CN110524004A - A kind of preparation method of the dispersed nano porous Fe@C core-shell structure of size adjustable - Google Patents
A kind of preparation method of the dispersed nano porous Fe@C core-shell structure of size adjustable Download PDFInfo
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- CN110524004A CN110524004A CN201910818927.9A CN201910818927A CN110524004A CN 110524004 A CN110524004 A CN 110524004A CN 201910818927 A CN201910818927 A CN 201910818927A CN 110524004 A CN110524004 A CN 110524004A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F2009/245—Reduction reaction in an Ionic Liquid [IL]
Abstract
The invention discloses a kind of monodispersed preparation methods with nanoporous Fe@C core-shell structure of size adjustable, and polyvinylpyrrolidone (PVP) powder is added in the mixed solution of water and ethyl alcohol and is stirred evenly, clarified solution is obtained；Ferrous salt solution is added into clarified solution, be passed through argon gas and stirs 30min in ice-water bath, obtains light green solution；Sodium borohydride (NaBH is added dropwise4) solution, obtained black product centrifuge washing and drying be can be obtained into Fe@C core-shell structure powder by the heat treatment of different temperatures and soaking time.It is this method simple process, low in cost; pass through the regulation of ingredient, reaction time and heat treatment temperature and time in the mixed solution to water and ethyl alcohol; obtaining the monodispersed of size adjustable, there is nanoporous Fe@C core-shell structure powder to show excellent electromagnetic wave absorption performance; suitable for the industrial production of large-scale, have a good application prospect.
Description
Technical field
The invention belongs to Material Fields, are related to the preparation method of nano material, and in particular to a kind of size adjustable list
Disperse the preparation method of nanoporous Fe@C core-shell structure powder.
Background technique
Ferromagnetic metal micro Nano material has high saturation magnetization, high Snoek's cutoff frequency and high Curie
Temperature, and the advantages that absorbing by force to electromagnetic wave can be realized in very wide frequency range, it is the excellent ultra-thin electromagnetic of processability
The ideal selection of wave absorber coatings.But feeromagnetic metal micro-nano granules are easy to oxidize in air, easy under acidic environment
Corrosion, and due to high interfacial energy, ferromagnetic metal micro-nano granules are easy to happen agglomeration, for such existing
Shape, the electromagnetic wave absorption performance for improving ferromagnetic nano metal by various modes have become current research hotspot.It is existing
Mode reported in the literature mainly has surface insulation processing, adulterates dielectric element, cladding dielectric layer etc..Related ferromagnetic nano metal
Preparation method is concentrated mainly on hydro-thermal method, and perhaps this method of thermal oxidation method needs to carry out under high temperature or hyperbaric environment, technique
It is relative complex, greatly constrain the large scale preparation of material.
Therefore, a kind of inexpensive and good synthesis mode of controllability is developed, dielectric layer encapsulated ferromagnetic is can be realized and receives
Rice metallic particles has great importance to the electromagnetic wave absorption performance for improving ferromagnetic nano metal with its application is extended.Text
Offer retrieval to show: it is related using water-ethanol as solvent that at home and abroad there is no reported in literature, and PVP does surfactant and carbon source, boron hydrogen
Change sodium (NaBH4) result of study of Fe@C nano particle is prepared as reducing agent room temperature liquid-phase reduction.
Summary of the invention
The purpose of the present invention is to provide a kind of size adjustable systems with nanoporous Fe@C core-shell structure powder
Preparation Method, this method processing step is simple, can obtain size adjustable with nanoporous Fe C Core-shell structure material.
In order to achieve the above objectives, the technical solution adopted by the present invention are as follows:
A kind of size adjustable monodispersed preparation method with nanoporous Fe@C core-shell structure powder, including with
Lower step:
1) the PVP powder of certain mass is added in the water of different proportion and the mixed solution of ethyl alcohol, stirs evenly, obtains
Clarified solution；
2) ferrous salt solution that certain molar concentration is is added in clarified solution, in ice-water bath stirring and dissolving 15min, is obtained
To light green solution；Ar gas is passed through solution exhaust 15min again, prevents Fe2+It is oxidized, entire reaction system is made to be in Ar atmosphere
In；
3) by the sodium borohydride (NaBH of certain molar concentration4) solution is added dropwise in above-mentioned solution, black precipitate is obtained,
It is isolated, washs repeatedly, be centrifuged, freeze-drying obtains Primary product Fe@PVP powder；
4) Fe@PVP powder is placed in tube furnace, H2High-temperature heat treatment under atmosphere adjusts the temperature and time of heat treatment,
It is size adjustable with nanoporous Fe@C core-shell structure powder to obtain final product.
Stirring evenly in the step 1) is 10~30min of stirring at 15~35 DEG C.
The average molecular weight of the PVP is 3000-400000.
The mixed solution of the water and ethyl alcohol, wherein volume ratio shared by dehydrated alcohol is 0~75%.
Ferrous salt solution in the step 2) refers to frerrous chloride, ferrous nitrate, ferrous sulfate.
Washing in the step 3) is centrifuge washing, and cleaning solvent is water and dehydrated alcohol.
The number of the centrifuge washing is 5~8 times, every time 3~5min, and centrifugal rotational speed is 7000~9000rpm/min.
The temperature being freeze-dried in the step 3) is -40 DEG C, pressure 120Pa, and the time is 10~25h.
The Primary product Fe@PVP that the step 3) obtains is core-shell structure.
The process being heat-treated in the step 4) is the 30min that ventilates at room temperature, is warming up to 500 DEG C of heat preservation 0-2h, heating speed
Rate is 5-20 DEG C/min.
Compared with the existing technology, the invention has the benefit that
The size adjustable monodispersed preparation side with nanoporous Fe@C core-shell structure powder provided by the invention
PVP powder is added in the water of different proportion and the mixed solution of ethyl alcohol and stirs evenly, obtains clarified solution by method；To clarified solution
Middle addition solution of ferrous chloride, stirs in ice-water bath, obtains light green solution；NaBH4 solution is added dropwise, it will be obtained
Black product centrifuge washing and drying, further high-temperature heat treatment can be obtained size adjustable with nanoporous later
Fe@C core-shell structure powder.It is this method simple process, low in cost, pass through ingredient to water and alcohol mixed solution, stirring temperature
The adjusting of degree and heat treatment time can obtain size adjustable monodispersed with nanoporous Fe C core-shell structure powder
End, this method is suitable for the industrial production of large-scale, and there is obtained Fe@C core-shell structure powder excellent electromagnetic wave to inhale
Performance is received, is had a good application prospect.
Detailed description of the invention
Fig. 1 is the SEM figure and partial size statistics of nanometer Fe@C powder prepared by the embodiment of the present invention 1；
Fig. 2 is the SEM figure and partial size statistics of nanometer Fe@C powder prepared by the embodiment of the present invention 2；
Fig. 3 is the SEM figure and partial size statistics of nanometer Fe@C powder prepared by the embodiment of the present invention 3；
Fig. 4 is the SEM figure and partial size statistics of nanometer Fe@C powder prepared by the embodiment of the present invention 4；
Fig. 5 is the SEM figure of nanometer Fe@C powder prepared by the embodiment of the present invention 5；
Fig. 6 is the TEM figure of nanometer Fe@C powder prepared by the embodiment of the present invention 5；
Fig. 7 is the TEM figure of nanometer Fe@C powder prepared by the embodiment of the present invention 6；
Fig. 8 is the electromagnetic wave absorption performance phenogram of nanometer Fe@C powder prepared by the embodiment of the present invention 5.
Specific embodiment
The present invention is described in further details with reference to the accompanying drawing.
Embodiment 1
1) 1g PVP powder is added to the mixed solution (V of 30mL water and ethyl alcoholWater/VEthyl alcohol=30mL/0mL) in, stirring is equal
It is even, obtain clarified solution；
2) 95mg frerrous chloride powder is added in clarified solution, in ice-water bath stirring and dissolving 15min, it is molten obtains light green color
Liquid；Ar gas is passed through solution exhaust 15min again, prevents Fe2+It is oxidized, is in entire reaction system in Ar atmosphere；
3) the NaBH4 solution that 45ml concentration is 100mM is added dropwise in above-mentioned solution, black precipitate is obtained, by its point
From, wash repeatedly, be centrifuged, freeze-drying, obtain monodisperse Fe ball powders；
It is as shown in Figure 1 that embodiment 1 obtains powder morphology, it can be seen that the pattern of the powder is monodisperse spheres, average grain
Diameter is 724nm or so.
Embodiment 2
1) 1g PVP powder is added to the mixed solution (V of 30mL water and ethyl alcoholWater/VEthyl alcohol=22.5mL/7.5mL) in, stirring
Uniformly, clarified solution is obtained；
2) 95mg frerrous chloride powder is added in clarified solution, in ice-water bath stirring and dissolving 15min, it is molten obtains light green color
Liquid；Ar gas is passed through solution exhaust 15min again, prevents Fe2+It is oxidized, is in entire reaction system in Ar atmosphere；
3) the NaBH4 solution that 45ml concentration is 100mM is added dropwise in above-mentioned solution, black precipitate is obtained, by its point
From, wash repeatedly, be centrifuged, freeze-drying, obtain monodisperse Fe powder；
The pattern for the monodisperse Fe powder that embodiment 2 obtains is as shown in Figure 2, it can be seen that the pattern of the powder is monodisperse
Spherical, average grain diameter is 656nm or so.
Embodiment 3
1) 1g PVP powder is added to the mixed solution (V of 30mL water and ethyl alcoholWater/VEthyl alcohol=15mL/15mL) in, stirring is equal
It is even, obtain clarified solution；
2) 95mg frerrous chloride powder is added in clarified solution, in ice-water bath stirring and dissolving 15min, it is molten obtains light green color
Liquid；Ar gas is passed through solution exhaust 15min again, prevents Fe2+It is oxidized, is in entire reaction system in Ar atmosphere；
3) the NaBH4 solution that 45ml concentration is 100mM is added dropwise in above-mentioned solution, black precipitate is obtained, by its point
From, wash repeatedly, be centrifuged, freeze-drying, obtain monodisperse Fe powder；
The pattern for the powder that embodiment 3 obtains is as shown in Figure 3, it can be seen that the pattern of the powder is that monodisperse is spherical, is put down
Equal partial size is 466nm or so.
Embodiment 4
1) 1g PVP powder is added to the mixed solution (V of 30mL water and ethyl alcoholWater/VEthyl alcohol=7.5mL/22.5mL) in, stirring
Uniformly, clarified solution is obtained；
2) 95mg frerrous chloride powder is added in clarified solution, in ice-water bath stirring and dissolving 15min, it is molten obtains light green color
Liquid；Ar gas is passed through solution exhaust 15min again, prevents Fe2+It is oxidized, is in entire reaction system in Ar atmosphere；
3) the NaBH4 solution that 45ml concentration is 100mM is added dropwise in above-mentioned solution, black precipitate is obtained, by its point
From, wash repeatedly, be centrifuged, freeze-drying, obtain monodisperse Fe powder；
The pattern that embodiment 4 obtains powder is as shown in Figure 4, it can be seen that the pattern of the powder is that monodisperse is spherical, average
Partial size is 311nm or so.
Embodiment 5
1) 1g PVP powder is added to the mixed solution (V of 30mL water and ethyl alcoholWater/VEthyl alcohol=5mL/20mL) in, stirring is equal
It is even, obtain clarified solution；
2) 95mg frerrous chloride powder is added in clarified solution, in ice-water bath stirring and dissolving 15min, it is molten obtains light green color
Liquid；Ar gas is passed through solution exhaust 15min again, prevents Fe2+It is oxidized, is in entire reaction system in Ar atmosphere；
3) the NaBH4 solution that 45ml concentration is 100mM is added dropwise in above-mentioned solution, black precipitate is obtained, by its point
From, wash repeatedly, be centrifuged, freeze-drying, obtain Primary product Fe@PVP powder；
4) Fe@PVP powder is placed in tube furnace, H2High-temperature heat treatment under atmosphere, ventilate 30min at room temperature, is warming up to
500 DEG C of heat preservation 2h, heating rate are 5 DEG C/min, and it is size adjustable with nanoporous Fe@C nucleocapsid knot to obtain final product
Structure powder.
The pattern for the nanoporous Fe@C core-shell structure powder that embodiment 5 obtains is as it can be seen in figures 5 and 6, it can be seen that the powder
The pattern at end is that nanometer is spherical, and porous structure occurs in core portion, and average grain diameter is 170nm or so.
Embodiment 6
1) 1g PVP powder is added to the mixed solution (V of 30mL water and ethyl alcoholWater/VEthyl alcohol=5mL/20mL) in, stirring is equal
It is even, obtain clarified solution；
2) 95mg frerrous chloride powder is added in clarified solution, in ice-water bath stirring and dissolving 15min, it is molten obtains light green color
Liquid；Ar gas is passed through solution exhaust 15min again, prevents Fe2+It is oxidized, is in entire reaction system in Ar atmosphere；
3) the NaBH4 solution that 45ml concentration is 100mM is added dropwise in above-mentioned solution, black precipitate is obtained, by its point
From, wash repeatedly, be centrifuged, freeze-drying, obtain Primary product Fe@PVP powder；
4) Fe@PVP powder is placed in tube furnace, H2High-temperature heat treatment under atmosphere, ventilate 30min at room temperature, is warming up to
500 DEG C of heat preservation 2h, heating rate are 20 DEG C/min, and it is size adjustable with nanoporous Fe@C nucleocapsid knot to obtain final product
Structure powder.
The pattern for the nanoporous Fe C core-shell structure powder that embodiment 6 obtains is as shown in Figure 7, it can be seen that the powder
Pattern is that nanometer is spherical, occurs gap among nucleocapsid, and partial size is 170nm or so.
Claims (7)
1. a kind of preparation method of the dispersed nano porous Fe@C core-shell structure of size adjustable, which is characterized in that including following
Step:
1) the PVP powder that quality is 0.5-3g is added in the water of different proportion and the mixed solution of ethyl alcohol, wherein dehydrated alcohol
Shared volume ratio is 0~75%, stirs evenly, obtains clarified solution；
2) ferrous salt solution that molar concentration is 10-200mM is added in clarified solution, in ice-water bath stirring and dissolving 15min, is obtained
To light green solution；Ar gas is passed through solution exhaust 10-15min again, prevents Fe2+It is oxidized, entire reaction system is made to be in Ar
In atmosphere；
3) the NaBH4 solution that molar concentration is 50-300mM is added dropwise in above-mentioned solution, black precipitate is obtained, by its point
From, wash repeatedly, be centrifuged, freeze-drying, obtain Primary product Fe@PVP powder；
4) Fe@PVP powder is placed in tube furnace, H2High-temperature heat treatment under gas atmosphere adjusts the temperature and time of heat treatment, room
The lower 30-60min that ventilates of temperature, is warming up to 500 DEG C of heat preservation 0-2h, heating rate is 5-30 DEG C/min, and obtaining final product size can
Regulation has nanoporous Fe@C core-shell structure powder.
2. the size adjustable monodispersed system with nanoporous Fe@C core-shell structure powder according to claim 1
Preparation Method, it is characterised in that: PVP average molecular weight used in the step 1) is 3000-400000.
3. the size adjustable monodispersed system with nanoporous Fe@C core-shell structure powder according to claim 1
Preparation Method, it is characterised in that: in the mechanical agitation process, stirring evenly is 5~10min of stirring at 15~35 DEG C.
4. the size adjustable monodispersed system with nanoporous Fe@C core-shell structure powder according to claim 1
Preparation Method, it is characterised in that: the ferrous salt solution in the step 2) can be frerrous chloride, ferrous nitrate, ferrous sulfate.
5. the size adjustable monodispersed system with nanoporous Fe@C core-shell structure powder according to claim 1
Preparation Method, it is characterised in that: the washing in the step 3) is centrifuge washing, and cleaning solvent is water and dehydrated alcohol.
6. the size adjustable monodispersed system with nanoporous Fe@C core-shell structure powder according to claim 1
Preparation Method, it is characterised in that: the number of the centrifuge washing is 2~5 times, every time 1~5min, centrifugal rotational speed is 7000~
9000rpm/min。
7. the size adjustable monodispersed system with nanoporous Fe@C core-shell structure powder according to claim 1
Preparation Method, it is characterised in that: the temperature being freeze-dried in the step 3) is -40 to -56 DEG C, pressure 50-120Pa, the time
For 10~25h.
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| CN115477329A (en) * | 2022-09-14 | 2022-12-16 | 北京信息科技大学 | Preparation method of carbon-based core-shell structure pine cone-shaped nanometer flower magnetic composite material |
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