CN102990075A - Method for preparing carbon-coated iron nano particles - Google Patents
Method for preparing carbon-coated iron nano particles Download PDFInfo
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- CN102990075A CN102990075A CN2012104347021A CN201210434702A CN102990075A CN 102990075 A CN102990075 A CN 102990075A CN 2012104347021 A CN2012104347021 A CN 2012104347021A CN 201210434702 A CN201210434702 A CN 201210434702A CN 102990075 A CN102990075 A CN 102990075A
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Abstract
The invention discloses a method for preparing carbon-coated iron nano particles. The method comprises the following steps of: firstly preparing nano FexOy hydrate from ferrous sulfate and sodium hydroxide which serve as raw materials by adopting a fast-precipitation method; and performing carbon coating in a backflow mode by adopting FexOy particles as an iron source and a liquid alkane mixture (C11-C16) as a carbon source. The process comprises the following steps of: material preparation, esterification and modification, alkane backflow and carbon coating, drying, charging, heat treatment and sampling in sequence. Precursor powders with different carbon contents can be prepared by controlling the backflow time and backflow temperature of the materials; and the carbon-coated iron nano particles can be prepared by heat treatment. The carbon-coated iron nano particles prepared by using the method are uniformly distributed in size, and are of a typical core-shell-shaped structure, the inner core is metallic iron and the shell is amorphous carbon; and the particle size of the carbon-coated iron nano particles is 20-50nm, and the thickness of a carbon-coated layer is 5-10nm. The method disclosed by the invention has the advantages of mild condition, easiness for control, simplicity in operation, low cost and suitability for large-scale preparation and the like.
Description
Technical field
The invention belongs to the based composite material of carbon preparation field, be specifically related to a kind of method for preparing Carbon-coated iron nanoparticles take liquid alkane as carbon source.
Background technology
Carbon-encapsulated iron nano-metal particle (carbon-encapsulated iron nanoparticles, CEIN) be a kind of novel nano-sized carbon/ferrous metal composite, huge applications prospect in that the aspects such as Ultrahigh-Density Data Storage, catalysis, giant magnetic impedance, magneto-optic memory technique, absorbing material, ferrofluid and biomedicine demonstrate has caused people's very big interest.Wherein several layers of graphite flake layer form class onion structure closely around the Fe nanometer particles ordered arrangement, and Fe nanometer particles then is in the core of onion.Can strengthen the stability of Fe nanometer particles with carbon as the nanocapsule of shell, overcome and reunite and oxidation.Be coated on the degraded that outer carbon-coating protection Fe nanometer particles avoids environment.
The clad of CEIN plays the effect that reduces magnetic couplings between Fe nanometer particles effectively.Shell is by closely orderly forming of graphitic carbon, can be antiacid, alkali, oil, in 350-400 ℃ of pure oxygen atmosphere, keep stable (Materials Research Bulletin, 2011,46: 2408 – 2417).The carbon shell can connect functional group easily, thereby realizes well surface modification.This is even more important for improving the dispersiveness of Carbon-coated iron nanoparticles in desirable polar solvent.(the Adv. Mater such as the Peng of Peking University, 2004,16: 401-05) tested the Radar Absorbing Property of pure iron, CNT, carbon-encapsulated iron nano particle and nano wire, found that by contrast the material of carbon clad structure has good radar wave assimilation effect.
Just present research situation, the CEIN material that adopts which kind of preparation method and which kind of process conditions to synthesize to meet people to require comprises that can ratio that Fe nanometer particles coated by carbon, grain diameter size, uniform particle diameter degree, iron dispersion situation and the final productive rate etc. in carbon reach the also fully solutions of problem such as optimal cases.In addition, present research is owing to be subjected to preparation method's restriction, and this material still can not be synthesized on a large scale, causes its application and development to relatively lag behind.
Use at present maximum methods for preparing CEIN and mainly contain arc discharge method and CVD method.But the arc discharge temperature has accessory substance (such as CNT, fullerene and carbon black etc.) to generate up to 4000K, and equipment is complicated, and power consumption is large, and cost is high.And the CVD method to early stage metallic particles particle diameter and distribute to require very high, early stage nanocatalyst preparation and the Uniform Dispersion more complicated on substrate, the difficulty of separating also of later stage product and substrate and catalyst carrier.S.H.Tsai etc. (Carbon, 2000,38:781-785.) adopt the CVD method of microwave plasma enhanced to prepare carbon bag particle, but product purity is still lower.In addition, German scholar M Bystrzejewski(Nanotechnology, 2011,22:315606) adopt ironic citrate and vinyl alcohol to be total to thermal decomposition and prepare CEIN, reaction condition is simpler, but Fe is arranged
3The accessory substances such as C and naked Fe particle generate, and need acid etching purification.The liquid alkane backflow method is a kind of method for preparing CEIN of novelty, and equipment requirement is simple, and maximum heat treatment temperature only has 700 ℃, does not almost have accessory substance to generate, and product cut size is more even, is suitable for the scale preparation.
Basic conception of the present invention is: take ferrous sulfate and NaOH as raw material, prepare San oxidation Er Tie ∕ ferrous oxide particle (Fe with coprecipitation
xO
y), remove foreign ion and with alcohol esterification modification is carried out on its surface afterwards; Take the alkane of liquid state as carbon source, backflow Fe
xO
y-liquid alkane suspension makes organic carbochain be wrapped in Fe
xO
yParticle surface, thus make organic and inorganic composite precursor powder, then by heat treatment with Fe
xO
yBe reduced to fe, make simultaneously Fe
xO
yThe unnecessary organic carbon dehydrogenation that particle surface wraps up is converted into DIC and is wrapped in the fe particle surface, finally makes Carbon-coated iron nanoparticles.
Summary of the invention
The invention provides a kind of organic carbon parcel Fe that utilizes the liquid alkane backflow method to obtain of novelty
xO
yBe precursor, make method and the technology path of Carbon-coated iron nanoparticles through subsequent heat treatment.
Specifically the present invention prepares Fe take ferrous sulfate and NaOH as raw material with Hydrolyze method
xO
yParticle, take the liquid alkane mixture as carbon source, wherein, the carbon chain lengths of liquid alkane mixture between 11-16 carbon atom, 160 ~ 250 ℃ of boiling points.Both prepare organic carbon through refluxing and coat Fe
xO
yThe organic and inorganic composite precursor powder of particle, this precursor powder is realized organic carbon fully inorganicization transformation and carbothermic reduction reaction through subsequent heat treatment, finally prepares Carbon-coated iron nanoparticles.
Its concrete process is as follows:
(1) gets the raw materials ready: hydration Fe
xO
yFe is pressed in the particle preparation
2+With OH
-Mol ratio is 1:3, get 0.1mol ferrous sulfate and 0.3mol NaOH, be mixed with respectively the aqueous solution of the isopyknic ferrous sulfate of 1000ml and NaOH, then two solution are mixed rapidly, and rapid stirring, obtain the ferrous hydroxide precipitation, filter, and with the hydroxide iron precipitate under mechanical agitation, washing for several times in 90 ℃ of distilled water, until exist with barium chloride solution check filtrate sulfate radical-free ion, the ferrous iron partial oxidation is ferric iron in washing process, thereby makes the inferior iron ∕ of aqua oxidation di-iron trioxide stuff and other stuff (Fe
xO
y), the carbon chain lengths of liquid alkane mixture between 11 carbon atoms and 16 carbon atoms, 160 ~ 250 ℃ of boiling points;
(2) esterification modification: with gained hydration Fe in (1)
xO
yThe absolute ethyl alcohol of particle and 300ml is at 50-70 ℃ of lower backflow 7h; Then filter; Gained precipitates with the absolute ethyl alcohol of fresh 300ml and mixes, and 50-70 ℃ of lower the backflow 7 hours, above reflux course repeats 5 times again;
(3) alkane backflow: sediment and the 500ml liquid alkane mixture of gained in (2) were at first refluxed 24 hours under 100 ℃, then powder is filtered out, repeatedly extract ethanol in the alkane filtrate with distilled water, next in filtrate, add an amount of anhydrous CaCl
2The water that removal left behind, obtain reusable paraffins mixture, the liquid alkane mixture of regeneration is mixed with the powder that filters out again 120 ℃ of lower backflows 24 hours, the paraffins mixture that obtains recycling with above-mentioned same method, next successively 150 ℃ of lower backflows 48 hours, 180-210 ℃ of lower the backflow 96 hours filters out the black powder at last, and with liquid alkane mixture cyclic washing 5 times;
(4) drying: the high alumina porcelain boat that will carry black precipitate is put in the airtight tube-type atmosphere furnace, then passes into mobile argon gas, under the protection of the argon gas that flows, is warming up to 80-120 ℃, insulation 5-10h; Then cool to room temperature takes out sample, obtains the presoma powder of black;
(5) charging: pack into black presoma powder in the high alumina porcelain boat and compress, it is airtight to put into tube-type atmosphere furnace;
(6) heat treatment: the alundum tube reative cell of tube furnace is extracted into-0.09～-0.1MPa vacuum, then close vavuum pump, then, pass into the argon hydrogen gaseous mixture that flows, be warming up to 700 ℃, then insulation 10h cools to room temperature with the furnace;
(7) sampling: take out product in the porcelain boat of reative cell, thereby obtain Carbon-coated iron nanoparticles, average grain size: 25nm, particle diameter: 20-50nm, carbon coating layer thickness are 5-10nm.
Course of reaction of the present invention can be summed up as organic carbon and coat Fe
xO
yThe transformation of inorganicization of organic carbon and the Fe of nucleocapsid powder
xO
yCarbon thermal reduction.Be coated on Fe under the hot conditions
xO
yThe at first thermal decomposition of the organic carbon of nanoparticle surface forms DIC and is coated on Fe
xO
yNanoparticle surface, simultaneously, Fe
xO
yBe reduced to fe and coated by remaining carbon, thereby make Carbon-coated iron nanoparticles.The nucleocapsid powder that is coated by organic carbon has than bigger serface, and reactivity is higher, be difficult for to produce reunites in heat treatment process, therefore is easy to obtain the Fe nanometer particles that the DIC of nano-scale particle coats, and even particle size; In addition, the Fe nanometer particles that is coated by DIC because the iris action of carbon hinders the fe particle migration, can suppress growing up of fe nano particle in heat treatment process, therefore prepares easily the Carbon-coated iron nanoparticles of nano-scale particle.
What the present invention was prepared is Carbon-coated iron nanoparticles.By adjusting reflux temperature and the return time of precursor when standby, can prepare the nanoscale nucleocapsid composite precursor powder of different phosphorus content (organic carbon); Can adjust the carbon amount of inorganicization of organic carbon transformation by different Technologies for Heating Processing; Therefore the preparation condition (reflux temperature, return time) of precursor need to mate with corresponding Technology for Heating Processing, just can prepare the Carbon-coated iron nanoparticles of different carbon coating layer thickness.
Precursor preparation facilities required for the present invention is simple, mainly is comprised of two parts: heating return stirring device, condensing unit.Effect and correlation between two parts are as follows: 1) heating return stirring device is used for taking up raw material, realizes adjustment and material stirring to reflux temperature; 2) condensing unit utilizes it can realize the repeatedly backflow of liquid alkane or absolute ethyl alcohol.Two parts coordinate operation guarantees fully to mix between the raw material.
Precursor annealing device required for the present invention is simple and easy to operate, mainly is comprised of three parts: body of heater, air distribution system, vacuum system.Effect and correlation between three parts are as follows: 1) the alundum tube reative cell places in the tube furnace, is used for the high alumina crucible of carrying precursor or the center that container places the alundum tube reative cell; 2) air distribution system is comprised of pressure-reducing valve, gas circuit and gas flowmeter, is connected to an end of alundum tube reative cell, utilize it can the conditioned reaction chamber in kind, flow and the proportioning of protective gas; 3) vacuum system; utilize it can be before pioneer's body heat is processed; extracting vacuum repeatedly, be full of inert protective gas; air in the eliminating alundum tube reative cell is to prevent that airborne oxygen is to the oxidation of reactant under the hot conditions; the vacuum that simultaneously also can regulate reative cell, the assurance reative cell is heat-treated under the condition of certain vacuum.
The present invention compares with existing technology of preparing and synthetic route, has following advantage and beneficial effect:
1. adopt new carbon source and new bag carbon mode, this is so that the precursor particle is monodisperse status, and grain size is little, and specific area is large, and the reactivity of precursor is high.The crystal grain of the Carbon-coated iron nanoparticles that the present invention prepares and the size of particle little (all less than 50nm).
2. precursor powder phosphorus content (organic carbon) is controlled, and the carbon amount of inorganicization of organic carbon transformation is controlled in the precursor powder, finally can control the thickness of carbon coating layer.
3. do not need strict dosage relation between this preparation method raw material, so technological operation is simple; Simultaneously preparation, Equipment for Heating Processing is simple, and alkane filtrate reclaiming clean reclaim equiment is simple, is convenient to the scale operation.
4. the liquid alkane mixture of the present invention's use can be recycled.
The specific embodiment
Embodiment one
(1) Fe
xO
yPrecursor is standby: take by weighing respectively 0.1mol ferrous sulfate (FeSO
46H
2O) and 0.3mol NaOH, and be dissolved in respectively in the 1000ml distilled water, then two solution mixed rapidly under rapid stirring, precipitation.Filter, and with Fe
xO
yHydrate washs under mechanical agitation, in 90 ℃ of distilled water for several times, until exist with barium chloride solution check filtrate sulfate radical-free ion.Thereby make hydration Fe
xO
yParticle.
(2) esterification modification: with gained hydration Fe in (1)
xO
yThen the absolute ethyl alcohol of particle and 300ml filters 50 ℃ of lower backflows 7 hours; Gained precipitates with the absolute ethyl alcohol of fresh 300ml and mixes, and 70 ℃ of lower backflows 7 hours, above reflux course repeats 5 times again;
(3) alkane backflow: sediment and the 500ml liquid alkane mixture (C that then will filter gained
11-C
16) at first 100 ℃ of lower backflows 24 hours, then powder is filtered out, repeatedly extract ethanol in the alkane filtrate with distilled water, next in filtrate, add an amount of anhydrous CaCl
2The water that removal left behind, obtain reusable paraffins mixture, the liquid alkane mixture of regeneration is mixed with the powder that filters out again 120 ℃ of lower backflows 24 hours, the paraffins mixture that obtains recycling with above-mentioned same method, next successively at 150 ℃, respectively refluxed under 180 ℃ 48 hours, 96 hours, and filtered out at last the black powder, and wash 5 times with the liquid alkane mixture.
(4) drying: put in the high alumina porcelain boat wet black precipitate and compression, place tube-type atmosphere furnace airtight.Then pass into mobile argon gas, under the protection of the argon gas that flows, be warming up to 100 ℃, insulation 8h; Then naturally cool to room temperature; Sampling obtains the precursor powder of black.
(5) charging: put in the high alumina porcelain boat black precursor powder and compression, place tube-type atmosphere furnace airtight.
(6) heat treatment: with precursor powder at argon hydrogen (15%H
2) under the mixed atmosphere, temperature programming to 700 ℃, insulation 10h, reative cell is with the stove cool to room temperature.
(7) sampling: take out sample in the porcelain boat from the alundum tube reative cell, thereby obtain Carbon-coated iron nanoparticles.The evaluation of powder sees Table one.
Embodiment two
(8) Fe
xO
yPrecursor is standby: take by weighing respectively 0.1mol ferrous sulfate (FeSO
46H
2O) and 0.3mol NaOH, and be dissolved in respectively in the 1000ml distilled water, then two solution mixed rapidly under rapid stirring, precipitation.Filter, and with Fe
xO
yHydrate washs under mechanical agitation, in 90 ℃ of distilled water for several times, until exist with barium chloride solution check filtrate sulfate radical-free ion.Thereby make hydration Fe
xO
yParticle.
(9) esterification modification: with gained hydration Fe in (1)
xO
yThen the absolute ethyl alcohol of particle and 300ml filters 50 ℃ of lower backflows 7 hours; Gained precipitates with the absolute ethyl alcohol of fresh 300ml and mixes, and 70 ℃ of lower backflows 7 hours, above reflux course repeats 5 times again;
(10) alkane backflow: sediment and the 500ml liquid alkane mixture (C that then will filter gained
11-C
16) at first 100 ℃ of lower backflows 24 hours, then powder is filtered out, repeatedly extract ethanol in the alkane filtrate with distilled water, next in filtrate, add an amount of anhydrous CaCl
2The water that removal left behind, obtain reusable paraffins mixture, the liquid alkane mixture of regeneration is mixed with the powder that filters out again 120 ℃ of lower backflows 24 hours, the paraffins mixture that obtains recycling with above-mentioned same method, next successively at 150 ℃, respectively refluxed 24 hours, 48 hours under 180 ℃, again 210 ℃ of lower backflows 96 hours, filter out at last the black powder, and wash 5 times with the liquid alkane mixture.
(11) drying: put in the high alumina porcelain boat wet black precipitate and compression, place tube-type atmosphere furnace airtight.Then pass into mobile argon gas, under the protection of the argon gas that flows, be warming up to 100 ℃, insulation 8h; Then naturally cool to room temperature; Sampling obtains the precursor powder of black.
(12) charging: put in the high alumina porcelain boat black precursor powder and compression, place tube-type atmosphere furnace airtight.
(13) heat treatment: with precursor powder at argon hydrogen (15%H
2) under the mixed atmosphere, temperature programming to 700 ℃, insulation 10h, reative cell is with the stove cool to room temperature.
(14) sampling: take out sample in the porcelain boat from the alundum tube reative cell, thereby obtain Carbon-coated iron nanoparticles.The evaluation of the evaluation powder of powder sees Table one.
The evaluation of precursor powder and carbon iron clad product in each example of table one
Claims (1)
1. method for preparing Carbon-coated iron nanoparticles is characterized in that comprising following process:
Get the raw materials ready: hydration Fe
xO
yFe is pressed in the particle preparation
2+With OH
-Mol ratio is 1:3, get 0.1mol ferrous sulfate and 0.3mol NaOH, be mixed with respectively the ferrous sulfate of 1000ml and the aqueous solution of NaOH, then two solution are mixed rapidly, and rapid stirring, obtain the ferrous hydroxide precipitation, filter, and with the hydroxide iron precipitate under mechanical agitation, washing for several times in 90 ℃ of distilled water, until exist with barium chloride solution check filtrate sulfate radical-free ion, the ferrous iron partial oxidation is ferric iron in washing process, thereby makes the inferior iron ∕ of aqua oxidation di-iron trioxide stuff and other stuff (Fe
xO
y); The carbon chain lengths of liquid alkane mixture between 11 carbon atoms and 16 carbon atoms, 160 ~ 250 ℃ of boiling points;
Esterification modification: with gained hydration Fe in (1)
xO
yThe absolute ethyl alcohol of particle and 300ml is at 50 ℃ of lower backflow 7h; Then filter; Gained precipitates with the absolute ethyl alcohol of fresh 300ml and mixes, and 70 ℃ of lower backflows 7 hours, above reflux course repeats 5 times again;
Alkane backflow: the sediment after the modification and 500ml liquid alkane mixture 100 ℃ of lower backflows 24 hours, are then filtered out powder, repeatedly extract ethanol in the alkane filtrate with distilled water, next in filtrate, add an amount of anhydrous CaCl
2The water that removal left behind, obtain reusable paraffins mixture, the liquid alkane mixture of regeneration is mixed with the powder that filters out again 120 ℃ of lower backflows 24 hours, the paraffins mixture that obtains recycling with above-mentioned same method, next 150 ℃ of lower backflows 48 hours, 180-210 ℃ of lower the backflow 96 hours filters out at last the black powder, and washs 5 times with the liquid alkane mixture;
Dry: the high alumina porcelain boat that will carry black precipitate is put in the airtight tube-type atmosphere furnace, then passes into mobile argon gas, under the protection of the argon gas that flows, is warming up to 80-120 ℃, insulation 5-10h; Then cool to room temperature takes out sample, obtains the presoma powder of black;
Charging: pack into black presoma powder in the high alumina porcelain boat and compress, it is airtight to put into tube-type atmosphere furnace;
Heat treatment: the alundum tube reative cell of tube furnace is extracted into-0.09-0.1MPa vacuum, then closes vavuum pump, then, pass into the argon hydrogen gaseous mixture that flows, be warming up to 700 ℃, then insulation 10h cools to room temperature with the furnace;
Sampling: in the porcelain boat of reative cell, take out product, thereby obtain Carbon-coated iron nanoparticles.
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Cited By (4)
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| CN104801534A (en) * | 2015-04-15 | 2015-07-29 | 刘骁勇 | Magnetic nanomaterial for remediating heavy metal contaminated soil |
| CN105159040A (en) * | 2015-07-22 | 2015-12-16 | 佛山市南海区希望陶瓷机械设备有限公司 | Preparation technology of magnetic powder |
| CN107159902A (en) * | 2017-06-27 | 2017-09-15 | 大连理工大学 | Iron pentacarbonyl is the method that source of iron Gaseous Detonation synthesizes Capability of Carbon-coated Iron Nano-particle |
| CN109128215A (en) * | 2018-09-21 | 2019-01-04 | 郑忆依 | A kind of carbon nickel coat raw powder's production technology |
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Application publication date: 20130327 |