml/min, and heating rate is 10 ℃/min, is warming up to 170 ℃, solidifies 1h, then continues to be warming up to 400 ℃, constant temperature 4h charing.Charing finishes the back and keeps gas flow, naturally cools to room temperature, takes out powder sample, is the nano metallic nickel granular material that carbon coats, wherein the about 25wt% of metallic nickel content.
Embodiment 7
Take by weighing 14.2g four hydration nickel acetates, be dissolved in (V/V=1/1) in 200ml ethanol and the acetone mixed solvent, stir.Take by weighing thermoset phenolic resin 5.0g, be dissolved in (V/V=1/1) in 40ml ethanol and the acetone mixed solvent, add behind the polyethylene glycol 0.96g and aforementioned solution mixing and stirring, 80 ℃ of water-bath evaporating solvents are done near, pulverize behind 100 ℃ of dry about 4h, must contain the polymeric solid of metal precursor.Getting this solid 10g in the porcelain container, place quartz ampoule central authorities in the tube furnace, is 40ml/min in the Ar throughput, and heating rate is 10 ℃/min, is warming up to 170 ℃, solidifies 1h, then is warming up to 300 ℃ of insulation 4h charing.Charing finishes the back and keeps gas flow, naturally cools to room temperature, takes out powder sample, promptly gets the composite of the nano metal nickel particle of carbon coating, wherein the about 40wt% of metallic nickel content.
The foregoing description gained material made behind the sample observe granule-morphology with transmission electron microscope (TEM), with X-ray diffraction (XRD) characterizing metal nickel thing phase, the result shows: material monolithic particle average grain diameter is less than 100nm, and wherein nickel is metallic state, the about 40-80nm of its granular size; Outer carbon-coating for coating, the about 5-10nm of thickness; Coat all right.This result proves that fully method involved in the present invention is practical.
Claims (6)
1. the preparation method of the nano metal nickel particle that coats of a carbon, it is characterized by: be dissolved in the organic solvent respectively the predecessor and the macromolecule resin of nickel in proportion, mix the predecessor of back adding nickel and the auxiliary reagent of the two gross mass 5% of macromolecule resin, described auxiliary reagent is a kind of or its mixture in polyethylene glycol, the methylcellulose; Ultrasonic being uniformly dispersed, evaporating solvent is done near, and 100 ℃ of dryings are after 4 hours, again 120-170 ℃ of heating 1 hour, make macromolecule resin be cured as thermosets, be placed on charing 1-4h in 300-1000 ℃ of inertia or the reducibility gas again, obtain the nano metallic nickel granular material that carbon coats.
2. according to the described method of claim 1, it is characterized in that: the predecessor of described nickel is a kind of in nickel nitrate, nickel acetylacetonate, dicyclopentadienyl nickel, nickel oxalate, the nickel acetate or several.
3. according to the described method of claim 1, it is characterized in that: described macromolecule resin is for being dissolved in a kind of of epoxy resin in the organic solvent, thermoset phenolic resin, low-molecular-weight polyvinyl resin, styrene base resin or several.
4. according to the described method of claim 1, it is characterized in that: described organic solvent is a kind of in ethanol, ethylene glycol, propyl alcohol, acetone, the ether or several.
5. according to the described method of claim 1, it is characterized in that: described inertia or reducibility gas are H
2, N
2, He, Ar or their mist.
6. according to the described method of claim 1, it is characterized in that: the metallic nickel mass content in the nano metallic nickel granular material that described carbon coats is 1-90%.
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| EP4184620A1 (en) * | 2021-11-17 | 2023-05-24 | Institut Polytechnique de Grenoble | Method for the synthesis of a metal catalyst surrounded with a carbon matrix |
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| EP4184620A1 (en) * | 2021-11-17 | 2023-05-24 | Institut Polytechnique de Grenoble | Method for the synthesis of a metal catalyst surrounded with a carbon matrix |
| WO2023088965A1 (en) * | 2021-11-17 | 2023-05-25 | Institut Polytechnique De Grenoble | Method for the synthesis of a metal catalyst surrounded with a carbon matrix |
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