CN106001605A - Method for preparing Fe nanoparticles with carbon quantum dots used as seed crystals - Google Patents
Method for preparing Fe nanoparticles with carbon quantum dots used as seed crystals Download PDFInfo
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- CN106001605A CN106001605A CN201610510520.6A CN201610510520A CN106001605A CN 106001605 A CN106001605 A CN 106001605A CN 201610510520 A CN201610510520 A CN 201610510520A CN 106001605 A CN106001605 A CN 106001605A
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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
- 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
- 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
- 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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- 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
Abstract
The invention relates to a method for preparing Fe nanoparticles with carbon quantum dots used as seed crystals. The method includes the following steps that ferric acetylacetonate is dissolved in an oleylamine solution, stirring is conducted at the room temperature, inert gas nitrogen is pumped in, heating and heat preservation are conducted, tri-n-octylphosphine is rapidly injected at the temperature at the same time, then, the temperature rises and is kept, and black red liquid is obtained; secondly, citric acid is added in the oleylamine solution, octadecene is then added to be stirred and evenly mixed, stirring is conducted at the room temperature, inert gas nitrogen is pumped in, heating and heat preservation are conducted, tri-n-octylphosphine is rapidly injected at the same time, and faint yellow clear liquid is obtained after heat preservation ends; thirdly, the temperature of the faint yellow clear liquid rises, the faint yellow clear liquid is injected into the black red liquid obtained in the first step, the temperature of the mixture is lowered to the room temperature under the protection of inert gas nitrogen after injection is completed, and black liquid is obtained; and fourthly, the black liquid is subjected to centrifuging, washing and vacuum drying till the weight is constant, and the magnetic metal Fe nanoparticles are obtained. The method is simple, low in cost and little in environment pollution.
Description
Technical field
The present invention relates to the preparing technical field of magnetic Nano material, particularly relate to one and prepare for crystal seed with carbon quantum dot
The method of Fe nano-particle.
Background technology
In recent years, magnetic Nano material is owing to having the chemical property of electricity, optics, magnetics and the excellence of uniqueness, at core
The aspects such as nuclear magnetic resonance, optical nano device, targeted drug, magnetic storage, catalyst have it to be widely applied, thus preparation is single
Dispersion, the focus that particle diameter is little, even size distribution magnetic nano-particle has become research functional type nano material.Magnetic Nano
The preparation method of particle is generally divided into Physical, chemical method and physical-chemical process, wherein Physical predominantly organic tool ball-milling method, magnetic
Control sputtering method etc..Owing to the technological process of these physical methods is complex, the highest to equipment requirements, come relative to Physical
Saying, chemical method has more the biggest advantage at aspects such as controlling the size of particle, crystal formation and pattern.
Summary of the invention
The technical problem to be solved is to provide that a kind of method is simple, cost is relatively low, environmental pollution is little with carbon
Quantum dot is the method that crystal seed prepares Fe nano-particle.
For solving the problems referred to above, a kind of method preparing Fe nano-particle for crystal seed with carbon quantum dot of the present invention,
Comprise the following steps:
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through inert nitrogen gas 10 ~ 40min, with
After under the protection of inert nitrogen gas, be heated to 100 ~ 200 DEG C with the speed of 5 ~ 20 DEG C/min, and at a temperature of this be incubated 10 ~
60min, is rapidly injected tri octyl phosphine simultaneously at such a temperature；Then temperature is raised to 150 ~ 250 DEG C, and in this lower insulation 10 ~
60min, obtains dark red liquid；The mass volume ratio of described ferric acetyl acetonade and described oleyl amine solution be 0.1 ~ 1.5mmol:5 ~
20mL；Described ferric acetyl acetonade is 0.1 ~ 1.5mmol:1.00 ~ 5.00mmol with the mass ratio of described tri octyl phosphine；
(2) citric acid is joined in oleyl amine solution, add octadecylene and be uniformly mixed, be stirred at room temperature and be passed through lazy
Property gas nitrogen 10 ~ 40min, is heated to 150 ~ 250 with the speed of 5 ~ 20 DEG C/min subsequently under the protection of inert nitrogen gas
DEG C, and at a temperature of this, it is incubated 20 ~ 100min, it is rapidly injected tri octyl phosphine at such a temperature simultaneously；After insulation terminates, obtain light
Yellow clear liquor；Described citric acid is 0.01 ~ 0.1g:0.5 ~ 5mL with the mass volume ratio of described oleyl amine solution；Described citric acid
It is 0.01 ~ 0.1g:1 ~ 10mL with the mass volume ratio of described octadecylene；Described citric acid with the mass ratio of described tri octyl phosphine is
0.01 ~ 0.1g:1.00 ~ 5.00mmol；
(3) described faint yellow clear liquor is continued to be warmed up to 250 ~ 350 DEG C, and use syringe pump to inject described step at a temperature of this
The dark red liquid of rapid (1) gained, injects the complete protection at inert nitrogen gas and drops to room temperature, obtain black liquor；
The most described black liquor by centrifugation after, be precipitated thing, this precipitate through normal hexane-ethanol mixed liquor wash 3 ~ 9 times,
Vacuum dried to constant weight, obtain magnetic metal Fe nano-particle.
Described step (1) ~ (3) in the flow velocity of inert nitrogen gas be 30 ~ 60mL/min.
Described step (3) middle injection rate is 1 ~ 10mL/h.
The described step (4) middle mixed liquor of normal hexane-ethanol is 0.5 ~ 3 mL:1 mL with the volume ratio of black liquor.
Described step (4) in the mixed liquor of normal hexane-ethanol refer to normal hexane with dehydrated alcohol by the volume ratio of 2 ~ 4:1
Mix.
Described step (4) in centrifugal condition refer to that centrifugation rate is 4000 ~ 9000rpm, the time is 120 ~ 300 seconds.
Described step (4) in vacuum drying condition refer to temperature be 30 ~ 60 DEG C, vacuum be-0.09 ~-0.07MPa.
The present invention compared with prior art has the advantage that
1, the present invention is with ferric acetyl acetonade as presoma, and oleyl amine and octadecylene are solvent, and introducing carbon quantum dot, as crystal seed, is passed through
High temperature organic liquid phase method prepared highly crystalline, purity is high, the Fe nanoparticle of the body-centered cubic phase of uniform particle diameter.
2, in the present invention, the addition of quantum dot improves the apparent condition of the Fe nanoparticle that high temperature organic liquid phase method produces,
It is beneficial to the ripening crystallization of amorphous Fe, thus obtains the product that crystallinity is the highest.
3, the present invention have chosen nontoxic and that boiling point is higher oleyl amine and octadecylene as reaction dissolvent, reduces environment
Pollute.
4, gained Fe nano-particle of the present invention is carried out x-ray diffraction experiment, it appeared that 2 θ=(44.673,65.021 Hes
82.333 °) place occurs in that diffraction maximum, these diffraction maximums correspond respectively to (110), (200) of Fe, (211) crystal face (sees figure
1), illustrating that the Fe nanoparticle obtained is body-centered cubic phase, and as can be seen from the figure product crystallinity is high, purity is high.Enter one
Walk and test (seeing Fig. 3) through SEAD, it can be seen that product crystallinity is the highest, with XRD test result is consistent.
5, present invention synthesis Fe nanoparticle size is homogeneous and narrow distribution, good dispersion (seeing Fig. 2).
6, the present invention uses and is continuously injected into method so that product grain is uniform.
7, the inventive method is simple, cost is relatively low.
Accompanying drawing explanation
Below in conjunction with the accompanying drawings the detailed description of the invention of the present invention is described in further detail.
Fig. 1 is the X ray diffracting spectrum (XRD) of Fe nano-particle of the present invention.Use D/max-2400 type X-ray diffraction
Instrument, excitation source is λ=1.5406 Rigaku companies of nm(Japan).
Fig. 2 is transmission electron microscope (TEM) photo (100nm) of Fe nano-particle of the present invention.Use TECNAI G2 TF20 type
Transmission electron microscope (FEI Co. of the U.S.).
Fig. 3 is SEAD (SAED) photo of Fe nano-particle of the present invention.Use TECNAI G2 TF20 type saturating
Penetrate ultramicroscope (FEI Co. of the U.S.).
Detailed description of the invention
1 one kinds of methods preparing Fe nano-particle for crystal seed with carbon quantum dot of embodiment, comprise the following steps:
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through inert nitrogen gas 10min, exist subsequently
It is heated to 100 DEG C with the speed of 5 DEG C/min under the protection of inert nitrogen gas, and at a temperature of this, is incubated 10min, simultaneously at this
At a temperature of be rapidly injected tri octyl phosphine；Then temperature is raised to 150 DEG C, and in this lower insulation 10min, obtains dark red liquid.
Wherein: ferric acetyl acetonade is 0.1mmol:5mL with the mass volume ratio of oleyl amine solution；Ferric acetyl acetonade and trioctylphosphine
The mass ratio of phosphine is 0.1mmol:1.00mmol.
(2) citric acid is joined in oleyl amine solution, add octadecylene and be uniformly mixed, be stirred at room temperature and lead to
Enter inert nitrogen gas 10min, under the protection of inert nitrogen gas, be heated to 150 DEG C with the speed of 5 DEG C/min subsequently, and in
It is incubated 20min at a temperature of Gai, is rapidly injected tri octyl phosphine at such a temperature simultaneously；After insulation terminates, obtain faint yellow clear liquor.
Wherein: citric acid is 0.01g:0.5mL with the mass volume ratio of oleyl amine solution；Citric acid and the mass body of octadecylene
Long-pending ratio is 0.01g:1mL；Citric acid is 0.01g:1.00mmol with the mass ratio of tri octyl phosphine.
(3) faint yellow clear liquor is continued to be warmed up to 250 DEG C, and use syringe pump to note with the speed of 1mL/h at a temperature of this
Enter the dark red liquid of step (1) gained, inject the complete protection at inert nitrogen gas and drop to room temperature, obtain black liquor.
Black liquor centrifugation rate be 4000rpm, the time be under conditions of 120 seconds by centrifugation after, be precipitated thing,
This precipitate washs 3 times through the mixed liquor of normal hexane-ethanol, temperature be 30 DEG C, vacuum for-0.09MPa under conditions of warp
It is dried under vacuum to constant weight, obtains magnetic metal Fe nano-particle.
Wherein:
The mixed liquor of normal hexane-ethanol and the volume ratio of black liquor are 0.5 mL:1 mL.
The mixed liquor of normal hexane-ethanol refers to mix normal hexane by the volume ratio of 2:1 with dehydrated alcohol.
Above-mentioned steps (1) ~ (3) in the flow velocity of inert nitrogen gas be 30mL/min.
2 one kinds of methods preparing Fe nano-particle for crystal seed with carbon quantum dot of embodiment, comprise the following steps:
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through inert nitrogen gas 40min, exist subsequently
It is heated to 200 DEG C with the speed of 20 DEG C/min under the protection of inert nitrogen gas, and at a temperature of this, is incubated 60min, exist simultaneously
Tri octyl phosphine it is rapidly injected at a temperature of Gai；Then temperature is raised to 250 DEG C, and in this lower insulation 60min, obtains dark red liquid
Body.
Wherein: ferric acetyl acetonade is 1.5mmol:20mL with the mass volume ratio of oleyl amine solution；Ferric acetyl acetonade and three pungent
The mass ratio of base phosphine is 1.5mmol:5.00mmol.
(2) citric acid is joined in oleyl amine solution, add octadecylene and be uniformly mixed, be stirred at room temperature and lead to
Enter inert nitrogen gas 40min, under the protection of inert nitrogen gas, be heated to 250 DEG C with the speed of 20 DEG C/min subsequently, and
At a temperature of this, it is incubated 100min, is rapidly injected tri octyl phosphine at such a temperature simultaneously；After insulation terminates, obtain faint yellow clarification
Liquid.
Wherein: citric acid is 0.1g:5mL with the mass volume ratio of oleyl amine solution；Citric acid and the quality volume of octadecylene
Ratio is 0.1g:10mL；Citric acid is 0.1g:5.00mmol with the mass ratio of tri octyl phosphine.
(3) faint yellow clear liquor is continued to be warmed up to 350 DEG C, and use syringe pump with the speed of 10mL/h at a temperature of this
The dark red liquid of implantation step (1) gained, injects the complete protection at inert nitrogen gas and drops to room temperature, obtain black liquid
Body.
Black liquor centrifugation rate be 9000rpm, the time be under conditions of 300 seconds by centrifugation after, be precipitated thing,
This precipitate washs 9 times through the mixed liquor of normal hexane-ethanol, temperature be 60 DEG C, vacuum for-0.07MPa under conditions of warp
It is dried under vacuum to constant weight, obtains magnetic metal Fe nano-particle.
Wherein:
The mixed liquor of normal hexane-ethanol and the volume ratio of black liquor are 3 mL:1 mL.
The mixed liquor of normal hexane-ethanol refers to mix normal hexane by the volume ratio of 4:1 with dehydrated alcohol.
Above-mentioned steps (1) ~ (3) in the flow velocity of inert nitrogen gas be 60mL/min.
3 one kinds of methods preparing Fe nano-particle for crystal seed with carbon quantum dot of embodiment, comprise the following steps:
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through inert nitrogen gas 30min, exist subsequently
It is heated to 130 DEG C with the speed of 10 DEG C/min under the protection of inert nitrogen gas, and at a temperature of this, is incubated 30min, exist simultaneously
Tri octyl phosphine it is rapidly injected at a temperature of Gai；Then temperature is raised to 180 DEG C, and in this lower insulation 30min, obtains dark red liquid
Body.
Wherein: ferric acetyl acetonade is 0.5mmol:15mL with the mass volume ratio of oleyl amine solution；Ferric acetyl acetonade and three pungent
The mass ratio of base phosphine is 0.5mmol:2.00mmol.
(2) citric acid is joined in oleyl amine solution, add octadecylene and be uniformly mixed, be stirred at room temperature and lead to
Enter inert nitrogen gas 30min, under the protection of inert nitrogen gas, be heated to 200 DEG C with the speed of 10 DEG C/min subsequently, and
At a temperature of this, it is incubated 50min, is rapidly injected tri octyl phosphine at such a temperature simultaneously；After insulation terminates, obtain faint yellow clarification
Liquid.
Wherein: citric acid is 0.05g:2mL with the mass volume ratio of oleyl amine solution；Citric acid and the quality volume of octadecylene
Ratio is 0.05g:5mL；Citric acid is 0.05g:2.40mmol with the mass ratio of tri octyl phosphine.
(3) faint yellow clear liquor is continued to be warmed up to 315 DEG C, and use syringe pump to note with the speed of 5mL/h at a temperature of this
Enter the dark red liquid of step (1) gained, inject the complete protection at inert nitrogen gas and drop to room temperature, obtain black liquor.
Black liquor centrifugation rate be 8000rpm, the time be under conditions of 180 seconds by centrifugation after, be precipitated thing,
This precipitate washs 7 times through the mixed liquor of normal hexane-ethanol, temperature be 30 DEG C, vacuum for-0.07MPa under conditions of warp
It is dried under vacuum to constant weight, obtains magnetic metal Fe nano-particle.
Wherein:
The mixed liquor of normal hexane-ethanol and the volume ratio of black liquor are 0.5 mL:1 mL.
The mixed liquor of normal hexane-ethanol refers to mix normal hexane by the volume ratio of 3:1 with dehydrated alcohol.
Above-mentioned steps (1) ~ (3) in the flow velocity of inert nitrogen gas be 40mL/min.
4 one kinds of methods preparing Fe nano-particle for crystal seed with carbon quantum dot of embodiment, comprise the following steps:
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through inert nitrogen gas 20min, exist subsequently
It is heated to 150 DEG C with the speed of 8 DEG C/min under the protection of inert nitrogen gas, and at a temperature of this, is incubated 20min, simultaneously at this
At a temperature of be rapidly injected tri octyl phosphine；Then temperature is raised to 170 DEG C, and in this lower insulation 20min, obtains dark red liquid.
Wherein: ferric acetyl acetonade is 0.3mmol:10mL with the mass volume ratio of oleyl amine solution；Ferric acetyl acetonade and three pungent
The mass ratio of base phosphine is 0.3mmol:1.50mmol.
(2) citric acid is joined in oleyl amine solution, add octadecylene and be uniformly mixed, be stirred at room temperature and lead to
Enter inert nitrogen gas 20min, under the protection of inert nitrogen gas, be heated to 170 DEG C with the speed of 8 DEG C/min subsequently, and in
It is incubated 30min at a temperature of Gai, is rapidly injected tri octyl phosphine at such a temperature simultaneously；After insulation terminates, obtain faint yellow clear liquor.
Wherein: citric acid is 0.03g:1mL with the mass volume ratio of oleyl amine solution；Citric acid and the quality volume of octadecylene
Ratio is 0.03g:3mL；Citric acid is 0.03g:1.50mmol with the mass ratio of tri octyl phosphine.
(3) faint yellow clear liquor is continued to be warmed up to 280 DEG C, and use syringe pump to note with the speed of 3mL/h at a temperature of this
Enter the dark red liquid of step (1) gained, inject the complete protection at inert nitrogen gas and drop to room temperature, obtain black liquor.
Black liquor centrifugation rate be 6000rpm, the time be under conditions of 180 seconds by centrifugation after, be precipitated thing,
This precipitate washs 5 times through the mixed liquor of normal hexane-ethanol, temperature be 40 DEG C, vacuum for-0.08MPa under conditions of warp
It is dried under vacuum to constant weight, obtains magnetic metal Fe nano-particle.
Wherein:
The mixed liquor of normal hexane-ethanol and the volume ratio of black liquor are 1.5 mL:1 mL.
The mixed liquor of normal hexane-ethanol refers to mix normal hexane by the volume ratio of 2.5:1 with dehydrated alcohol.
Above-mentioned steps (1) ~ (3) in the flow velocity of inert nitrogen gas be 50mL/min.
5 one kinds of methods preparing Fe nano-particle for crystal seed with carbon quantum dot of embodiment, comprise the following steps:
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through inert nitrogen gas 25min, exist subsequently
It is heated to 160 DEG C with the speed of 15 DEG C/min under the protection of inert nitrogen gas, and at a temperature of this, is incubated 40min, exist simultaneously
Tri octyl phosphine it is rapidly injected at a temperature of Gai；Then temperature is raised to 200 DEG C, and in this lower insulation 40min, obtains dark red liquid
Body.
Wherein: ferric acetyl acetonade is 1mmol:10mL with the mass volume ratio of oleyl amine solution；Ferric acetyl acetonade and trioctylphosphine
The mass ratio of phosphine is 1mmol:3.50mmol.
(2) citric acid is joined in oleyl amine solution, add octadecylene and be uniformly mixed, be stirred at room temperature and lead to
Enter inert nitrogen gas 25min, under the protection of inert nitrogen gas, be heated to 210 DEG C with the speed of 15 DEG C/min subsequently, and
At a temperature of this, it is incubated 60min, is rapidly injected tri octyl phosphine at such a temperature simultaneously；After insulation terminates, obtain faint yellow clarification
Liquid.
Wherein: citric acid is 0.08g:3mL with the mass volume ratio of oleyl amine solution；Citric acid and the quality volume of octadecylene
Ratio is 0.08g:7mL；Citric acid is 0.08g:3.20mmol with the mass ratio of tri octyl phosphine.
(3) faint yellow clear liquor is continued to be warmed up to 300 DEG C, and use syringe pump to note with the speed of 5mL/h at a temperature of this
Enter the dark red liquid of step (1) gained, inject the complete protection at inert nitrogen gas and drop to room temperature, obtain black liquor.
Black liquor centrifugation rate be 7500rpm, the time be under conditions of 240 seconds by centrifugation after, be precipitated thing,
This precipitate washs 5 times through the mixed liquor of normal hexane-ethanol, temperature be 50 DEG C, vacuum for-0.08MPa under conditions of warp
It is dried under vacuum to constant weight, obtains magnetic metal Fe nano-particle.
Wherein:
The mixed liquor of normal hexane-ethanol and the volume ratio of black liquor are 2 mL:1 mL.
The mixed liquor of normal hexane-ethanol refers to mix normal hexane by the volume ratio of 3.5:1 with dehydrated alcohol.
Above-mentioned steps (1) ~ (3) in the flow velocity of inert nitrogen gas be 35mL/min.
6 one kinds of methods preparing Fe nano-particle for crystal seed with carbon quantum dot of embodiment, comprise the following steps:
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through inert nitrogen gas 35min, exist subsequently
It is heated to 180 DEG C with the speed of 10 DEG C/min under the protection of inert nitrogen gas, and at a temperature of this, is incubated 45min, exist simultaneously
Tri octyl phosphine it is rapidly injected at a temperature of Gai；Then temperature is raised to 230 DEG C, and in this lower insulation 45min, obtains dark red liquid
Body.
Wherein: ferric acetyl acetonade is 1.3mmol:15mL with the mass volume ratio of oleyl amine solution；Ferric acetyl acetonade and three pungent
The mass ratio of base phosphine is 1.3mmol:4.00mmol.
(2) citric acid is joined in oleyl amine solution, add octadecylene and be uniformly mixed, be stirred at room temperature and lead to
Enter inert nitrogen gas 35min, under the protection of inert nitrogen gas, be heated to 230 DEG C with the speed of 10 DEG C/min subsequently, and
At a temperature of this, it is incubated 80min, is rapidly injected tri octyl phosphine at such a temperature simultaneously；After insulation terminates, obtain faint yellow clarification
Liquid.
Wherein: citric acid is 0.05g:3mL with the mass volume ratio of oleyl amine solution；Citric acid and the quality volume of octadecylene
Ratio is 0.05g:8mL；Citric acid is 0.05g:4.40mmol with the mass ratio of tri octyl phosphine.
(3) faint yellow clear liquor is continued to be warmed up to 330 DEG C, and use syringe pump to note with the speed of 8mL/h at a temperature of this
Enter the dark red liquid of step (1) gained, inject the complete protection at inert nitrogen gas and drop to room temperature, obtain black liquor.
Black liquor centrifugation rate be 8000rpm, the time be under conditions of 240 seconds by centrifugation after, be precipitated thing,
This precipitate washs 7 times through the mixed liquor of normal hexane-ethanol, temperature be 40 DEG C, vacuum for-0.09MPa under conditions of warp
It is dried under vacuum to constant weight, obtains magnetic metal Fe nano-particle.
Wherein:
The mixed liquor of normal hexane-ethanol and the volume ratio of black liquor are 0.5 mL:1 mL.
The mixed liquor of normal hexane-ethanol refers to mix normal hexane by the volume ratio of 3:1 with dehydrated alcohol.
Above-mentioned steps (1) ~ (3) in the flow velocity of inert nitrogen gas be 45mL/min.
Claims (7)
1. the method preparing Fe nano-particle with carbon quantum dot for crystal seed, comprises the following steps:
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through inert nitrogen gas 10 ~ 40min, with
After under the protection of inert nitrogen gas, be heated to 100 ~ 200 DEG C with the speed of 5 ~ 20 DEG C/min, and at a temperature of this be incubated 10 ~
60min, is rapidly injected tri octyl phosphine simultaneously at such a temperature；Then temperature is raised to 150 ~ 250 DEG C, and in this lower insulation 10 ~
60min, obtains dark red liquid；The mass volume ratio of described ferric acetyl acetonade and described oleyl amine solution be 0.1 ~ 1.5mmol:5 ~
20mL；Described ferric acetyl acetonade is 0.1 ~ 1.5mmol:1.00 ~ 5.00mmol with the mass ratio of described tri octyl phosphine；
(2) citric acid is joined in oleyl amine solution, add octadecylene and be uniformly mixed, be stirred at room temperature and be passed through lazy
Property gas nitrogen 10 ~ 40min, is heated to 150 ~ 250 with the speed of 5 ~ 20 DEG C/min subsequently under the protection of inert nitrogen gas
DEG C, and at a temperature of this, it is incubated 20 ~ 100min, it is rapidly injected tri octyl phosphine at such a temperature simultaneously；After insulation terminates, obtain light
Yellow clear liquor；Described citric acid is 0.01 ~ 0.1g:0.5 ~ 5mL with the mass volume ratio of described oleyl amine solution；Described citric acid
It is 0.01 ~ 0.1g:1 ~ 10mL with the mass volume ratio of described octadecylene；Described citric acid with the mass ratio of described tri octyl phosphine is
0.01 ~ 0.1g:1.00 ~ 5.00mmol；
(3) described faint yellow clear liquor is continued to be warmed up to 250 ~ 350 DEG C, and use syringe pump to inject described step at a temperature of this
The dark red liquid of rapid (1) gained, injects the complete protection at inert nitrogen gas and drops to room temperature, obtain black liquor；
The most described black liquor by centrifugation after, be precipitated thing, this precipitate through normal hexane-ethanol mixed liquor wash 3 ~ 9 times,
Vacuum dried to constant weight, obtain magnetic metal Fe nano-particle.
A kind of method preparing Fe nano-particle for crystal seed with carbon quantum dot, it is characterised in that: institute
State step (1) ~ (3) in the flow velocity of inert nitrogen gas be 30 ~ 60mL/min.
A kind of method preparing Fe nano-particle for crystal seed with carbon quantum dot, it is characterised in that: institute
Stating step (3) middle injection rate is 1 ~ 10mL/h.
A kind of method preparing Fe nano-particle for crystal seed with carbon quantum dot, it is characterised in that: institute
Stating the step (4) middle mixed liquor of normal hexane-ethanol is 0.5 ~ 3 mL:1 mL with the volume ratio of black liquor.
A kind of method preparing Fe nano-particle for crystal seed with carbon quantum dot, it is characterised in that: institute
The mixed liquor stating step (4) middle normal hexane-ethanol refers to mix normal hexane by the volume ratio of 2 ~ 4:1 with dehydrated alcohol.
A kind of method preparing Fe nano-particle for crystal seed with carbon quantum dot, it is characterised in that: institute
State step (4) in centrifugal condition refer to that centrifugation rate is 4000 ~ 9000rpm, the time is 120 ~ 300 seconds.
A kind of method preparing Fe nano-particle for crystal seed with carbon quantum dot, it is characterised in that: institute
State step (4) in vacuum drying condition refer to temperature be 30 ~ 60 DEG C, vacuum be-0.09 ~-0.07MPa.
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| CN103192086A (en) * | 2012-01-10 | 2013-07-10 | 中国科学院宁波材料技术与工程研究所 | Preparation method for controllable duplex metal alloy nano particle |
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| US20030121364A1 (en) * | 2002-01-02 | 2003-07-03 | International Business Machines Corporation | Metal salt reduction to form alloy nanoparticles |
| CN101241788A (en) * | 2007-01-15 | 2008-08-13 | 中国科学院化学研究所 | Biological compatibility magnetic nano crystal for high dissolving and stable distribution in physiologicalbuffer liquid and its making method |
| CN101433965A (en) * | 2008-12-17 | 2009-05-20 | 厦门大学 | Method for preparing monodisperse nickel nanoparticle |
| CN101525159A (en) * | 2009-04-20 | 2009-09-09 | 中南大学 | Solvothermal preparation method of monodisperse Fe3O4 nano-particles |
| CN103192086A (en) * | 2012-01-10 | 2013-07-10 | 中国科学院宁波材料技术与工程研究所 | Preparation method for controllable duplex metal alloy nano particle |
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| 中国优秀硕士学位论文全文数据库工程科技Ⅰ辑: "磁性金属铁、镍纳米粒子及其复合结构的合成与研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
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