CN106984829B - A kind of synthetic method of the FeCoNi ternary asymmetric particle of core-shell structure - Google Patents
A kind of synthetic method of the FeCoNi ternary asymmetric particle of core-shell structure Download PDFInfo
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- CN106984829B CN106984829B CN201710307561.XA CN201710307561A CN106984829B CN 106984829 B CN106984829 B CN 106984829B CN 201710307561 A CN201710307561 A CN 201710307561A CN 106984829 B CN106984829 B CN 106984829B
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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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
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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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Abstract
A kind of synthetic method of the FeCoNi ternary asymmetric particle 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 makes it dissolve；3) solution prepared in the solution and step 2) that prepare in step 1) is mixed, continues heating stirring, place the reaction of baking oven high temperature；4) precipitating that step 3) reaction obtains is separated with magnet, is washed 1 time, dehydrated alcohol is at least washed 4 times, and the FeCoNi ternary asymmetric particle of core-shell structure is finally obtained.It is prepared the FeCoNi ternary asymmetry recess particle of core-shell structure for the first time using hydro-thermal method, this material is constructing new function device or material has a good application prospect；Easy to operate, strong operability, favorable reproducibility, yield is up to 95%.
Description
Technical field
The present invention relates to core-shell materials, more particularly, to a kind of synthesis of the FeCoNi ternary asymmetric particle of core-shell structure
Method.
Background technique
1991, De Genne proposed the concept of asymmetric particle in its Nobel gives a lecture for the first time.Due to same
The form or property of particle two sides are different, are referred to as Janus particle.Janus particle is due to unique structure and physical chemistry
The asymmetry of property leads it 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 particle is broadly divided into 3 classes, i.e., organic-organic asymmetric particle, hybrid inorganic-organic asymmetric particle and
Inorganic-inorganic asymmetric particle.There are two main classes for the preparation method of inorganic matter asymmetric particle: one kind is that topology selection is modified
Method can be divided into according to the difference of topology interface: based on flat topology modified (Lin, C.-C.；Liao,C.-W.；Chao,Y.-
C.；Kuo, C.ACS Appl.Mater.Interfaces 2010,2,3185-3191.), Pickering droplet interfaces (spherical surface)
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 of FeCoNi ternary asymmetric particle is rarely reported at present, meanwhile, this ternary alloy three-partalloy has ferromagnetism feature
And preferable electric conductivity, constructing new function device or material has a good application prospect.
Summary of the invention
It is relatively simple that the purpose of the present invention is to provide processing steps, the FeCoNi of the submicron-scale of synthesis 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 resulting ternary alloy three-partalloy
The synthetic method of ternary asymmetric particle.
The present invention the following steps are included:
1) mixed solution of molysite, cobalt salt and nickel salt is prepared；
In step 1), the specific method of the mixed solution for preparing molysite, cobalt salt and nickel salt can are as follows: by sulfuric acid Asia
Iron, cobalt acetate, nickel acetate, or frerrous chloride, cobalt chloride, nickel chloride are added in propylene glycol solution, heating stirring keeps its molten
Solution；
2) sodium hydroxide is added in ethylene glycol solution, heating stirring makes it dissolve；
3) solution prepared in the solution and step 2) that prepare in step 1) is mixed, continues heating stirring, place baking oven
High temperature reaction；
4) precipitating that step 3) reaction obtains is separated with magnet, is washed 1 time, dehydrated alcohol is at least washed 4 times, is finally obtained
The FeCoNi ternary asymmetric particle of core-shell structure.
In step 1), the molar concentration of the molysite, cobalt salt and nickel salt can be 0.025~0.4M.
In step 2), the molar concentration of the sodium hydroxide can be 0.2~2M.
In step 3), solution prepared in step 1) and step 2) is sufficiently mixed, the total volume of ethylene glycol can be
1/2~3/4.
Of the invention has the prominent advantages that: 1) the FeCoNi ternary that core-shell structure is prepared for the first time using hydro-thermal method is not right
Claim recess particle, this material is constructing new function device or material has a good application prospect；2) this synthetic method is grasped
Make simply, strong operability, favorable reproducibility, yield is up to 95%.
Detailed description of the invention
Fig. 1 is that the SEM of the embodiment of the present invention 1 schemes.
Fig. 2 is that the SEM of the embodiment of the present invention 2 schemes.
Fig. 3 is 3SEM of embodiment of the present invention figure.
Fig. 4 is that the SEM of the embodiment of the present invention 4 schemes.
Fig. 5 is that the SEM of the embodiment of the present invention 5 schemes.
Fig. 6 is the obtained X-ray powder diffraction figure of the embodiment of the present invention.
Fig. 7 is the XPS spectrum figure of Fe element in the embodiment of the present invention 3.
Fig. 8 is the XPS spectrum figure of Co element in the embodiment of the present invention 3.
Fig. 9 is the XPS spectrum figure of Ni element in the embodiment of the present invention 3.
Specific embodiment
Below by embodiment combination attached drawing, the invention will be further described.
Embodiment 1
(1) in the reaction kettle of 50ml, 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 is added is 1 ︰, 1 ︰ 2, guarantees that the sum of three's concentration is 0.025M, heating stirring prepares hydroxide later
The ethylene glycol solution of sodium makes its concentration 0.2M, then heating stirring mixes the two, continues stirring and dissolving, final solution
Volume about 30ml, is finally placed in baking oven, 180 DEG C of isothermal reaction 1h or more.
(2) after reaction, reaction solution is cooled to room temperature, is separated product with magnet, resulting product water is clear
It washes, then is cleaned repeatedly with EtOH Sonicate, is dried in vacuo to get FeCoNi ternary alloy three-partalloy.
The ternary asymmetry recess particle for the core-shell structure being 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 be according to the ternary asymmetric particle of the obtained different proportion of feed ratio different in Examples 1 to 5, from
It is also seen that the ratio of Fe meets original ingredient proportion relative to original relatively low, the Co that feeds intake, Ni in table 1.Fig. 6 is basis
The X-ray powder diffraction figure that Examples 1 to 5 obtains, it can be seen that: 44.5 ° of angle of diffraction, 51.8 °, 76.7 ° and 92.7 °
With (111) of Fe:JCPDS No.04-0850, Co:15-0806, or the Ni:65-4150 of face-centred cubic structure, (200),
(220) corresponding with (311) crystal face, and it is not found the appearance of other impurity peaks.In conjunction with the XPS spectrum figure of Fig. 7~9, root
According to the combination energy of tri- kinds of elements of Fe, Co, Ni, by tabling look-up it can be concluded that the surface layer of asymmetric particle is Fe3O4,CoO,Ni2O3,
So it is final we it can be concluded that the asymmetric particle kernel of preparation is the ternary alloy three-partalloy of Fe, Co, Ni, shell Fe, Co, Ni's
Oxide.
Table 1
Embodiment 2
(1) in the reaction kettle of 5L, by ferrous sulfate, cobalt acetate and nickel acetate be added in 1,2-PD stir it is molten
Solution, the ratio between amount of substance that three is added are 1 ︰, 1 ︰ 4, and the sum of control three's concentration is 0.4M, and heating stirring prepares hydroxide later
The ethylene glycol solution of sodium guarantees that its concentration is 2M, then heating stirring mixes the two, continues stirring and dissolving, final solution
Volume about 2.5L, is finally placed in baking oven, 240 DEG C of isothermal reaction 1h or more.
(2) after reaction, reaction solution is cooled to room temperature, is separated product with magnet, resulting product water is clear
It washes, then is cleaned repeatedly with EtOH Sonicate, is dried in vacuo to get FeCoNi ternary alloy three-partalloy.
Embodiment 3
(1) in the reaction kettle of 100ml, 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 is added is 1 ︰, 1 ︰ 6, guarantees that the sum of three's concentration is 0.1M, heating stirring prepares sodium hydroxide later
Ethylene glycol solution, make its concentration 1M, then heating stirring mixes the two, continue stirring and dissolving, the volume of final solution
About 60ml is finally placed in baking oven, 200 DEG C of isothermal reaction 1h or more.
(2) after reaction, reaction solution is cooled to room temperature, is separated product with magnet, resulting product water is clear
It washes, then is cleaned repeatedly with EtOH Sonicate, is dried in vacuo to get FeCoNi ternary alloy three-partalloy.
Embodiment 4
(1) in the reaction kettle of 100ml, 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 is added is 1 ︰, 2 ︰ 3, guarantees that the sum of three's concentration is 0.1M, heating stirring prepares sodium hydroxide later
Ethylene glycol solution, make its concentration 1M, then heating stirring mixes the two, continue stirring and dissolving, the volume of final solution
About 60ml is finally placed in baking oven, 200 DEG C of isothermal reaction 1h or more.
(2) after reaction, reaction solution is cooled to room temperature, is separated product with magnet, resulting product water is clear
It washes, then is cleaned repeatedly with EtOH Sonicate, is dried in vacuo to get FeCoNi ternary alloy three-partalloy.
Embodiment 5
(1) in the reaction kettle of 100ml, 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 is added is 1 ︰, 3 ︰ 2, guarantees that the sum of three's concentration is 0.1M, heating stirring prepares sodium hydroxide later
Ethylene glycol solution, make its concentration 1M, then heating stirring mixes the two, continue stirring and dissolving, the volume of final solution
About 75ml is finally placed in baking oven, 200 DEG C of isothermal reaction 1h or more.
(2) after reaction, reaction solution is cooled to room temperature, is separated product with magnet, resulting product water is clear
It washes, then is cleaned repeatedly with EtOH Sonicate, is dried in vacuo to get FeCoNi ternary alloy three-partalloy.
Claims (2)
1. a kind of synthetic method of the FeCoNi ternary asymmetric particle of core-shell structure, it is characterised in that the following steps are included:
1) mixed solution of molysite, cobalt salt and nickel salt is prepared；The molar concentration of the molysite, cobalt salt and nickel salt summation is 0.025
~0.4M；
2) sodium hydroxide is added in ethylene glycol solution, heating stirring makes it dissolve；The molar concentration of the sodium hydroxide is
0.2~2M；
3) solution prepared in the solution and step 2) that prepare in step 1) is mixed, continues heating stirring, placed high in baking oven
Temperature reaction；
4) precipitating that step 3) reaction obtains is separated with magnet, is washed 1 time, dehydrated alcohol is at least washed 4 times, and nucleocapsid is finally obtained
The FeCoNi ternary asymmetric particle of structure.
2. a kind of synthetic method of the FeCoNi ternary asymmetric particle of core-shell structure as described in claim 1, it is characterised in that
In step 1), the mixed solution for preparing molysite, cobalt salt and nickel salt method particularly includes: by ferrous sulfate, cobalt acetate, second
Sour nickel, or frerrous chloride, cobalt chloride, nickel chloride are added in propylene glycol solution, heating stirring makes it dissolve.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102513125A (en) * | 2011-11-01 | 2012-06-27 | 天津天环光伏太阳能有限公司 | Ternary transition-metal catalyst for ammonia borane hydrolysis and preparation method thereof |
| CN102554257A (en) * | 2012-01-16 | 2012-07-11 | 北京航空航天大学 | Amorphous core-shell structure nanoparticle and preparation method thereof |
| CN102642029A (en) * | 2012-04-24 | 2012-08-22 | 同济大学 | Preparation method of FeNi-Ru alloy nanosphere |
| CN103317146A (en) * | 2013-07-09 | 2013-09-25 | 中国石油大学(华东) | Method for preparing neodymium iron boron powder by means of hydrothermal method |
| CN106229482A (en) * | 2016-08-23 | 2016-12-14 | 兰州金川新材料科技股份有限公司 | A kind of method preparing ternary precursor for raw material with nickel cobalt mixed solution |
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| US7033416B2 (en) * | 2003-05-22 | 2006-04-25 | The United States Of America As Represented By The Secretary Of The Navy | Low temperature synthesis of metallic nanoparticles |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102513125A (en) * | 2011-11-01 | 2012-06-27 | 天津天环光伏太阳能有限公司 | Ternary transition-metal catalyst for ammonia borane hydrolysis and preparation method thereof |
| CN102554257A (en) * | 2012-01-16 | 2012-07-11 | 北京航空航天大学 | Amorphous core-shell structure nanoparticle and preparation method thereof |
| CN102642029A (en) * | 2012-04-24 | 2012-08-22 | 同济大学 | Preparation method of FeNi-Ru alloy nanosphere |
| CN103317146A (en) * | 2013-07-09 | 2013-09-25 | 中国石油大学(华东) | Method for preparing neodymium iron boron powder by means of hydrothermal method |
| CN106229482A (en) * | 2016-08-23 | 2016-12-14 | 兰州金川新材料科技股份有限公司 | A kind of method preparing ternary precursor for raw material with nickel cobalt mixed solution |
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