CN106984829A - A kind of synthetic method of the FeCoNi ternary asymmetric particles of core shell structure - Google Patents
A kind of synthetic method of the FeCoNi ternary asymmetric particles of core shell structure Download PDFInfo
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- CN106984829A CN106984829A CN201710307561.XA CN201710307561A CN106984829A CN 106984829 A CN106984829 A CN 106984829A CN 201710307561 A CN201710307561 A CN 201710307561A CN 106984829 A CN106984829 A CN 106984829A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- 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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- 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
- B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
A kind of synthetic method of the FeCoNi ternary asymmetric particles of core shell structure, is related to core-shell material.1) mixed solution of molysite, cobalt salt and nickel salt is prepared；2) sodium hydroxide is added in ethylene glycol solution, heating stirring dissolves it；3) by step 1) in the solution and the step 2 that prepare) in the solution for preparing mix, continue heating stirring, place the reaction of baking oven high temperature；4) by step 3) the obtained precipitation of reaction separates with magnet, washed 1 time, absolute ethyl alcohol is at least washed 4 times, finally obtains the FeCoNi ternary asymmetric particles of core shell structure.Prepare the asymmetric recess particle of FeCoNi ternarys of core shell structure first using hydro-thermal method, this material has good application prospect constructing new function device or material；It is simple to operate, workable, favorable reproducibility, yield is up to 95%.
Description
Technical field
The present invention relates to core-shell material, more particularly, to a kind of synthesis of the FeCoNi ternary asymmetric particles of core shell structure
Method.
Background technology
1991, De Genne proposed the concept of asymmetric particle for the first time in its Nobel gives a lecture.Due to same
The form or property of particle both sides are different, are referred to as Janus particles.Janus particles are due to unique structure and physical chemistry
The asymmetry of property makes it be led in modifying interface, Electronic Paper, surfactant, molecular recognition and self assembly, target administration etc.
Domain has a wide range of applications, therefore causes the great interest of scientist.
Janus particles are broadly divided into 3 classes, i.e., organic-organic asymmetric particle, hybrid inorganic-organic asymmetric particle and
Inorganic-inorganic asymmetric particle.The preparation method of inorganic matter asymmetric particle mainly has two classes：One class is that topology selection is modified
Method, according to the difference of topology interface, can be divided into：(Lin, C.-C. are modified based on flat topology；Liao,C.-W.；Chao,Y.-
C.；Kuo, C.ACS Appl.Mater.Interfaces 2010,2,3185-3191.), Pickering droplet interfaces (sphere)
Topology modification etc.；Another kind of is asymmetric deposition growing (Choi, J.-S. based on seed nanoparticles；Jun,Y.-W.；
Yeon,S.I.；Kim,H.C.；Shin,J.-S.；Cheon,J.J.Am.Chem.Soc.2006,128,15982-15983.).So
And, the research for FeCoNi ternary asymmetric particles at present is rarely reported, meanwhile, this ternary alloy three-partalloy has ferromagnetism feature
And preferable electric conductivity, there is good application prospect constructing new function device or material.
The content of the invention
It is relatively simple it is an object of the invention to provide processing step, synthesize the FeCoNi of the submicron-scale of core shell structure
Ternary alloy three-partalloy particle, the FeCoNi for being structurally characterized in that a kind of core shell structure with obvious recess pattern of the ternary alloy three-partalloy of gained
The synthetic method of ternary asymmetric particle.
The present invention comprises the following steps：
1) mixed solution of molysite, cobalt salt and nickel salt is prepared；
In step 1) in, the specific method of the mixed solution for preparing molysite, cobalt salt and nickel salt can be：Sulfuric acid is sub-
Iron, cobalt acetate, nickel acetate, or frerrous chloride, cobalt chloride, nickel chloride are added in propylene glycol solution, heating stirring makes its molten
Solution；
2) sodium hydroxide is added in ethylene glycol solution, heating stirring dissolves it；
3) by step 1) in the solution and the step 2 that prepare) in the solution for preparing mix, continue heating stirring, place baking oven
High temperature is reacted；
4) by step 3) the obtained precipitation of reaction separates with magnet, washed 1 time, absolute ethyl alcohol is at least washed 4 times, is finally obtained
The FeCoNi ternary asymmetric particles of core shell structure.
In step 1) in, the molar concentration of the molysite, cobalt salt and nickel salt can be 0.025~0.4M.
In step 2) in, the molar concentration of the sodium hydroxide can be 0.2~2M.
In step 3) in, by step 1) and step 2) in prepared solution be sufficiently mixed, the cumulative volume of ethylene glycol can be
1/2~3/4.
The present invention's has the prominent advantages that：1) the FeCoNi ternarys for preparing core shell structure first using hydro-thermal method are not right
Claim recess particle, this material has good application prospect constructing new function device or material；2) this synthetic method is grasped
Make simple, workable, favorable reproducibility, yield is up to 95%.
Brief description of the drawings
Fig. 1 schemes for the SEM of the embodiment of the present invention 1.
Fig. 2 schemes for the SEM of the embodiment of the present invention 2.
Fig. 3 schemes for 3SEM of the embodiment of the present invention.
Fig. 4 schemes for the SEM of the embodiment of the present invention 4.
Fig. 5 schemes for the SEM of the embodiment of the present invention 5.
Fig. 6 is the X-ray powder diffraction figure obtained by embodiments of the invention.
Fig. 7 is the XPS spectrum figure of Fe elements in the embodiment of the present invention 3.
Fig. 8 is the XPS spectrum figure of Co elements in the embodiment of the present invention 3.
Fig. 9 is the XPS spectrum figure of Ni elements in the embodiment of the present invention 3.
Embodiment
Below by embodiment combination accompanying drawing, the invention will be further described.
Embodiment 1
(1) in 50ml reactor, by ferrous sulfate, cobalt acetate and nickel acetate are added to stirring and dissolving in ethylene glycol,
The ratio between amount of substance that three adds is the ︰ 2 of 1 ︰ 1, it is ensured that three's concentration sum is 0.025M, and heating stirring prepares hydroxide afterwards
The ethylene glycol solution of sodium, it is 0.2M to make its concentration, and then heating stirring mixes both, continues stirring and dissolving, final solution
Volume about 30ml, is finally placed in baking oven, 180 DEG C of more than isothermal reaction 1h.
(2) after reaction terminates, reaction solution is cooled to room temperature, product is separated with magnet, the product of gained is clear with water
Wash, then cleaned repeatedly with EtOH Sonicate, be dried in vacuo, produce FeCoNi ternary alloy three-partalloys.
The asymmetric recess particle of ternary of the core shell structure prepared as seen from Figure 1 according to embodiment 1.By Fig. 2
~5 be the asymmetric particle of the different proportion obtained according to embodiment 2~5, and scale topography is more unified, it was demonstrated that synthesis mode
Universality.Table 1 is the ternary asymmetric particle according to the different proportion obtained by rate of charge different in embodiment 1~5, from
It is also seen that Fe ratio is relatively low relative to original rate of charge in table 1, Co, Ni meets original ingredient proportion.Fig. 6 is basis
The X-ray powder diffraction figure that embodiment 1~5 is obtained, it can be seen that：44.5 °, 51.8 °, 76.7 ° and 92.7 ° of angle of diffraction
With the Fe of face-centred cubic structure:JCPDS No.04-0850,Co:15-0806, or Ni：65-4150 (111), (200),
(220) it is corresponding with (311) crystal face, and the appearance of other impurity peaks is not found.With reference to the XPS spectrum figure of Fig. 7~9, root
According to the combination energy of tri- kinds of elements of Fe, Co, Ni, the top layer that asymmetric particle can be drawn by tabling look-up is Fe3O4,CoO,Ni2O3,
So finally we can draw ternary alloy three-partalloy of the asymmetric particle kernel of preparation for Fe, Co, Ni, shell is Fe, Co, Ni
Oxide.
Table 1
Embodiment 2
(1) in 5L reactor, by ferrous sulfate, cobalt acetate and nickel acetate are added in 1,2-PD and stir molten
Solve, the ratio between amount of substance that three adds is the ︰ 4 of 1 ︰ 1, it is 0.4M to control three's concentration sum, heating stirring prepares hydroxide afterwards
The ethylene glycol solution of sodium, it is ensured that its concentration is 2M, then heating stirring mixes both, continues stirring and dissolving, final solution
Volume about 2.5L, is finally placed in baking oven, 240 DEG C of more than isothermal reaction 1h.
(2) after reaction terminates, reaction solution is cooled to room temperature, product is separated with magnet, the product of gained is clear with water
Wash, then cleaned repeatedly with EtOH Sonicate, be dried in vacuo, produce FeCoNi ternary alloy three-partalloys.
Embodiment 3
(1) in 100ml reactor, by ferrous sulfate, cobalt acetate and nickel acetate are added to stirring and dissolving in ethylene glycol,
The ratio between amount of substance that three adds is the ︰ 6 of 1 ︰ 1, it is ensured that three's concentration sum is 0.1M, and heating stirring prepares sodium hydroxide afterwards
Ethylene glycol solution, it is 1M to make its concentration, and then heating stirring mix both, continues stirring and dissolving, the volume of final solution
About 60ml, is finally placed in baking oven, 200 DEG C of more than isothermal reaction 1h.
(2) after reaction terminates, reaction solution is cooled to room temperature, product is separated with magnet, the product of gained is clear with water
Wash, then cleaned repeatedly with EtOH Sonicate, be dried in vacuo, produce FeCoNi ternary alloy three-partalloys.
Embodiment 4
(1) in 100ml reactor, by frerrous chloride, cobalt chloride and nickel chloride are added to stirring and dissolving in ethylene glycol,
The ratio between amount of substance that three adds is the ︰ 3 of 1 ︰ 2, it is ensured that three's concentration sum is 0.1M, and heating stirring prepares sodium hydroxide afterwards
Ethylene glycol solution, it is 1M to make its concentration, and then heating stirring mix both, continues stirring and dissolving, the volume of final solution
About 60ml, is finally placed in baking oven, 200 DEG C of more than isothermal reaction 1h.
(2) after reaction terminates, reaction solution is cooled to room temperature, product is separated with magnet, the product of gained is clear with water
Wash, then cleaned repeatedly with EtOH Sonicate, be dried in vacuo, produce FeCoNi ternary alloy three-partalloys.
Embodiment 5
(1) in 100ml reactor, by frerrous chloride, cobalt nitrate and nickel nitrate are added to stirring and dissolving in ethylene glycol,
The ratio between amount of substance that three adds is the ︰ 2 of 1 ︰ 3, it is ensured that three's concentration sum is 0.1M, and heating stirring prepares sodium hydroxide afterwards
Ethylene glycol solution, it is 1M to make its concentration, and then heating stirring mix both, continues stirring and dissolving, the volume of final solution
About 75ml, is finally placed in baking oven, 200 DEG C of more than isothermal reaction 1h.
(2) after reaction terminates, reaction solution is cooled to room temperature, product is separated with magnet, the product of gained is clear with water
Wash, then cleaned repeatedly with EtOH Sonicate, be dried in vacuo, produce FeCoNi ternary alloy three-partalloys.
Claims (5)
1. the synthetic method of the FeCoNi ternary asymmetric particles of a kind of core shell structure, it is characterised in that comprise the following steps：
1) mixed solution of molysite, cobalt salt and nickel salt is prepared；
2) sodium hydroxide is added in ethylene glycol solution, heating stirring dissolves it；
3) by step 1) in the solution and the step 2 that prepare) in the solution for preparing mix, continue heating stirring, place high in baking oven
Temperature reaction；
4) by step 3) the obtained precipitation of reaction separates with magnet, washed 1 time, absolute ethyl alcohol is at least washed 4 times, finally obtains nucleocapsid
The FeCoNi ternary asymmetric particles of structure.
2. a kind of synthetic method of the FeCoNi ternary asymmetric particles of core shell structure as claimed in claim 1, it is characterised in that
In step 1) in, the specific method of the mixed solution for preparing molysite, cobalt salt and nickel salt is：By ferrous sulfate, cobalt acetate, second
Sour nickel, or frerrous chloride, cobalt chloride, nickel chloride are added in propylene glycol solution, heating stirring dissolves it.
3. a kind of synthetic method of the FeCoNi ternary asymmetric particles of core shell structure as claimed in claim 1, it is characterised in that
In step 1) in, the molar concentration of the molysite, cobalt salt and nickel salt is 0.025~0.4M.
4. a kind of synthetic method of the FeCoNi ternary asymmetric particles of core shell structure as claimed in claim 1, it is characterised in that
In step 2) in, the molar concentration of the sodium hydroxide is 0.2~2M.
5. a kind of synthetic method of the FeCoNi ternary asymmetric particles of core shell structure as claimed in claim 1, it is characterised in that
In step 3) in, by step 1) and step 2) in prepared solution be sufficiently mixed, the cumulative volume of ethylene glycol is 1/2~3/4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111363517A (en) * | 2020-04-16 | 2020-07-03 | 广州特种承压设备检测研究院 | CoNi @ C/PVDF composite efficient wave-absorbing material and preparation method thereof |
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| US20040231464A1 (en) * | 2003-05-22 | 2004-11-25 | Kurihara Lynn K. | Low temperature synthesis of metallic nanoparticles |
| CN102274977A (en) * | 2011-08-19 | 2011-12-14 | 北京航空航天大学 | Method for preparing synthesized cobalt-gold double-metal alloy nano particle |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111363517A (en) * | 2020-04-16 | 2020-07-03 | 广州特种承压设备检测研究院 | CoNi @ C/PVDF composite efficient wave-absorbing material and preparation method thereof |
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