CN110202166A - The chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle - Google Patents
The chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle Download PDFInfo
- Publication number
- CN110202166A CN110202166A CN201910549952.1A CN201910549952A CN110202166A CN 110202166 A CN110202166 A CN 110202166A CN 201910549952 A CN201910549952 A CN 201910549952A CN 110202166 A CN110202166 A CN 110202166A
- Authority
- CN
- China
- Prior art keywords
- powder
- mixed
- nacl
- kcl
- fct
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Power Engineering (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
A kind of chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle of the invention, step are as follows: take metal precursor powder and NaCl/KCl powder, it is mixed according to the ratio with low boiling point solvent, heating stirring, after being uniformly dissolved the above two in low boiling point solvent, heating, which is stirred continuously, evaporates solvent, form metal precursor and the uniform mixed powder of NaCl/KCl, mixed-powder is after annealing, it is cooled to room temperature, separately removes the mixed liquor dissolution dispersion of ionized water and dehydrated alcohol, centrifugation, NaCl/KCl is removed, upper layer centrifugate is outwelled；Dehydrated alcohol is added, after dissolution dispersion, adds and outwells upper layer centrifugate with dehydrated alcohol grade ratio deionized water, centrifuge separation；It repeats dissolution centrifugally operated 3~5 times that add dehydrated alcohol and deionized water, fct-FePt nanoparticle is made.This method operating process is simple, low-carbon environment-friendly, and obtained nano-particles size fine uniform, pattern are uniform, and dispersibility preferably, has the higher degree of order.
Description
Technical field:
The invention belongs to magnetic Nano material technical fields, and in particular to a kind of liquid phase assisted Solid-state sintering synthesis fct-
The chemical method of FePt nanoparticle.
Background technique:
Fct-FePt nano material is due to high magnetocrystalline anisotropy (Kμ≈7×106J/cm3), low superparamagnetic faces
Ungraduated ruler cun (2.8~3.3nm) and excellent catalytic performance, in high density magnetic recording, permanent magnet, biological medicine and electrochemical catalysis
Equal fields wide application prospect.The homogeneity and phase structure of fct-FePt applications to nanostructures performance and its morphology and size
It is closely related.The method of synthesis fct-FePt nanoparticle specifically includes that physical method and chemical method at present.Physical method is with ball-milling method
Based on magnetron sputtering method, the problems such as FePt appearance of nano material of synthesis is not easy to control, and size is uneven；Chemical method can obtain
More uniform consistent nano material is obtained, but the FePt directly prepared is fcc structure, magnetic property and catalytic performance are lower, Wu Faman
Foot application.Just FePt nano particle must can be made to be converted into fct (L1 from fcc using 550 DEG C or more high-temperature heat treatments0) structure,
However high-temperature heat treatment can cause nanoparticle reunion and abnormal growth, therefore it is tiny uniform how to obtain good dispersion, size
Fct-FePt nano material be the field bottleneck problem.
Summary of the invention:
In response to the problems existing in the prior art, the purpose of the present invention is to provide a kind of liquid phase assisted Solid-states to be sintered synthesis fct-
The chemical method of FePt nanoparticle, this method assist combining with solid sintering technology by liquid phase, one-step synthesis size is tiny,
The uniform and high fct-FePt nanoparticle of the degree of order.Product chemistry ingredient can be adjusted by regulating and controlling presoma ratio；By changing
Be lower the ratio of boiling point solvent, NaCl/KCl and presoma, adjusts the NaCl/KCl of buffer action and the mixing ratio of presoma, into
And regulate and control the size of particle；Pattern, size and the degree of order of product are controlled by adjusting solid phase calcination temperature and time.
To achieve the above object, the invention adopts the following technical scheme:
A kind of chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle, comprising the following steps:
Step 1: the pretreatment of presoma
(1) ball milling NaCl/KCl particle is utilized, the NaCl/KCl powder that granularity is 500nm~500 μm is obtained, it is standby
With；
(2) metal precursor powder, including metal precursor Fe (acac) are weighed3Powder and metal precursor Pt (acac)2
Powder, the two molar ratio is 0.3~2, spare；
Step 2: the mixing of presoma
(1) according to the ratio, metal precursor powder: low boiling point solvent=1: the two is added by (300~500), unit g:ml
In container；
(2) by heating stirring, it is uniformly dissolved metal precursor powder in low boiling point solvent, wherein described adds
Hot temperature is 50-100 DEG C, and the time is 10~30min；
(3) in metal salt presoma, addition quality is 50~400 times of step of metal precursor powder quality after dissolution
Rapid 1 (1) NaCl/KCl powder, heats and is stirred continuously, and successively realizes the dissolution of NaCl/KCl powder, and low boiling point solvent volatilizees,
NaCl/KCl and metal precursor are precipitated, and ultimately form metal precursor and NaCl/KCl mixed-powder, wherein the heating
Temperature is 50~150 DEG C, and heating time is 60~150min；
Step 3: the sintering of presoma
Metal precursor and NaCl/KCl mixed-powder are put into crucible, and are placed in vacuum heat treatment furnace, anaerobic
It anneals under atmosphere, 550~750 DEG C of annealing temperature, keeps the temperature 30~150min, form mixed-powder after annealing；
The removal of step 4:NaCl/KCl
(1) mixed-powder after annealing is cooled to room temperature, the mixed liquor of ionized water and dehydrated alcohol is separately removed, after annealing
Mixed-powder carries out dissolution dispersion, is centrifuged later, centrifugal speed be 6000~10000rpm, centrifugation time be 5~
10min removes NaCl/KCl, outwells upper layer centrifugate；
(2) dehydrated alcohol is added, dissolution dispersion is carried out, wherein the additive amount of the dehydrated alcohol is according to the ratio, to move back
Mixed-powder after fire: dehydrated alcohol=1: (30~50), unit g:ml；
(3) add with the deionized water of step (2) dehydrated alcohol grade ratios, be centrifuged again, outwell leafing
Heart liquid；Wherein, centrifugal rotational speed is 6000~10000rpm, and centrifugation time is 5~10min；
(4) step (2)~(3) repeat 3~5 times, and fct-FePt nanoparticle is made.
In the step 1 (1), the expression of NaCl/KCl particle takes one of NaCl particle or KCl particle, is located
Reason；It is same afterwards.
In the step 2 (2) and 2 (3), stirring rate is 1000~2500 revs/min.
In the step 2 (3), after NaCl/KCl powder is added, at 50~150 DEG C, 60~150min of heating occurs
Specific change procedure are as follows: at 50~150 DEG C, heat 40~100min, the dissolution of NaCl/KCl powder forms lysate；Continue
At 150~150 DEG C, 20~50min is heated, low boiling point solvent is made to volatilize, metal precursor and NaCl/KCl are precipitated, and form metal
Presoma and NaCl/KCl mixed-powder.
It, can be abundant since NaCl/KCl and metal precursor are to be precipitated in the solution in the step 2 (3)
Mix so that the mixed-powder for forming NaCl/KCl and metal precursor is uniform mixed-powder.
In the step 3, mixed-powder uses 95%Ar+5%H in advance2After mixed gas carries out gas washing, then anneal
Processing.
In the step 3, oxygen-free atmosphere 95%Ar+5%H2Mixed-gas atmosphere.
In the step 4 (1), deionized water and dehydrated alcohol are to wait bodies in the mixed liquor of deionized water and dehydrated alcohol
Product mixing.
In the step 4 (1), the mixed liquor of mixed-powder and deionized water and dehydrated alcohol proportion is 1 after annealing:
(60~100), unit g:ml.
In the step 2 (1), low boiling point solvent is one kind or two of ethyl alcohol, ethyl acetate, petroleum ether or n-hexane
Kind.
In the step 4 (4), the fct-FePt nanoparticle of acquisition, which is scattered in n-hexane, to be saved.
In the step 4 (4), the magnetic property of its nanoparticle is measured by comprehensive physical property measuring system (PPMS), is adopted
Use transmission Electronic Speculum observes pattern and the distribution of nanoparticle, utilizes the object phase of X-ray diffraction analysis nanoparticle, confirmation
Obtain fct-FePt nanoparticle.
In the step 4 (4), the average-size of the fct-FePt nanoparticle of preparation is 4~15nm.
In the step 4 (4), the fct-FePt nanoparticle of preparation has the very high degree of order, and coercivity reaches 2.0
~2.4T.
The present invention assists chemically reacting the preparation method combined with solid-phase sintering using liquid phase, and it is tiny directly to have synthesized size
Uniformly, the high fct-FePt nanoparticle of the degree of order.First by a certain proportion of NaCl/KCl particle and metal precursor powder
Low boiling point solvent is added in (Fe and Pt), is uniformly mixed and is allowed to sufficiently dissolve.Then solution is heated, it is low in temperature environment
Boiling point solvent volatilization, NaCl/KCl and metal precursor are precipitated from solution, form uniform mixture.Then mixture is existed
A period of time is calcined under certain temperature, directly synthesizes monodispersed fct-FePt nanoparticle.Wherein use low boiling point liquid phase
Ancillary technique is reduced the size of presoma, improves it and be uniformly distributed, improved the local concentration of presoma, be situated between using NaCl/KCl
Matter induces heterogeneous forming core, Lai Tigao nucleation rate, and ensure that being sufficiently mixed for presoma and NaCl/KCl particle, improves subsequent
The uniformity of sintered product size.After metal precursor calcination reaction, formed nano particle, due to have NaCl/KCl particle every
From effect, the homogeneous mixture that forming salt is well isolated by metal precursor can reunite at high temperature and abnormal to avoid particle
It grows up.
Beneficial effects of the present invention:
(1) metal precursor and NaCl/KCl are dissolved by low boiling point solvent, makes metal precursor using agitating and heating
It being uniformly precipitated with NaCl/KCl, formation is sufficiently mixed uniform presoma and NaCl/KCl mixed powder, and low boiling point solvent is volatile,
It is easily operated, low-carbon environment-friendly；
(2) the finely dispersed mixed-powder of metal precursor, Fe, Pt presoma are evenly distributed in annealing process, pass through
Reasonable process, the coercivity that can obtain fct-FePt nanoparticle reach 2.4T.And particle size is tiny, pattern is uniform, simultaneously
It is dispersed preferable；
(4) mixed-powder after annealing is removed NaCl/KCl using deionized water and ethyl alcohol, and cleaning effect is good, nontoxic nothing
Pollution；
(5) all there is important application in fields such as electronics, information, biological medicine, electrochemical catalysis due to fct-FePt, but
High preparation cost limits its use scope, and the present invention will push one-step synthesis fct-FePt technical application, and simplify
Prior art further saves cost, and dispersion effect is good, and magnetic property is excellent after annealing, has extensive theoretical and application meaning
Justice.
Detailed description of the invention:
Fig. 1 is the hysteresis loop of fct-FePt nanoparticle prepared by embodiment of the present invention method 1；
Fig. 2 is the XRD spectrum of fct-FePt nanoparticle prepared by embodiment of the present invention method 1；
Fig. 3 is the TEM image of fct-FePt nanoparticle prepared by embodiment of the present invention method 1；
Fig. 4 is the grain size distribution of fct-FePt nanoparticle prepared by embodiment of the present invention method 1；
Fig. 5 is the hysteresis loop of fct-FePt nanoparticle prepared by embodiment of the present invention method 2；
Fig. 6 is the XRD spectrum of fct-FePt nanoparticle prepared by embodiment of the present invention method 2；
Fig. 7 is the TEM image of fct-FePt nanoparticle prepared by embodiment of the present invention method 2；
Fig. 8 is the grain size distribution of fct-FePt nanoparticle prepared by embodiment of the present invention method 2；
Fig. 9 is the hysteresis loop of fct-FePt nanoparticle prepared by embodiment of the present invention method 3；
Figure 10 is the XRD spectrum of fct-FePt nanoparticle prepared by embodiment of the present invention method 3.
Specific embodiment:
Below with reference to embodiment, the present invention is described in further detail.
In following embodiment:
Preparation equipment is that business is used, and can be bought in market, and Preparation equipment includes: that silica crucible, wide neck flask, machinery stir
Mix the equipment such as heating mantle, vacuum oven, vacuum heat treatment furnace, centrifuge, ball mill.
Commercially available NaCl/KCl powder is obtained into the reasonable NaCl/KCl granularity (μ of 500nm~500 by ball mill
m)；
Mechanical stirring heating mantle main purpose is so that material mixing more evenly, is heated so that low boiling point solvent volatilizees；
Vacuum oven uses blowing-type vacuum oven；
Vacuum heat treatment furnace, the Tubular thermal treatment furnace of diffusion pump is added using commercially available vacuum pump, and vacuum degree can reach
To 10-3Pa；
Wide neck flask and quartzy mortar are that market purchase business is used；
Centrifuge is the supercentrifuge of HC-2066 model.
Acetylacetone,2,4-pentanedione platinum [the Pt (acac) used in the embodiment of the present invention2] and ferric acetyl acetonade [Fe (acac)3] be from
Buy commercial product (purity > 98%) in market；
To mixed-powder after annealing carry out dissolution disperse the statement of used dehydrated alcohol A, B and deionized water A, B only for
Facilitate differentiation, dehydrated alcohol used and deionized water are that business is used；
Ball mill is PBM-V-2L-AD type high speed rotation ball mill.
Low boiling point solvent used in embodiment are as follows: the one or two of ethyl alcohol, ethyl acetate, petroleum ether and n-hexane.
When low boiling point solvent is 2 kinds, the volume ratio of ethyl alcohol and ethyl acetate is 1: 1；The volume ratio of ethyl alcohol and petroleum ether is 1
:1；The volume ratio of ethyl alcohol and n-hexane is 1: 1；The volume ratio of ethyl acetate and petroleum ether is 1: 1；Ethyl acetate and n-hexane
Volume ratio is 1: 1.
Metallic precursor mixed-powder and low boiling point solvent proportion unit are g:ml；
The proportion unit of mixed-powder and deionized water A and dehydrated alcohol A mixed liquor are g:ml after annealing；
The proportion unit of mixed-powder and dehydrated alcohol B are g:ml after annealing；
NaCl/KCl powder dissolves and in the heating process after forming lysate that is uniformly dispersed, due to NaCl/KCl and gold
Belong to presoma and be to be precipitated in the solution, therefore can adequately mix, so that forming NaCl/KCl and metal front
The mixed-powder of body is uniform mixed-powder.
Embodiment 1:
First with ball mill grinding NaCl powder, the NaCl powder that granularity is 20 μm is obtained.Weigh metal precursor Fe
(acac)3With Pt (acac)2Powder (molar ratio ratio is 1) and low boiling point solvent are added in wide-mouth bottle, and low boiling point solvent is positive oneself
Alkane, metallic precursor mixed-powder and low boiling point solvent proportion are 1: 400.Heating is carried out by mechanical stirring heating mantle first to stir
It mixes, stirring rate is 1000 revs/min, and metal precursor mixed-powder is substantially dissolved in low boiling point solvent, at 70 DEG C, is added
Hot 24min is uniformly dissolved metal salt presoma；Add 100 times of the NaCl powder that quality is metal front weight, phase
With heating stirring is continued under stirring rate, at 90 DEG C, 60min is heated, so that NaCl powder dissolve and is uniformly dispersed, is formed and is dissolved
Liquid；Continuation is heated at 90 DEG C, and in the heating process, low boiling point solvent constantly volatilizees in lysate, and has part NaCl analysis
Out, NaCl is as heterogeneous forming core medium, homogeneous nucleation on the surface NaCl that metal precursor is formerly precipitated, until heating 40min,
Low boiling point solvent volatilizees completely, and NaCl and metal precursor are precipitated completely, acquires before the surface NaCl uniform fold has metal
Drive the mixed-powder of body.
Mixed-powder is put into silica crucible, and is placed in tube type vacuum heat-treatment furnace, 95%Ar+5%H is used2Also
Primordial Qi atmosphere carries out gas washing, and 700 DEG C of annealing 60min are warming up under this atmospheric condition.Then mixed-powder is cooling after annealing
To room temperature, taking volume ratio is the mixed liquor of 1: 1 deionized water A and dehydrated alcohol A, carries out dissolution point to mixed-powder after annealing
It dissipates；Wherein, according to the ratio, mixed-powder after annealing: deionized water A and mixed liquor=1 dehydrated alcohol A: 60；After dissolution dispersion, warp
High speed centrifugation 8000rpm, centrifugation time 10min remove NaCl, outwell upper layer centrifugate, add dehydrated alcohol B dissolution point
It dissipating, wherein mixed-powder after annealing: dehydrated alcohol B=1: 30 adds the deionized water B with the isometric ratio of dehydrated alcohol B,
It is centrifuged again, centrifugal rotational speed 6000rpm, centrifugation time 10min, outwells upper layer centrifugate, repeat: nothing is added
Water-ethanol B dissolution dispersion, deionized water B step with centrifugal separation 3 times, are made fct-FePt nanoparticle, are scattered in n-hexane
It is saved.The magnetic property of its nanoparticle is measured by comprehensive physical property measuring system (PPMS), coercivity is 2.4T, such as attached
Shown in Fig. 1.Contain fct characteristic peak (110), (001) and (002) by the phase structure that X-ray diffractometer measures sample, it is such as attached
Shown in Fig. 2.Sample particle pattern using Flied emission transmission electron microscope observing nanoparticle is uniform, and dispersibility is preferable, such as 3 institute of attached drawing
Show, average-size 7.5nm, grain size distribution is as shown in Fig. 4.
Embodiment 2:
First with ball mill grinding NaCl powder, the NaCl powder that granularity is 25 μm is obtained.Weigh metal precursor Fe
(acac)3With Pt (acac)2(molar ratio ratio is 0.8) mixed-powder and low boiling point solvent are added in wide-mouth bottle, and low boiling point is molten
Agent is the mixed solution of ethyl alcohol and the isometric ratio of ethyl acetate, and metallic precursor mixed-powder and low boiling point solvent proportion are 1:
500.Heating stirring is carried out by mechanical stirring heating mantle first, stirring rate is 1000 revs/min, and metal precursor is mixed
Powder is substantially dissolved in low boiling point solvent, and at 75 DEG C, heating 20min adds quality after metal salt presoma is uniformly dissolved
For 400 times of NaCl powder of metal front weight, continue to stir under identical stirring rate, at 100 DEG C, heats 50min, make
It obtains NaCl powder to dissolve and be uniformly dispersed, forms lysate；Continuation is heated at 100 DEG C, in the heating process, in lysate
Low boiling point solvent constantly volatilizees, and has part NaCl precipitation, NaCl as heterogeneous forming core medium, what metal precursor was formerly precipitated
Homogeneous nucleation on the surface NaCl, until heating 30min, low boiling point solvent volatilize completely, NaCl and metal precursor are precipitated completely,
Acquire the mixed-powder that the surface NaCl uniform fold has metal precursor.
Mixed-powder is put into silica crucible, and is placed in tube type vacuum heat-treatment furnace, 95%Ar+5%H is used2Also
Primordial Qi atmosphere carries out gas washing, and 750 DEG C of annealing 60min are warming up under this atmospheric condition.Then mixed-powder is cooling after annealing
To room temperature, taking volume ratio is the mixed liquor of 1: 1 deionized water A and dehydrated alcohol A, carries out dissolution point to mixed-powder after annealing
It dissipates；Wherein, according to the ratio, mixed-powder after annealing: deionized water A and mixed liquor=1 dehydrated alcohol A: 100；After dissolution dispersion, warp
High speed centrifugation 7000rpm, centrifugation time 8min remove NaCl, outwell upper layer centrifugate, add dehydrated alcohol B dissolution point
It dissipating, wherein mixed-powder after annealing: dehydrated alcohol B=1: 30 adds the deionized water B with the isometric ratio of dehydrated alcohol B,
It is centrifuged again, centrifugal rotational speed 6000rpm, centrifugation time 10min, outwells upper layer centrifugate, repeat: nothing is added
Water-ethanol B dissolution dispersion, deionized water B step with centrifugal separation 4 times, be made fct-FePt nanoparticle be scattered in n-hexane into
Row saves.The magnetic property of its nanoparticle is measured by comprehensive physical property measuring system (PPMS), coercivity is 2.2T such as attached drawing 5
It is shown.Contain fct characteristic peak (110), (001) and (002) such as attached drawing 6 by the phase structure that X-ray diffractometer measures sample
It is shown.Sample particle pattern using Flied emission transmission electron microscope observing nanoparticle is uniform, and dispersibility is preferably as shown in Fig. 7,
Its average-size is 6.1nm, and grain size distribution is as shown in Fig. 8.
Embodiment 3:
First with ball mill grinding NaCl powder, the NaCl powder that granularity is 500nm is obtained.Weigh metal precursor Fe
(acac)3With Pt (acac)2(molar ratio ratio is 1.2) and low boiling point solvent are added in wide-mouth bottle, and low boiling point solvent is ethyl alcohol,
Metallic precursor mixed-powder and low boiling point solvent proportion are 1: 300.Heating stirring is carried out by mechanical stirring heating mantle first,
Stirring rate is 1000 revs/min, and metal precursor mixed-powder is substantially dissolved in low boiling point solvent, at 85 DEG C, heating
15min after metal salt presoma is uniformly dissolved, adds 50 times of the NaCl powder that quality is metal front weight, identical
Continue to stir under stirring rate, at 120 DEG C, heat 40min, so that NaCl powder is dissolved and is uniformly dispersed, forms lysate；After
Continue and is heated at 120 DEG C, in the heating process, low boiling point solvent constantly volatilizees in lysate, and has part NaCl precipitation,
NaCl is as heterogeneous forming core medium, homogeneous nucleation on the surface NaCl that metal precursor is formerly precipitated, until 20min is heated, it is low
Boiling point solvent volatilizees completely, and NaCl and metal precursor are precipitated completely, and acquiring the surface NaCl uniform fold has metal front
The mixed-powder of body.
Mixed-powder is put into silica crucible, and is placed in tube type vacuum heat-treatment furnace, 95%Ar+5%H is used2Also
Primordial Qi atmosphere carries out gas washing, and 650 DEG C of annealing 30min are warming up under this atmospheric condition.Then mixed-powder is cooling after annealing
To room temperature, taking volume ratio is the mixed liquor of 1: 1 deionized water A and dehydrated alcohol A, carries out dissolution point to mixed-powder after annealing
It dissipates；Wherein, according to the ratio, mixed-powder after annealing: deionized water A and mixed liquor=1 dehydrated alcohol A: 80；After dissolution dispersion, warp
High speed centrifugation 6000rpm, centrifugation time 5min remove NaCl, outwell upper layer centrifugate, add dehydrated alcohol B dissolution point
It dissipating, wherein mixed-powder after annealing: dehydrated alcohol B=1: 50 adds the deionized water B with the isometric ratio of dehydrated alcohol B,
It is centrifuged again, centrifugal rotational speed 6000rpm, centrifugation time 10min, outwells upper layer centrifugate, repeat: nothing is added
Water-ethanol B dissolution dispersion, deionized water B step with centrifugal separation 5 times, be made fct-FePt nanoparticle be scattered in n-hexane into
Row saves.The magnetic property of its nanoparticle is measured by comprehensive physical property measuring system (PPMS), coercivity is 2.3T such as attached drawing 9
It is shown.Contain fct characteristic peak (110), (001) and (002) such as attached drawing 10 by the phase structure that X-ray diffractometer measures sample
It is shown.Use the sample particle average-size of Flied emission transmission electron microscope observing nanoparticle for 8.7nm.
Embodiment 4:
First with ball mill grinding NaCl powder, the NaCl powder that granularity is 500 μm is obtained.Weigh metal precursor Fe
(acac)3With Pt (acac)2(molar ratio ratio is 0.5) and low boiling point solvent are added in wide-mouth bottle, and low boiling point solvent is acetic acid second
Ester, metallic precursor mixed-powder and low boiling point solvent proportion are 1: 500.Heating is carried out by mechanical stirring heating mantle first to stir
It mixes, stirring rate is 1000 revs/min, and metal precursor mixed-powder is substantially dissolved in low boiling point solvent, at 75 DEG C, is added
Hot 20min after metal salt presoma is uniformly dissolved, adds 400 times of the NaCl powder that quality is metal front weight, phase
With continuing to stir under stirring rate, at 100 DEG C, 55min is heated, so that NaCl powder is dissolved and is uniformly dispersed, forms lysate；
Continuation is heated at 100 DEG C, and in the heating process, low boiling point solvent constantly volatilizees in lysate, and has part NaCl precipitation,
NaCl is as heterogeneous forming core medium, homogeneous nucleation on the surface NaCl that metal precursor is formerly precipitated, until 35min is heated, it is low
Boiling point solvent volatilizees completely, and NaCl and metal precursor are precipitated completely, and acquiring the surface NaCl uniform fold has metal front
The mixed-powder of body.
Mixed-powder is put into silica crucible, and is placed in tube type vacuum heat-treatment furnace, 95%Ar+5%H is used2Also
Primordial Qi atmosphere carries out gas washing, and 750 DEG C of annealing 150min are warming up under this atmospheric condition.Then mixed-powder is cooling after annealing
To room temperature, taking volume ratio is the mixed liquor of 1: 1 deionized water A and dehydrated alcohol A, carries out dissolution point to mixed-powder after annealing
It dissipates；Wherein, according to the ratio, mixed-powder after annealing: deionized water A and mixed liquor=1 dehydrated alcohol A: 100；After dissolution dispersion, warp
High speed centrifugation 10000rpm, centrifugation time 8min remove NaCl, outwell upper layer centrifugate, add dehydrated alcohol B dissolution point
It dissipating, wherein mixed-powder after annealing: dehydrated alcohol B=i: 40 adds the deionized water B with the isometric ratio of dehydrated alcohol B,
It is centrifuged again, centrifugal rotational speed 8000rpm, centrifugation time 8min, outwells upper layer centrifugate, repeat: nothing is added
Water-ethanol B dissolution dispersion, deionized water B step with centrifugal separation 3 times, be made obtain fct-FePt nanoparticle be scattered in just oneself
It is saved in alkane.Measuring the coercivity of its nanoparticle by comprehensive physical property measuring system (PPMS) is 2.1T, is sent out using field
The sample particle average-size for penetrating transmission electron microscope observing nanoparticle is 15nm.
Embodiment 5:
First with ball mill grinding NaCl powder, the NaCl powder that granularity is 400 μm is obtained.Weigh metal precursor Fe
(acac)3With Pt (acac)2(molar ratio ratio is 0.3) and low boiling point solvent are added in wide-mouth bottle, and low boiling point solvent is petroleum
Ether, metallic precursor mixed-powder and low boiling point solvent proportion are 1: 400.Heating is carried out by mechanical stirring heating mantle first to stir
It mixes, stirring rate is 1500 revs/min, and metal precursor mixed-powder is substantially dissolved in low boiling point solvent, at 60 DEG C, is added
Hot 28min after metal salt presoma is uniformly dissolved, adds 300 times of the NaCl powder that quality is metal front weight, phase
With continuing to stir under stirring rate, at 80 DEG C, 80min is heated, so that NaCl powder is dissolved and is uniformly dispersed, forms lysate；
Continuation is heated at 80 DEG C, and in the heating process, low boiling point solvent constantly volatilizees in lysate, and has part NaCl precipitation,
NaCl is as heterogeneous forming core medium, homogeneous nucleation on the surface NaCl that metal precursor is formerly precipitated, until 60min is heated, it is low
Boiling point solvent volatilizees completely, and NaCl and metal precursor are precipitated completely, and acquiring the surface NaCl uniform fold has metal front
The mixed-powder of body.
Mixed-powder is put into silica crucible, and is placed in tube type vacuum heat-treatment furnace, 95%Ar+5%H is used2Also
Primordial Qi atmosphere carries out gas washing, and 700 DEG C of annealing 60min are warming up under this atmospheric condition.Then mixed-powder is cooling after annealing
To room temperature, taking volume ratio is the mixed liquor of 1: 1 deionized water A and dehydrated alcohol A, carries out dissolution point to mixed-powder after annealing
It dissipates；Wherein, according to the ratio, mixed-powder after annealing: deionized water A and mixed liquor=1 dehydrated alcohol A: 80；After dissolution dispersion, warp
High speed centrifugation 8000rpm, centrifugation time 10min remove NaCl, outwell upper layer centrifugate, add dehydrated alcohol B dissolution point
It dissipating, wherein mixed-powder after annealing: dehydrated alcohol B=1: 40 adds the deionized water B with the isometric ratio of dehydrated alcohol B,
It being centrifuged again, it is 8000rpm, centrifugation time 8min that centrifugal rotational speed, which is centrifugal rotational speed,, upper layer centrifugate is outwelled,
It repeats: dehydrated alcohol B dissolution dispersion, deionized water B step with centrifugal separation 3 times is added, the dispersion of fct-FePt nanoparticle is made
It is saved in n-hexane.Measuring the coercivity of its nanoparticle by comprehensive physical property measuring system (PPMS) is 2.2T, is adopted
The sample particle average-size that use transmission Electronic Speculum observes nanoparticle is 6.5nm.
Embodiment 6:
First with ball mill grinding NaCl powder, the NaCl powder that granularity is 10 μm is obtained.Weigh metal precursor Fe
(acac)3With Pt (acac)2(molar ratio ratio be 0.5) and low boiling point solvent are added in wide-mouth bottle, low boiling point solvent be ethyl alcohol with
For petroleum ether in equal volume than mixed solution, metallic precursor mixed-powder and low boiling point solvent proportion are 1: 500.Pass through machinery first
Agitating and heating set carries out heating stirring, and stirring rate is 1500 revs/min, metal precursor mixed-powder is substantially dissolved in low
In boiling point solvent, at 85 DEG C, 15min is heated, after metal salt presoma is uniformly dissolved, adding quality is metal front weight
400 times of NaCl powder, continue to stir under identical stirring rate, at 120 DEG C, heat 40min, so that the dissolution of NaCl powder is simultaneously
It is uniformly dispersed, forms lysate；Continuation is heated at 120 DEG C, and in the heating process, low boiling point solvent is constantly waved in lysate
Hair, and have part NaCl precipitation, NaCl is as heterogeneous forming core medium, uniform shape on the surface NaCl that metal precursor is formerly precipitated
Core, until heating 20min, low boiling point solvent volatilize completely, NaCl and metal precursor are precipitated completely, acquire the surface NaCl
Uniform fold has the mixed-powder of metal precursor.
Mixed-powder is put into silica crucible, and is placed in tube type vacuum heat-treatment furnace, 95%Ar+5%H is used2Also
Primordial Qi atmosphere carries out gas washing, and 550 DEG C of annealing 120min are warming up under this atmospheric condition.Then mixed-powder is cooling after annealing
To room temperature, taking volume ratio is the mixed liquor of 1: 1 deionized water A and dehydrated alcohol A, carries out dissolution point to mixed-powder after annealing
It dissipates；Wherein, according to the ratio, mixed-powder after annealing: deionized water A and mixed liquor=1 dehydrated alcohol A: 60；After dissolution dispersion, warp
High speed centrifugation 6000rpm, centrifugation time 6min remove NaCl, outwell upper layer centrifugate, add dehydrated alcohol B dissolution point
It dissipating, wherein mixed-powder after annealing: dehydrated alcohol B=1: 50 adds the deionized water B with the isometric ratio of dehydrated alcohol B,
It being centrifuged again, it is 8000rpm, centrifugation time 8min that centrifugal rotational speed, which is centrifugal rotational speed,, upper layer centrifugate is outwelled,
It repeats: dehydrated alcohol B dissolution dispersion, deionized water B step with centrifugal separation 3 times is added, the dispersion of fct-FePt nanoparticle is made
It is saved in n-hexane.Measuring the coercivity of its nanoparticle by comprehensive physical property measuring system (PPMS) is 2.2T, is adopted
The sample particle average-size that use transmission Electronic Speculum observes nanoparticle is 4.0nm.
Embodiment 7:
First with ball mill grinding KCl powder, the KCl powder that granularity is 100 μm is obtained.Weigh metal precursor Fe
(acac)3With Pt (acac)2(molar ratio ratio be 2) and low boiling point solvent are added in wide-mouth bottle, low boiling point solvent be petroleum ether with
For ethyl acetate in equal volume than mixed solution, metallic precursor mixed-powder and low boiling point solvent proportion are 1: 300.Pass through machine first
Tool agitating and heating set carries out heating stirring, and stirring rate is 1500 revs/min, and metal precursor mixed-powder is substantially dissolved in
In low boiling point solvent, at 50 DEG C, 30min is heated, after metal salt presoma is uniformly dissolved, adding quality is metal front constitution
50 times of KCl powder of amount continues to stir under identical stirring rate, at 50 DEG C, heats 100min, so that the dissolution of KCl powder is simultaneously
It is uniformly dispersed, forms lysate；Continuation is heated at 50 DEG C, and in the heating process, low boiling point solvent is constantly waved in lysate
Hair, and have part KCl precipitation, KCl is as heterogeneous forming core medium, homogeneous nucleation on the surface KCl that metal precursor is formerly precipitated,
Until heating 50min, low boiling point solvent volatilize completely, KCl and metal precursor are precipitated completely, and it is uniform to acquire the surface KCl
It is covered with the mixed-powder of metal precursor.
Mixed-powder is put into silica crucible, and is placed in tube type vacuum heat-treatment furnace, 95%Ar+5%H is used2Also
Primordial Qi atmosphere carries out gas washing, and 700 DEG C of annealing 60min are warming up under this atmospheric condition.Then mixed-powder is cooling after annealing
To room temperature, taking volume ratio is the mixed liquor of 1: 1 deionized water A and dehydrated alcohol A, carries out dissolution point to mixed-powder after annealing
It dissipates；Wherein, according to the ratio, mixed-powder after annealing: deionized water A and mixed liquor=1 dehydrated alcohol A: 80；After dissolution dispersion, warp
High speed centrifugation 8000rpm, centrifugation time 8min remove KCl, outwell upper layer centrifugate, add dehydrated alcohol B dissolution point
It dissipating, wherein mixed-powder after annealing: dehydrated alcohol B=1: 40 adds the deionized water B with the isometric ratio of dehydrated alcohol B,
It being centrifuged again, it is 8000rpm, centrifugation time 8min that centrifugal rotational speed, which is centrifugal rotational speed,, upper layer centrifugate is outwelled,
It repeats: dehydrated alcohol B dissolution dispersion, deionized water B step with centrifugal separation 3 times is added, the dispersion of fct-FePt nanoparticle is made
It is saved in n-hexane.Measuring the coercivity of its nanoparticle by comprehensive physical property measuring system (PPMS) is 2.3T, is adopted
The sample particle average-size that use transmission Electronic Speculum observes nanoparticle is 8.6nm.
Embodiment 8:
First with ball mill grinding KCl powder, the KCl powder that granularity is 150 μm is obtained.Weigh metal precursor Fe
(acac)3With Pt (acac)2(molar ratio ratio be 1) and low boiling point solvent are added in wide-mouth bottle, low boiling point solvent be n-hexane with
For ethyl alcohol in equal volume than mixed solution, metallic precursor mixed-powder and low boiling point solvent proportion are 1: 400.It is stirred first by machinery
It mixes heating mantle and carries out heating stirring, stirring rate is 2000 revs/min, and metal precursor mixed-powder is substantially dissolved in low boiling
In point solvent, at 75 DEG C, 20min is heated, after metal salt presoma is uniformly dissolved, adding quality is metal front weight
200 times of KCl powder continues to stir under identical stirring rate, at 100 DEG C, 60min is heated, so that KCl powder dissolves and disperses
Uniformly, lysate is formed；Continuation is heated at 100 DEG C, and in the heating process, low boiling point solvent constantly volatilizees in lysate,
And having part KCl precipitation, KCl is as heterogeneous forming core medium, homogeneous nucleation on the surface KCl that metal precursor is formerly precipitated, directly
To heating 40min, low boiling point solvent volatilizees completely, and KCl and metal precursor are precipitated completely, acquires the surface KCl and uniformly covers
It is stamped the mixed-powder of metal precursor.
Mixed-powder is put into silica crucible, and is placed in tube type vacuum heat-treatment furnace, 95%Ar+5%H is used2Also
Primordial Qi atmosphere carries out gas washing, and 600 DEG C of annealing 60min are warming up under this atmospheric condition.Then mixed-powder is cooling after annealing
To room temperature, taking volume ratio is the mixed liquor of 1: 1 deionized water A and dehydrated alcohol A, carries out dissolution point to mixed-powder after annealing
It dissipates；Wherein, according to the ratio, mixed-powder after annealing: deionized water A and mixed liquor=1 dehydrated alcohol A: 60；After dissolution dispersion, warp
High speed centrifugation 8000rpm, centrifugation time 8min remove KCl, outwell upper layer centrifugate, add dehydrated alcohol B dissolution point
It dissipating, wherein mixed-powder after annealing: dehydrated alcohol B=1: 50 adds the deionized water B with the isometric ratio of dehydrated alcohol B,
It is centrifuged again, centrifugal rotational speed 10000rpm, centrifugation time 5min, outwells upper layer centrifugate, repeat: nothing is added
Water-ethanol B dissolution dispersion, deionized water B step with centrifugal separation 3 times, be made fct-FePt nanoparticle be scattered in n-hexane into
Row saves.Measuring the coercivity of its nanoparticle by comprehensive physical property measuring system (PPMS) is 2.1T, is transmitted using Flied emission
The sample particle average-size that Electronic Speculum observes nanoparticle is 13.0nm.
Embodiment 9:
First with ball mill grinding KCl powder, the KCl powder that granularity is 50 μm is obtained.Weigh metal precursor Fe
(acac)3With Pt (acac)2(molar ratio ratio is 0.8) and low boiling point solvent are added in wide-mouth bottle, and low boiling point solvent is n-hexane
With ethyl acetate in equal volume than mixed solution, metallic precursor mixed-powder and low boiling point solvent proportion are 1: 350.Pass through first
Mechanical stirring heating mantle carries out heating stirring, and stirring rate is 2000 revs/min, and metal precursor mixed-powder is sufficiently dissolved
In low boiling point solvent, at 85 DEG C, 15min is heated, after metal salt presoma is uniformly dissolved, adding quality is metal precursor
100 times of KCl powder of quality continues to stir under identical stirring rate, at 120 DEG C, heats 50min, so that KCl powder dissolves
And be uniformly dispersed, form lysate；Continuation is heated at 120 DEG C, and in the heating process, low boiling point solvent is continuous in lysate
Volatilization, and have part KCl precipitation, KCl is as heterogeneous forming core medium, uniform shape on the surface KCl that metal precursor is formerly precipitated
Core, until heating 30min, low boiling point solvent volatilize completely, KCl and metal precursor are precipitated completely, and it is equal to acquire the surface KCl
The even mixed-powder for being covered with metal precursor.
Mixed-powder is put into silica crucible, and is placed in tube type vacuum heat-treatment furnace, 95%Ar+5%H is used2Also
Primordial Qi atmosphere carries out gas washing, and 700 DEG C of annealing 150min are warming up under this atmospheric condition.Then mixed-powder is cooling after annealing
To room temperature, taking volume ratio is the mixed liquor of 1: 1 deionized water A and dehydrated alcohol A, carries out dissolution point to mixed-powder after annealing
It dissipates；Wherein, according to the ratio, mixed-powder after annealing: deionized water A and mixed liquor=1 dehydrated alcohol A: 100；After dissolution dispersion, warp
High speed centrifugation 7000rpm, centrifugation time 8min remove KCl, outwell upper layer centrifugate, add dehydrated alcohol B dissolution point
It dissipating, wherein mixed-powder after annealing: dehydrated alcohol B=1: 50 adds the deionized water B with the isometric ratio of dehydrated alcohol B,
It is centrifuged again, centrifugal rotational speed 10000rpm, centrifugation time 5min, outwells upper layer centrifugate, repeat: nothing is added
Water-ethanol B dissolution dispersion, deionized water B step with centrifugal separation 3 times, be made fct-FePt nanoparticle be scattered in n-hexane into
Row saves.Measuring the coercivity of its nanoparticle by comprehensive physical property measuring system (PPMS) is 2.4T, is transmitted using Flied emission
The sample particle average-size that Electronic Speculum observes nanoparticle is 14.4nm.
Embodiment 10:
First with ball mill grinding KCl powder, the KCl powder that granularity is 300 μm is obtained.Weigh metal precursor Fe
(acac)3With Pt (acac)2(molar ratio ratio is 1.5) and low boiling point solvent are added in wide-mouth bottle, and low boiling point solvent is n-hexane
With petroleum ether in equal volume than mixed solution, metallic precursor mixed-powder and low boiling point solvent proportion are 1: 400.Pass through machine first
Tool agitating and heating set carries out heating stirring, and stirring rate is 2500 revs/min, and metal precursor mixed-powder is substantially dissolved in
In low boiling point solvent, at 100 DEG C, 10min is heated, after metal salt presoma is uniformly dissolved, adding quality is metal precursor
200 times of KCl powder of quality continues under identical stirring rate at 150 DEG C of stirring, heats 40min, so that KCl powder dissolves
And be uniformly dispersed, form lysate；Continuation is heated at 150 DEG C, and in the heating process, low boiling point solvent is continuous in lysate
Volatilization, and have part KCl precipitation, KCl is as heterogeneous forming core medium, uniform shape on the surface KCl that metal precursor is formerly precipitated
Core, until heating 20min, low boiling point solvent volatilize completely, KCl and metal precursor are precipitated completely, and it is equal to acquire the surface KCl
The even mixed-powder for being covered with metal precursor.
Mixed-powder is put into silica crucible, and is placed in tube type vacuum heat-treatment furnace, 95%Ar+5%H is used2Also
Primordial Qi atmosphere carries out gas washing, and 750 DEG C of annealing 30min are warming up under this atmospheric condition.Then mixed-powder is cooling after annealing
To room temperature, taking volume ratio is the mixed liquor of 1: 1 deionized water A and dehydrated alcohol A, carries out dissolution point to mixed-powder after annealing
It dissipates；Wherein, according to the ratio, mixed-powder after annealing: deionized water A and mixed liquor=1 dehydrated alcohol A: 60；After dissolution dispersion, warp
High speed centrifugation 10000rpm, centrifugation time 8min remove KCl, outwell upper layer centrifugate, add dehydrated alcohol B dissolution point
It dissipating, wherein mixed-powder after annealing: dehydrated alcohol B=1: 30 adds the deionized water B with the isometric ratio of dehydrated alcohol B,
It is centrifuged again, centrifugal rotational speed 10000rpm, centrifugation time 5min, outwells upper layer centrifugate, repeat: nothing is added
Water-ethanol B dissolution dispersion, deionized water B step with centrifugal separation 3 times, be made fct-FePt nanoparticle be scattered in n-hexane into
Row saves.Measuring the coercivity of its nanoparticle by comprehensive physical property measuring system (PPMS) is 2.2T, is transmitted using Flied emission
The sample particle average-size that Electronic Speculum observes nanoparticle is 13.6nm.
It can be seen from above-described embodiment that using chemical solid phase method one-step synthesis fct-FePt nanoparticle of the invention
Son has got high magnetic property and the high degree of order, and nanoparticle pattern is uniform, and dispersibility is preferably.
Claims (10)
1. a kind of chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle, which is characterized in that including following
Step:
Step 1: the pretreatment of presoma
(1) ball milling NaCl/KCl particle is utilized, the NaCl/KCl powder that granularity is 500nm~500 μm is obtained, it is spare；
(2) metal precursor powder, including metal precursor Fe (acac) are weighed3Powder and metal precursor Pt (acac)2Powder
End, the two molar ratio is 0.3~2, spare；
Step 2: the mixing of presoma
(1) according to the ratio, metal precursor powder: low boiling point solvent=1: container is added in the two by (300~500), unit g: ml
In；
(2) by heating stirring, it is uniformly dissolved metal precursor powder in low boiling point solvent, wherein the heating temperature
Degree is 50-100 DEG C, and the time is 10~30min；
(3) in metal salt presoma, addition quality is 50~400 times of NaCl/ of metal precursor powder quality after dissolution
KCl powder is heated and is stirred continuously, and successively realizes the dissolution of NaCl/KCl powder, low boiling point solvent volatilization, NaCl/KCl and metal
Presoma is precipitated, and ultimately forms metal precursor and NaCl/KCl mixed-powder, wherein the heating temperature is 50~150
DEG C, heating time is 60~150min；
Step 3: the sintering of presoma
Metal precursor and NaCl/KCl mixed-powder are put into crucible, and are placed in vacuum heat treatment furnace, oxygen-free atmosphere
Under anneal, 550~750 DEG C of annealing temperature, keep the temperature 30~150min, formed annealing after mixed-powder；
The removal of step 4:NaCl/KCl
(1) mixed-powder after annealing is cooled to room temperature, separately removes the mixed liquor of ionized water and dehydrated alcohol, to being mixed after annealing
Powder carries out dissolution dispersion, is centrifuged later, and centrifugal speed is 6000~10000rpm, and centrifugation time is 5~10min, goes
Except NaCl/KCl, upper layer centrifugate is outwelled；
(2) dehydrated alcohol is added, dissolution dispersion is carried out, wherein the additive amount of the dehydrated alcohol according to the ratio, mixes after annealing
Close powder: dehydrated alcohol=1: (30~50), unit g: ml；
(3) add with the deionized water of step (2) dehydrated alcohol grade ratios, be centrifuged again, outwell upper layer centrifugate；
Wherein, centrifugal rotational speed is 6000~10000rpm, and centrifugation time is 5~10min；
(4) step (2)~(3) repeat 3~5 times, and fct-FePt nanoparticle is made.
2. the chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle according to claim 1, special
Sign is, in the step 2 (2), stirring rate is 1000~2500 revs/min.
3. the chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle according to claim 1, special
Sign is, in the step 2 (3), after NaCl/KCl powder is added, and at 50~150 DEG C, the tool of heating 60~150min generation
Body change procedure are as follows: at 50~150 DEG C, heat 40~100min, the dissolution of NaCl/KCl powder forms lysate；Continue 150
At~150 DEG C, 20~50min is heated, low boiling point solvent is made to volatilize, NaCl/KCl and metal precursor are precipitated, before forming metal
Drive body and NaCl/KCl mixed-powder.
4. the chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle according to claim 1, special
Sign is, in the step 3, mixed-powder uses 95%Ar+5%H in advance2After mixed gas carries out gas washing, then anneal
Processing.
5. the chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle according to claim 1, special
Sign is, in the step 3, oxygen-free atmosphere 95%Ar+5%H2Mixed-gas atmosphere.
6. the chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle according to claim 1, special
Sign is, in the step 4 (1), deionized water and dehydrated alcohol are to wait bodies in the mixed liquor of deionized water and dehydrated alcohol
Product mixing.
7. the chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle according to claim 1, special
Sign is, in the step 4 (1), the mixed liquor of mixed-powder and deionized water and dehydrated alcohol proportion is 1: (60 after annealing
~100), unit g: ml.
8. the chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle according to claim 1, special
Sign is, in the step 2 (1), low boiling point solvent is the one or two of ethyl alcohol, ethyl acetate, petroleum ether or n-hexane.
9. the chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle according to claim 1, special
Sign is, in the step 4 (4), the average-size of the fct-FePt nanoparticle of preparation is 4~15nm.
10. the chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle according to claim 1, special
Sign is, in the step 4 (4), the fct-FePt nanoparticle coercivity of preparation reaches 2.0~2.4T.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910549952.1A CN110202166B (en) | 2019-06-24 | 2019-06-24 | Chemical method for synthesizing fct-FePt nano particle by liquid phase assisted solid phase sintering |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910549952.1A CN110202166B (en) | 2019-06-24 | 2019-06-24 | Chemical method for synthesizing fct-FePt nano particle by liquid phase assisted solid phase sintering |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110202166A true CN110202166A (en) | 2019-09-06 |
| CN110202166B CN110202166B (en) | 2021-08-24 |
Family
ID=67794240
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910549952.1A Active CN110202166B (en) | 2019-06-24 | 2019-06-24 | Chemical method for synthesizing fct-FePt nano particle by liquid phase assisted solid phase sintering |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110202166B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113247940A (en) * | 2021-04-26 | 2021-08-13 | 辽宁工程技术大学 | Method for preparing neodymium oxide nanoparticles with small size by solid-phase sintering |
| CN114888298A (en) * | 2022-05-20 | 2022-08-12 | 巢湖学院 | Two-dimensional high-entropy alloy and preparation method and application thereof |
| CN114964976A (en) * | 2022-08-01 | 2022-08-30 | 北矿检测技术有限公司 | Rare earth oxide standard sample and preparation method thereof |
| CN115064718A (en) * | 2022-06-03 | 2022-09-16 | 北京亿华通科技股份有限公司 | Small-particle-size PtFe structure ordered fuel cell catalyst and preparation method and application thereof |
| CN115446304A (en) * | 2022-10-27 | 2022-12-09 | 辽宁工程技术大学 | Superfine Pt-based alloy nano particle and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100759716B1 (en) * | 2006-09-26 | 2007-10-04 | 고려대학교 산학협력단 | Bifunctional magnetic core- semiconductor shell nanoparticles and manufacturing method thereof |
| US20110245068A1 (en) * | 2010-04-05 | 2011-10-06 | Uchicago Argonne, Llc | Highly durable nanoscale electrocatalyst based on core shell particles |
| CN102218543A (en) * | 2011-05-20 | 2011-10-19 | 湖北大学 | Method for one-step synthesis of FePt nanoparticles with an fct (face centered tetragonal) structure and product thereof |
| CN105436510A (en) * | 2014-08-29 | 2016-03-30 | 中国科学院宁波材料技术与工程研究所 | Method for preparing chemical and magnetic ordered-phase nanoparticles |
| CN106541147A (en) * | 2016-11-15 | 2017-03-29 | 哈尔滨工业大学 | A kind of method for preparing hard magnetic nanometer Fe-Pt particle as presoma with inorganic salts |
| CN108817412A (en) * | 2018-07-13 | 2018-11-16 | 陈秋霞 | A kind of preparation method of FePt/Co Nano composite granules |
| CN109604628A (en) * | 2019-02-01 | 2019-04-12 | 东南大学 | A kind of preparation method of ordered phase nanometer Fe-Pt particle and cobalt platinum nano particle |
-
2019
- 2019-06-24 CN CN201910549952.1A patent/CN110202166B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100759716B1 (en) * | 2006-09-26 | 2007-10-04 | 고려대학교 산학협력단 | Bifunctional magnetic core- semiconductor shell nanoparticles and manufacturing method thereof |
| US20110245068A1 (en) * | 2010-04-05 | 2011-10-06 | Uchicago Argonne, Llc | Highly durable nanoscale electrocatalyst based on core shell particles |
| CN102218543A (en) * | 2011-05-20 | 2011-10-19 | 湖北大学 | Method for one-step synthesis of FePt nanoparticles with an fct (face centered tetragonal) structure and product thereof |
| CN105436510A (en) * | 2014-08-29 | 2016-03-30 | 中国科学院宁波材料技术与工程研究所 | Method for preparing chemical and magnetic ordered-phase nanoparticles |
| CN106541147A (en) * | 2016-11-15 | 2017-03-29 | 哈尔滨工业大学 | A kind of method for preparing hard magnetic nanometer Fe-Pt particle as presoma with inorganic salts |
| CN108817412A (en) * | 2018-07-13 | 2018-11-16 | 陈秋霞 | A kind of preparation method of FePt/Co Nano composite granules |
| CN109604628A (en) * | 2019-02-01 | 2019-04-12 | 东南大学 | A kind of preparation method of ordered phase nanometer Fe-Pt particle and cobalt platinum nano particle |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113247940A (en) * | 2021-04-26 | 2021-08-13 | 辽宁工程技术大学 | Method for preparing neodymium oxide nanoparticles with small size by solid-phase sintering |
| CN114888298A (en) * | 2022-05-20 | 2022-08-12 | 巢湖学院 | Two-dimensional high-entropy alloy and preparation method and application thereof |
| CN114888298B (en) * | 2022-05-20 | 2024-01-16 | 巢湖学院 | Two-dimensional high-entropy alloy and preparation method and application thereof |
| CN115064718A (en) * | 2022-06-03 | 2022-09-16 | 北京亿华通科技股份有限公司 | Small-particle-size PtFe structure ordered fuel cell catalyst and preparation method and application thereof |
| CN114964976A (en) * | 2022-08-01 | 2022-08-30 | 北矿检测技术有限公司 | Rare earth oxide standard sample and preparation method thereof |
| CN115446304A (en) * | 2022-10-27 | 2022-12-09 | 辽宁工程技术大学 | Superfine Pt-based alloy nano particle and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110202166B (en) | 2021-08-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110202166A (en) | The chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle | |
| Wu et al. | Influence of some parameters on the synthesis of nanosized NiO material by modified sol–gel method | |
| CN105798320B (en) | A kind of method of low temperature preparation copper nanoparticle | |
| Zhu et al. | Rapid synthesis of copper nanoparticles by sodium hypophosphite reduction in ethylene glycol under microwave irradiation | |
| Ban et al. | A simple synthesis of metallic Ni and Ni–Co alloy fine powders from a mixed-metal acetate precursor | |
| JP4748989B2 (en) | Method for the synthesis of metal nanoparticles | |
| CN109371308B (en) | The method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end | |
| CN101948140B (en) | Method for preparing Fe2O3 and Fe3O4 nano materials by taking F2<2+> salt as raw material | |
| CN108706637B (en) | A kind of preparation method of adjustable magnetic iron oxide mesomorphic material of uniform size | |
| JP4774214B2 (en) | Method for synthesizing metal nanoparticles | |
| CN104891448B (en) | Transition metal oxide nano material, preparation method and application thereof | |
| CN113106281A (en) | Preparation method of yttrium oxide doped tungsten-based nano composite powder and alloy thereof | |
| CN103273071B (en) | Method for preparing nanometer second-phase particle molybdenum alloy mixed powder and product | |
| CN111187075A (en) | Precursor conversion method preparation process of self-dispersion superfine ZrC-SiC ceramic composite powder | |
| CN100467420C (en) | Process for synthesizing nano barium ferrite powder by microwave induction and low-temp combustion | |
| CN102557151A (en) | Method for preparing nanometer ferroferric oxide powder by reducing at one step | |
| CN111848178A (en) | Method for microwave synthesis of hafnium diboride nano powder by complex sol-gel technology | |
| CN102432341B (en) | Submicron-nanometer level red ceramic pigment and manufacturing method thereof | |
| CN102744420B (en) | Preparation method of magnetic nanometer particles with adjustable and controllable particle diameter | |
| CN102583567B (en) | Superfine high-dispersion super-paramagnetism ferrate nano particles and preparation method thereof | |
| Khurshid et al. | Chemically synthesized nanoparticles of iron and iron-carbides | |
| CN101698612B (en) | Homodisperse ferrite magnetic manoparticles and preparation method thereof | |
| CN108946828A (en) | A kind of NiO/In2O3Synthetic method of multilevel structure and products thereof | |
| CN108946812A (en) | Alkali tungsten bronze nanometer rods and its preparation method and application | |
| CN112743097A (en) | Preparation method of fully alloyed monodisperse gold-silver alloy nanoparticles |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |