CN109911881A - A kind of synthetic method of carbon-encapsulated iron nano particle - Google Patents
A kind of synthetic method of carbon-encapsulated iron nano particle Download PDFInfo
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Abstract
The invention discloses a kind of synthetic methods of carbon-encapsulated iron nano particle, are pyrolyzed to obtain carbonitride powder for melamine first, then by FeCl2·4H2O solid is added in KOH solution, and muddy object is obtained after dissolution, and the muddy object is transferred in reaction kettle and is sealed, and heats and precipitating through processing obtains Fe in reaction kettle3O4Powder, finally by the nitridation carbon dust and Fe3O4Powder is cooled to room temperature after reacting at least 1 hour at 620 ~ 680 DEG C, obtains carbon-encapsulated iron nano particle.The synthesising method reacting condition is mild, no pollution to the environment, products obtained therefrom purity is high, saturation magnetization, lower remanent magnetization and coercivity with higher.
Description
Technical field
The invention belongs to the synthesis fields of nano-functional material, and in particular to a kind of synthesis side of carbon-encapsulated iron nano particle
Method.
Background technique
Metal nanoparticle causes extensive concern since it is different from the unique property of block materials.However by
In dimensional effect, this kind of material is easily oxidized and reunites, therefore limits their application.With nucleocapsid structure
Carbon-coated metallic nano-particles be a kind of typical nanocomposite.Carbon coating layer can not only prevent metal nanoparticle
It is oxidized and reunites, and be functionalized nano particle further and provide possibility.Carbon-coated metallic nano-particles exist
The fields such as catalysis, biomedicine, magnetic data storage, magnetic resonance imaging, supercapacitor and optical Limiting device have good
Application prospect.As one of this kind of material, carbon-encapsulated iron nano particle attracts attention since its is stronger magnetic.Carbon packet
Coating can be avoided the oxidation and reunion of iron nano-particle, the magnetic property for keeping iron nano-particle itself excellent, in magnetic recording, iron
Many fields such as magnetic fluid, magnetic resonance imaging, electromagnetic shielding and absorbing material are with a wide range of applications.
Currently, the synthetic method of carbon-coated metallic nano-particles mainly includes arc discharge method, chemical vapour deposition technique, heat
Solution, liquid-phase impregnation process and explosion method etc..Arc discharge method process is complicated and is often accompanied by the generation of impurity；Chemical vapor deposition
The product of area method is not easy the catalyst used with reaction and separates；Liquid-phase impregnation process consumes energy height and low output；Explosion method is wanted
Ask that container material quality is high, temperature gradient is big and energy consumption is high.And pyrolysismethod is because reaction condition is mild, low energy consumption, controllability is strong, institute
To have attracted the great interest of people.
Summary of the invention
The object of the present invention is to provide a kind of synthetic method of carbon-encapsulated iron nano particle, the synthesising method reacting condition temperature
With, no pollution to the environment, products obtained therefrom purity is high and is rectified saturation magnetization with higher, lower remanent magnetization
Stupid power.
To achieve the goals above, the present invention adopts the following technical scheme that:
A kind of synthetic method of carbon-encapsulated iron nano particle, it is characterised in that include the following steps:
(a) melamine is pyrolyzed under the protection of inert gas in 540 ~ 560 DEG C, obtains nitridation carbon dust；
(b) by FeCl2·4H2O solid is being stirred and is being heated in KOH solution under bubbling inert gas, and muddiness is obtained after dissolution
The muddy object is transferred in reaction kettle and is sealed, reacted at 170 ~ 190 DEG C at least 10 hours, precipitating in reaction kettle by object
Fe is obtained through processing3O4Powder；
(c) by the nitridation carbon dust and Fe3O4Powder is uniformly mixed by 3 ~ 4:1 of the mass ratio of the material, is reacted at 620 ~ 680 DEG C
It is cooled to room temperature after at least 1 hour, inert gas shielding during reaction, obtains carbon-encapsulated iron nanometer after products therefrom grinding
Grain.
Preferably, it in the step (a), will be put into tube furnace quartz ampoule after melamine package with masking foil,
The temperature and constant temperature 3 ~ 5 hours are risen to the heating rate of 4 DEG C/min, the inert gas is the nitrogen of purity 99.999%,
Flow velocity of the nitrogen in the tube furnace quartz ampoule is 30mL/min.
Preferably, in the step (b), the concentration of the KOH solution is 1 ~ 1.5 mol/L, the FeCl2·4H2O with
The ratio between amount of substance of KOH is 0.125 ~ 0.15:1.
Preferably, in the step (b), reaction kettle used is the stainless steel cauldron with polytetrafluoroethyllining lining, will
The muddiness object reacts at least 12 hours in reaction kettle in 180 DEG C.
Preferably, in the step (c), by the nitridation carbon dust and Fe3O4Powder is mixed by the mass ratio of the material 3.5:1
Uniformly, it is cooled to room temperature after at least 2 hours are reacted at 650 DEG C, the inert gas is the nitrogen of 99.999 % of purity, nitrogen
Flow velocity of the gas in the tube furnace quartz ampoule is 25 ~ 35mL/min.
In above-mentioned technical proposal, by obtaining carbonitride to pyrolysis of melamine and as carbon source, with hydro-thermal method preparation
Ferroso-ferric oxide (Fe3O4) nano particle be source of iron, at high temperature in inert atmosphere using carbonitride restore Fe3O4Nano particle,
To synthesize carbon-encapsulated iron nano particle.This method is raw materials used nontoxic, from a wealth of sources, cheap, entire to synthesize
Process safety is reliable, mild condition, no pollution to the environment, products therefrom purity with higher, higher saturation magnetization,
Lower remanent magnetization and coercivity.
Detailed description of the invention
Fig. 1 is X-ray diffraction (XRD) spectrogram for the carbon-encapsulated iron nano particle that embodiment one, two, three synthesizes.
Fig. 2 is transmission electron microscope (TEM) photo for the carbon-encapsulated iron nano particle that embodiment two synthesizes.
Fig. 3 is that the transmission electron microscope (TEM) of individual particle in the carbon-encapsulated iron nano particle of the synthesis of embodiment two shines
Piece.
Fig. 4 is room temperature magnetic hysteresis (VSM) loop line for the carbon-encapsulated iron nano particle that embodiment one synthesizes.
Fig. 5 is room temperature magnetic hysteresis (VSM) loop line for the carbon-encapsulated iron nano particle that embodiment two synthesizes.
Fig. 6 is room temperature magnetic hysteresis (VSM) loop line for the carbon-encapsulated iron nano particle that embodiment three synthesizes.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
Embodiment one:
1, the preparation of carbonitride
It weighs 2.0 g melamine white powders to be placed in masking foil, be put it among tube furnace quartz ampoule after package is tight
Position.The flange at quartz ampoule both ends is tightened, is passed through the high pure nitrogen (purity that flow velocity is 30mL/min from quartz ampoule one end
99.999 %), the other end connects tail gas absorption bottle.After 5 min, tube furnace power switch is opened, operation program makes tube furnace liter
Temperature.540 DEG C are warming up to the heating rate of 4 DEG C/min, then constant temperature 5h at this temperature.It is then shut off tube furnace power supply,
Continue logical high pure nitrogen, is allowed to naturally cool to room temperature.Aluminium foil is finally taken out from quartz ampoule, and product is ground with agate mortar
Uniformly, carbonitride buff powder is obtained.
2、Fe3O4The preparation of nano particle
Weigh 1.0 g FeCl2·4H2In filling 40 mL KOH solutions, (concentration is 1 mol/L to O, at this time FeCl2·4H2O with
In small beaker of the ratio between the amount of substance of KOH for 0.125:1), it is passed through high pure nitrogen and carries out bubbling protection, and be put into one piece of magnetic force
Small beaker is placed on magnetic stirring apparatus by stirrer, is stirred at least 20 min, is obtained green turbid solution.Then solution is turned
It moves on in the polytetrafluoroethyllining lining of 50 mL stainless steel cauldrons, is put into after reaction kettle is tightened in 170 DEG C of drying box, instead
Answer 15 h.It is set to naturally ring to room temperature after taking-up, precipitating is washed several times in axe, is centrifuged to be placed in 60 DEG C of drying box and do
It is dry overnight, product agate mortar was ground uniformly in second day, obtains Fe3O4Black powder.
3, the Solid phase synthesis of carbon-encapsulated iron nano particle
The carbonitride and Fe prepared is weighed respectively3O4(molar ratio 3:1), by the two agate mortar mixed grinding at least 20
Min is then charged into porcelain boat, and porcelain boat is put into tube furnace quartz ampoule middle position.The flange at quartz ampoule both ends is tightened, from stone
English pipe one end is passed through the high pure nitrogen (99.999 % of purity) of 30 mL/min of flow velocity, and the other end connects tail gas absorption bottle.5 min
Afterwards, tube furnace power switch is opened, operation program makes tube furnace heat up.620 DEG C are warming up to the heating rate of 10 DEG C/min,
Then 3 h of constant temperature at this temperature.Tube furnace power supply is closed after EP (end of program), is continued logical high pure nitrogen, is allowed to naturally cool to
Room temperature.Porcelain boat is finally taken out from quartz ampoule, and product agate mortar is ground uniformly, carbon-encapsulated iron black powder is obtained.
The XRD spectra for indicating " 620 DEG C " in Fig. 1 bottom is the XRD for the carbon-encapsulated iron nano particle that embodiment one synthesizes
Spectrogram.With two peaks of " ▼ " symbol logo be respectively derived from iron (Fe) simple substance of body-centered cubic structure (bcc) (110) and
(200) two crystal faces illustrate that product is bcc-Fe.
Fig. 4 is the VSM curve for the carbon-encapsulated iron nano particle that embodiment one synthesizes.Measure the saturation magnetization of the product
For 101.0 emug-1。
Embodiment two:
1, the solid phase method preparation of carbonitride
It weighs 2.0 g melamine white powders to be placed in masking foil, be put it among tube furnace quartz ampoule after package is tight
Position.The flange at quartz ampoule both ends is tightened, is passed through the high pure nitrogen (purity that flow velocity is 30 mL/min from quartz ampoule one end
99.999 %), the other end connects tail gas absorption bottle.After 5 min, tube furnace power switch is opened, operation program makes tube furnace liter
Temperature.560 DEG C are warming up to the heating rate of 4 DEG C/min, then 3 h of constant temperature at this temperature.It is then shut off tube furnace power supply,
Continue logical high pure nitrogen, is allowed to naturally cool to room temperature.Aluminium foil is finally taken out from quartz ampoule, and product is ground with agate mortar
Uniformly, carbonitride buff powder is obtained.
2、Fe3O4It is prepared by the hydro-thermal method of nano particle
Weigh 1.2 g FeCl2·4H2In filling 27 mL KOH solutions, (concentration is 1.5 mol/L to O, at this time FeCl2·4H2O with
The ratio between amount of substance of KOH be 0.15:1)) small beaker in, be passed through high pure nitrogen and carry out bubbling protection, and be put into one piece of magnetic force
Small beaker is placed on magnetic stirring apparatus by stirrer, is stirred at least 20 min, is obtained green turbid solution.Then solution is turned
It moves on in the polytetrafluoroethyllining lining of 50 mL stainless steel cauldrons, is put into after reaction kettle is tightened in 190 DEG C of drying box, instead
Answer 10 h.It is set to naturally ring to room temperature after taking-up, precipitating is washed several times in axe, is centrifuged to be placed in 60 DEG C of drying box and do
It is dry overnight, product agate mortar was ground uniformly in second day, obtains Fe3O4Black powder.
3, the synthesis of carbon-encapsulated iron nano particle
The carbonitride and Fe prepared is weighed respectively3O4(molar ratio 3.5:1), by the two agate mortar mixed grinding at least 20
Min is then charged into porcelain boat, and porcelain boat is put into tube furnace quartz ampoule middle position.The flange at quartz ampoule both ends is tightened, from stone
English pipe one end is passed through the high pure nitrogen (99.999 % of purity) of 30 mL/min of flow velocity, and the other end connects tail gas absorption bottle.5 min
Afterwards, tube furnace power switch is opened, operation program makes tube furnace heat up.650 DEG C are warming up to the heating rate of 10 DEG C/min,
Then constant temperature 2h at this temperature.Tube furnace power supply is closed after EP (end of program), is continued logical high pure nitrogen, is allowed to naturally cool to room
Temperature.Porcelain boat is finally taken out from quartz ampoule, and product agate mortar is ground uniformly, carbon-encapsulated iron black powder is obtained.
Medial side indicates the XRD that the XRD spectra of " 650 DEG C " is the carbon-encapsulated iron nano particle that embodiment two synthesizes in Fig. 1
Spectrogram.Very similar with the XRD spectra of one product of embodiment, product is also bcc-Fe.
Fig. 2 is the TEM photo for the carbon-encapsulated iron nano particle that embodiment two synthesizes.It can be seen that black nano particle surface
There is light grey clad, particle diameter is not of uniform size, small tens nanometers, big at 200 nanometers or less.
Fig. 3 is the TEM photo of individual particle in the carbon-encapsulated iron nano particle of the synthesis of embodiment two.This it appears that
The clad structure of grain, the diameter of inner core particles (grey black) is about 50 nanometers, and the thickness of clad (light gray) is at 15-20 nanometers
In range.
Fig. 5 is the VSM curve for the carbon-encapsulated iron nano particle that embodiment two synthesizes.Measure the saturation magnetization of the product
For 99.1 emug-1。
Embodiment three:
1, the solid phase method preparation of carbonitride
It weighs 2.0 g melamine white powders to be placed in masking foil, be put it among tube furnace quartz ampoule after package is tight
Position.The flange at quartz ampoule both ends is tightened, is passed through the high pure nitrogen (purity that flow velocity is 30 mL/min from quartz ampoule one end
99.999 %), the other end connects tail gas absorption bottle.After 5 min, tube furnace power switch is opened, operation program makes tube furnace liter
Temperature.550 DEG C are warming up to the heating rate of 4 DEG C/min, then 4 h of constant temperature at this temperature.Tubular type is closed after EP (end of program)
Furnace power supply continues logical high pure nitrogen, is allowed to naturally cool to room temperature.Aluminium foil is finally taken out from quartz ampoule, by product agate
Mortar grinder is uniform, obtains carbonitride buff powder.
2、Fe3O4It is prepared by the hydro-thermal method of nano particle
Weigh 1.1 g FeCl2·4H2In filling 33 mL KOH solutions, (concentration is 1.3 mol/L to O, at this time FeCl2·4H2O
Be 0.14:1 with the ratio between the amount of substance of KOH)) small beaker in, be passed through high pure nitrogen and carry out bubbling protection, and be put into one piece of magnetic
Power stirrer, small beaker is placed on magnetic stirring apparatus, is stirred at least 20 min, is obtained green turbid solution.Then by solution
It is transferred in the polytetrafluoroethyllining lining of 50 mL stainless steel cauldrons, is put into after reaction kettle is tightened in 180 DEG C of drying box,
React 12 h.So that it is naturally rung to room temperature after taking-up, washed several times, centrifugation is precipitated in axe and is placed in 60 DEG C of drying box
It is dried overnight, product agate mortar was ground uniformly in second day, obtain Fe3O4Black powder.
3, the Solid phase synthesis of carbon-encapsulated iron nano particle
Suitable carbonitride and Fe are weighed respectively3O4(molar ratio 4:1), by the two agate mortar mixed grinding at least 20
Min is then charged into porcelain boat, and porcelain boat is put into tube furnace quartz ampoule middle position.The flange at quartz ampoule both ends is tightened, from stone
English pipe one end is passed through the high pure nitrogen (99.999 % of purity) of 30 mL/min of flow velocity, and the other end connects tail gas absorption bottle.5 min
Afterwards, tube furnace power switch is opened, operation program makes tube furnace heat up.680 DEG C are warming up to the heating rate of 10 DEG C/min,
Then constant temperature 1h at this temperature.It is then shut off tube furnace power supply, continues logical high pure nitrogen, is allowed to naturally cool to room temperature.Most
Porcelain boat is taken out from quartz ampoule afterwards, product agate mortar is ground uniformly, carbon-encapsulated iron black powder is obtained.
The XRD spectra that " 680 DEG C " are topmost indicated in Fig. 1 is the XRD for the carbon-encapsulated iron nano particle that embodiment three synthesizes
Spectrogram.It is very similar with the XRD spectra of two product of one product of embodiment and embodiment, illustrate that product is also bcc-Fe.
Fig. 6 is the VSM curve for the carbon-encapsulated iron nano particle that embodiment three synthesizes.Measure the saturation magnetization of the product
For 100.0 emug-1。
It will be seen from figure 1 that three embodiments synthesis carbon-encapsulated iron nano particle XRD spectra with the mark of bcc-Fe
Quasi- chromatogram accordance, without apparent impurity (such as Fe3C diffraction maximum) occurs, and illustrates the carbon-encapsulated iron nanometer that the present invention synthesizes
The purity of grain is higher.
The TEM photo for the carbon-encapsulated iron nano particle that embodiment one and embodiment three synthesize is very similar with Fig. 2, Fig. 3, this
Specification does not provide.
According to Fig. 4,5,6, the room temperature magnetism parameter for the carbon-encapsulated iron nano particle that three above embodiment synthesizes is listed in
Following table:
| Saturation magnetization (emug-1) | Remanent magnetization (emug-1) | Coercivity (Oe) | |
| Embodiment one | 101.0 | 19.7 | 241.5 |
| Embodiment two | 99.1 | 13.6 | 199.1 |
| Embodiment three | 100.0 | 9.3 | 145.8 |
As can be seen from the table, the saturation magnetization value of carbon-encapsulated iron nano particle synthesized by three embodiments all exists
100 emu·g-1Left and right, and very close, the remanent magnetization and coercive of the carbon-encapsulated iron nano particle that embodiment three synthesizes
Power is minimum.It can be seen that the present invention synthesize carbon-encapsulated iron nano particle saturation magnetization with higher, lower remanent magnetization
Intensity and coercivity.
The present embodiment is to be not intended to limit it, present inventive concept and the explanation realized in structure of the present invention
Under think of, without the technical solution that substantially converts still in protection scope.
Claims (5)
1. a kind of synthetic method of carbon-encapsulated iron nano particle, it is characterised in that include the following steps:
(a) melamine is pyrolyzed under the protection of inert gas in 540 ~ 560 DEG C, obtains nitridation carbon dust；
(b) by FeCl2·4H2O solid is being stirred and is being heated in KOH solution under bubbling inert gas, and muddiness is obtained after dissolution
The muddy object is transferred in reaction kettle and is sealed, reacted at 170 ~ 190 DEG C at least 10 hours, precipitating in reaction kettle by object
Fe is obtained through processing3O4Powder；
(c) by the nitridation carbon dust and Fe3O4Powder is uniformly mixed by 3 ~ 4:1 of the mass ratio of the material, is reacted at 620 ~ 680 DEG C
It is cooled to room temperature after at least 1 hour, inert gas shielding during reaction, obtains carbon-encapsulated iron nanometer after products therefrom grinding
Grain.
2. the synthetic method of carbon-encapsulated iron nano particle as described in claim 1, which is characterized in that in the step (a), use
Masking foil is put into tube furnace quartz ampoule after wrapping up the melamine, rises to the temperature with the heating rate of 4 DEG C/min
And constant temperature 3 ~ 5 hours, the inert gas is the nitrogen of purity 99.999%, flow velocity of the nitrogen in the tube furnace quartz ampoule
For 30 mL/min.
3. the synthetic method of carbon-encapsulated iron nano particle as described in claim 1, which is characterized in that in the step (b), institute
The concentration for stating KOH solution is 1 ~ 1.5 mol/L, the FeCl2·4H2The ratio between amount of substance of O and KOH is 0.125 ~ 0.15:1.
4. the synthetic method of carbon-encapsulated iron nano particle as claimed in claim 1 or 3, which is characterized in that the step (b)
In, reaction kettle used is the stainless steel cauldron with polytetrafluoroethyllining lining, by the muddy object in 180 DEG C in reaction kettle
Reaction at least 12 hours.
5. the synthetic method of carbon-encapsulated iron nano particle as described in claim 1, which is characterized in that, will in the step (c)
The nitridation carbon dust and Fe3O4Powder is uniformly mixed by the mass ratio of the material 3.5:1, cold after reacting at 650 DEG C at least 2 hours
But to room temperature, the inert gas is the nitrogen of purity 99.999%, and flow velocity of the nitrogen in the tube furnace quartz ampoule is
30mL/min。
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| CN110190269A (en) * | 2019-06-27 | 2019-08-30 | 广东工业大学 | A kind of C-base composte material and lithium ion battery |
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| CN102500295A (en) * | 2011-10-26 | 2012-06-20 | 天津大学 | Preparation method of carbon-coated metallic nano-particles |
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| CN102500295A (en) * | 2011-10-26 | 2012-06-20 | 天津大学 | Preparation method of carbon-coated metallic nano-particles |
| CN102784913A (en) * | 2012-07-26 | 2012-11-21 | 天津大学 | Hydrothermal preparation method of carbon-coated iron nanoparticles |
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