CN108856729A - The nanometer grain preparation method of the simple substance of Ferrious material or its binary, ternary alloy three-partalloy - Google Patents
The nanometer grain preparation method of the simple substance of Ferrious material or its binary, ternary alloy three-partalloy Download PDFInfo
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- CN108856729A CN108856729A CN201810782107.4A CN201810782107A CN108856729A CN 108856729 A CN108856729 A CN 108856729A CN 201810782107 A CN201810782107 A CN 201810782107A CN 108856729 A CN108856729 A CN 108856729A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a kind of simple substance of Ferrious material or the nanometer grain preparation methods of its binary, ternary alloy three-partalloy, belong to nano particle preparation technical field.It includes the following steps：S1, molysite and/or nickel salt and/or cobalt salt are weighed, is added in organic solvent of the boiling point higher than 250 DEG C, is heated to reflux to obtain precursor solution；S2, so that the precursor solution temperature is down to 150-250 DEG C, and organic reducing agent is added under the conditions of anaerobic is anhydrous, insulation reaction 15-60 minutes, obtain the reaction solution containing nano particle；S3, separation generation product obtains nano particle from the reaction solution containing nano particle；The organic reducing agent includes organolithium and/or Grignard Reagent.Method of the invention is easy to operate, and available degree of scatter is high, partial size is small and the dispersed nano material of consistent appearance, and process equipment requirement is low, process costs are low.
Description
Technical field
The present invention relates to nano particle preparation technical field more particularly to the simple substance or its binary, three of a kind of Ferrious material
The nanometer grain preparation method of first alloy.
Background technique
Magnetic material is a kind of important new material, above has rapid development in application in recent years, from simple letter
Breath storage, electronic device develop to carrier, bio-separation, catalyst, the chemistry of transmitting drug, gene and other biological molecule
Sensor and adsorbent etc..
Iron series element includes three kinds of iron, cobalt, nickel elements.Their atomic radiuses are close, electronegativity is similar, crystal structure phase
Together, therefore continuous solid solution alloy can be formed.More special value be them is the magnetic element of tool, not only metal list
Matter has magnetism, and the binary and ternary alloy three-partalloy of formation also have magnetism.
It is extensive due to application, for demand of the magnetic Nano material in performance also more diversity.Traditional simple substance
Metallic iron, cobalt, nickel, being no longer satisfied has demand, and alloying becomes a direction of magnetic Nano material development.Usually come
Say, second and the third element addition, the adduction of two or three not simple element properties can be in very great Cheng
Arrangement of elements, the lattice parameter of original base metal are adjusted on degree, so that the physical and chemical performance of alloy material is influenced, into
And it can control antioxygenic property, magnetism, the thermal stability etc. of magnetic material by alloying.Therefore, the alloy of magnetic material
Change is of great significance in the development of magnetic material.
The traditional selective laser melting method of method, mechanical ball mill for preparing magnetic nanoparticle and alloying pellet
Method, vapour deposition process, the high-temperature hydrogen reduction method of metal inorganic salt, iron series spinelle hydrogen reduction method, altogether hydrogen plasma method,
Template and electrochemical deposition method etc..Above method usually requires special equipment or relatively high temperature, at high cost, energy consumption
It is high.
It is more commonly used method that nano particle is prepared using wet chemical method.For example, hydro-thermal method can prepare tapping,
The nano particle and its alloying pellet of cobalt, nickel.But for aqueous systems the problem is that particle is uneven, reunion is serious.In for another example
State patent CN103056384B (publication date is on 2 18th, 2015) discloses a kind of preparation method of nano particle, this method
It is the intersolubility using the pure and mild organic solvent of polarity, water-soluble molysite and oil-soluble chemical reactant is fused to a class
In reaction system like microemulsion, reaction solution is centrifugated, lower sediment thing is taken both to obtain nano particle, the advantages of this method is
The nano particle diameter prepared using organic solvent as reaction medium is small and particle diameter distribution is narrow, but the reunion journey of nano particle
Degree is high, brings unfavorable effect to the application of nano particle.
Summary of the invention
(1) technical problems to be solved
In order to solve the above problem of the prior art, the present invention provides the simple substance or its binary, ternary of a kind of Ferrious material
The nanometer grain preparation method of alloy, this method is easy to operate, and available degree of scatter is high, partial size is small and the list of consistent appearance
Disperse nano material, process equipment requirement is low, process costs are low.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include：
A kind of simple substance of Ferrious material or the nanometer grain preparation method of its binary, ternary alloy three-partalloy, include the following steps：
S1, molysite and/or nickel salt and/or cobalt salt are weighed, is added in organic solvent of the boiling point higher than 250 DEG C, is protecting
It is heated to reflux to obtain precursor solution under gas；
S2, so that the precursor solution temperature is down to 150-250 DEG C, and organic reducing agent is added, insulation reaction 15-60 points
Clock, obtains the reaction solution containing nano particle, and the organic reducing agent includes organolithium or Grignard Reagent；
S3, separation generation product obtains nano particle from the reaction solution containing nano particle.
Preferred side as a kind of simple substance of Ferrious material or its bianry alloy, the nanometer grain preparation method of ternary alloy three-partalloy
Case, the organic solvent include diphenyl ether or/or benzyl ether.
As a kind of simple substance of Ferrious material or its binary, the preferred embodiment of the nanometer grain preparation method of ternary alloy three-partalloy,
The molysite includes the chloride, sulfate or acetylacetonate compound of iron；The nickel salt include the chloride of nickel, sulfate or
Acetylacetonate compound；The cobalt salt includes the chloride, sulfate or acetylacetonate compound of cobalt.
As a kind of simple substance of Ferrious material or its binary, the preferred embodiment of the nanometer grain preparation method of ternary alloy three-partalloy,
Integral molar quantity and organic solvent volume the ratio mol/V of the molysite and/or nickel salt and/or cobalt salt are 0.02-1.0mol/100ml.
As a kind of simple substance of Ferrious material or its binary, the preferred embodiment of the nanometer grain preparation method of ternary alloy three-partalloy,
Surface-active is added after the molysite and/or nickel salt and/or cobalt salt is added in organic solvent of the boiling point higher than 250 DEG C
Agent.
As a kind of simple substance of Ferrious material or its binary, the preferred embodiment of the nanometer grain preparation method of ternary alloy three-partalloy,
The surfactant is oleic acid, and the dosage of the oleic acid is the 0.01-1% of gross mass.
As a kind of simple substance of Ferrious material or its binary, the preferred embodiment of the nanometer grain preparation method of ternary alloy three-partalloy,
The dosage of the organic reducing agent is 2-100 times of real reaction dosage.
As a kind of simple substance of Ferrious material or its binary, the preferred embodiment of the nanometer grain preparation method of ternary alloy three-partalloy,
The generation product is cleaned three times with hexane and ethyl alcohol respectively, finally with being dried with nitrogen.
As a kind of simple substance of Ferrious material or its binary, the preferred embodiment of the nanometer grain preparation method of ternary alloy three-partalloy,
The reaction solution containing nano particle is separated with magnet in the space of starvation and generates product.
(3) beneficial effect
The beneficial effects of the invention are as follows：
1, molysite and/or cobalt salt and/or nickel salt are added in organic solvent, are heated to reflux 0.5-4h, what is used is organic
Solvent includes diphenyl ether or benzyl ether；Diphenyl ether and benzyl ether, the two solvent boiling points are respectively 259 DEG C and 298 DEG C, for having
Solvent is a relatively high temperature, since solubility is relatively small in common organic solvents for inorganic salts, herein, is passed through
Solution temperature is improved to improve the solubility of molysite, cobalt salt, nickel salt, the nano particle diameter obtained after redox reaction
Small, reunion degree is low.
2, molysite and/or cobalt salt and/or nickel salt are added in organic solvent, and a certain number of surface-actives is added
Agent；Surfactant molecule structure feature determines that it necessarily forms micella in the solution, passes through selection different structure and property
Surfactant, controls the structure and size of micella, the controllable nano particle of available size, particle shape, meanwhile,
The long tail end of surfactant forms steric hindrance in particle surface, prevents the reunion of nano particle.
3, organic reducing agent is added into reaction system, heats 15-60 minutes under nitrogen protection, the organic reducing used
Agent includes organolithium and Grignard Reagent；Organolithium and Grignard Reagent obtain under conditions of anaerobic is without active hydrogen with iron series reactant salt
Organo-metallic compound, covalent bond in this organo-metallic compound between metal and organic matter is simultaneously unstable, in fire-bar
Decomposite metal nanoparticle under part, if in system being mixed metal salt, since iron series element radius is similar, electronegativity is similar and
Crystal structure is similar, and the metal nanoparticle decomposited in a heated condition can be readily formed alloying pellet.Herein, instead
Process is answered to be divided into two steps, therefore the control that reaction is subject to is more, has eventually formed the dispersed nano that partial size is small, reunion degree is low
Particle.
Detailed description of the invention
The present invention is described by means of the following drawings：
Fig. 1 is transmission electron microscope (TEM) picture of the resulting ferrocobalt nano particle of the embodiment of the present invention 5；
Fig. 2 is transmission electron microscope (TEM) picture of the resulting iron-nickel alloy nano particle of the embodiment of the present invention 6.
Specific embodiment
In order to preferably explain the present invention, in order to understand, with reference to the accompanying drawing, by specific embodiment, to this hair
It is bright to be described in detail.
The present invention discloses a kind of simple substance of Ferrious material or the nanometer grain preparation method of its binary, ternary alloy three-partalloy, including
Following steps：
S1, molysite and/or nickel salt and/or cobalt salt are weighed, be added in organic solvent of the boiling point higher than 250 DEG C, and be added
Surfactant is heated to reflux to obtain precursor solution under protective gas, and the organic solvent includes diphenyl ether and/or dibenzyl
The integral molar quantity of ether, the molysite and/or nickel salt and/or cobalt salt and the organic solvent volume ratio (mol/V) are 0.02-
1.0mol/100ml, the surfactant are oleic acid, and the dosage of the oleic acid is the 0.01%-1% of gross mass；
S2, so that the precursor solution temperature is down to 150-250 DEG C, and organic reducing is added under the conditions of anaerobic is anhydrous
Agent insulation reaction 15-60 minutes, obtains the reaction solution containing nano particle, and the organic reducing agent includes organolithium and/or lattice
Family name's reagent, the dosage of the organic reducing agent are 2-100 times of real reaction dosage；
S3, separation generation product obtains nano particle from the reaction solution containing nano particle.
Embodiment 1
S1, the Fe (SO for weighing 0.1g4)2, it is added in the diphenyl ether of 100ml, and the oleic acid of 1ml is added, in high pure nitrogen
It is heated to reflux under protection 2 hours, after dissolving inorganic salts all, solution temperature is down to 200 DEG C.
S2, the commercially available Grignard Reagent of 3ml is quickly adding into the solution after cooling using syringe, continues to protect in nitrogen
The lower natural cooling after being kept for 200 DEG C of heating 30 minutes of shield.
Above-mentioned reaction solution is transferred in glove box by S3, end of reaction, is separated in glove box with magnet and is generated production
Object, generate product cleaned three times with hexane and ethyl alcohol respectively, i.e., first cleaned three times with hexane, then with ethyl alcohol clean three times (under
Together), to remove oleic acid and other impurities, finally, the iron nano-particle degree of scatter that product with being dried with nitrogen, obtains is high, pattern
Unanimously, particle size 3-9nm.
Embodiment 2
S1, the CoCl for weighing 0.05g2, it is added in the benzyl ether of 80ml, and the oleic acid of 0.5ml is added, in high pure nitrogen
It is heated to reflux under protection 2.5 hours, after dissolving inorganic salts all, solution temperature is down to 180 DEG C.
S2, the commercially available n-BuLi of 2.5ml is quickly adding into the solution after cooling using syringe, is continued in nitrogen
Protection is lower to keep 180 DEG C of heating natural cooling after twenty minutes.
Above-mentioned reaction solution is transferred in glove box by S3, end of reaction, is separated in glove box with magnet and is generated production
Object generates product and is cleaned three times with hexane and ethyl alcohol respectively, to remove oleic acid and other impurities, finally, product is with being dried with nitrogen,
Obtained cobalt nano-particle degree of scatter is high, consistent appearance, particle size 3-13nm.
Embodiment 3
S1, the Ni (acac) for weighing 0.2g2, it is added in the diphenyl ether of 150ml, and the oleic acid of 1.1ml is added, high-purity
It is heated to reflux under nitrogen protection 3 hours, after dissolving inorganic salts all, solution temperature is down to 210 DEG C.
S2, the commercially available Grignard Reagent of 3.5ml is quickly adding into the solution after cooling using syringe, is continued in nitrogen
The lower natural cooling after being kept for 210 DEG C of heating 25 minutes of protection.
Above-mentioned reaction solution is transferred in glove box by S3, end of reaction, is separated in glove box with magnet and is generated production
Object generates product and is cleaned three times with hexane and ethyl alcohol respectively, to remove oleic acid and other impurities, finally, product is with being dried with nitrogen,
Obtained nano nickel particles degree of scatter is high, consistent appearance, particle size 4-8nm.
Embodiment 4
S1, the NiCl for weighing 0.052g2With the CoCl of 0.060g2, it is added in the benzyl ether of 100ml, and 0.9ml is added
Oleic acid, high pure nitrogen protection under be heated to reflux 1 hour, make inorganic salts all dissolution after, solution temperature is down to 180 DEG C.
S2, the commercially available n-BuLi of 4ml is quickly adding into the solution after cooling using syringe, continues to protect in nitrogen
Shield is lower to keep 180 DEG C of heating natural cooling after sixty minutes.
Above-mentioned reaction solution is transferred in glove box by S3, end of reaction, is separated in glove box with magnet and is generated production
Object generates product and is cleaned three times with hexane and ethyl alcohol respectively, to remove oleic acid and other impurities, finally, product is with being dried with nitrogen,
Obtained nickel-cobalt alloy nano particle degree of scatter is high, consistent appearance, particle size 2-11nm.
Embodiment 5
S1, the FeCl for weighing 0.152g2With the CoCl of 0.160g2, it is added in the diphenyl ether of 200ml, and 1.2ml is added
Oleic acid, high pure nitrogen protection under be heated to reflux 1 hour, make inorganic salts all dissolution after, solution temperature is down to 180 DEG C.
S2, the commercially available Grignard Reagent of 5.5ml is quickly adding into the solution after cooling using syringe, is continued in nitrogen
Protection is lower to keep 180 DEG C of heating natural cooling after sixty minutes.
Above-mentioned reaction solution is transferred in glove box by S3, end of reaction, is separated in glove box with magnet and is generated production
Object generates product and is cleaned three times with hexane and ethyl alcohol respectively, to remove oleic acid and other impurities, finally, product is with being dried with nitrogen,
Obtain ferrocobalt nano particle.Fig. 1 is transmission electron microscope (TEM) figure of the ferrocobalt nano particle of the present embodiment
Piece, it can be seen from the figure that the diameter of gained ferrocobalt nano particle is 2-6nm.
Embodiment 6
S1, the NiCl for weighing 0.1g2With the FeCl of 0.070g2, it is added in the diphenyl ether of 130ml, and be added 0.9ml's
Oleic acid is heated to reflux 1.6 hours under high pure nitrogen protection, after dissolving inorganic salts all, solution temperature is down to 185 DEG C.
S2, the commercially available n-BuLi of 4.2ml is quickly adding into the solution after cooling using syringe, is continued in nitrogen
The lower natural cooling after being kept for 185 DEG C of heating 55 minutes of protection.
Above-mentioned reaction solution is transferred in glove box by S3, end of reaction, is separated in glove box with magnet and is generated production
Object generates product and is cleaned three times with hexane and ethyl alcohol respectively, to remove oleic acid and other impurities, finally, product is with being dried with nitrogen,
Obtain iron-nickel alloy nano particle.Fig. 1 is transmission electron microscope (TEM) figure of the iron-nickel alloy nano particle of the present embodiment
Piece, it can be seen from the figure that the diameter of gained iron-nickel alloy nano particle is 3-6nm.
Embodiment 7
S1, the Ni (acac) for weighing 0.056g2、0.065g Co(acac)2With the Fe (acac) of 0.066g2, it is added to
In the diphenyl ether of 100ml, and the oleic acid of 0.75ml is added, is heated to reflux 2 hours under high pure nitrogen protection, keeps inorganic salts whole
After dissolution, solution temperature is down to 250 DEG C.
S2, the commercially available n-BuLi of 4ml is quickly adding into the solution after cooling using syringe, continues to protect in nitrogen
Shield is lower to keep 250 DEG C of heating natural cooling after sixty minutes.
Above-mentioned reaction solution is transferred in glove box by S3, end of reaction, is separated in glove box with magnet and is generated production
Object generates product and is cleaned three times with hexane and ethyl alcohol respectively, to remove oleic acid and other impurities, finally, product is with being dried with nitrogen,
It is high to obtain teleoseal nano particle degree of scatter, consistent appearance, particle size 3-7nm.
It is to be appreciated that describing the skill simply to illustrate that of the invention to what specific embodiments of the present invention carried out above
Art route and feature, its object is to allow those skilled in the art to can understand the content of the present invention and implement it accordingly, but
The present invention is not limited to above-mentioned particular implementations.All various changes made within the scope of the claims are repaired
Decorations, should be covered by the scope of protection of the present invention.
Claims (9)
1. the nanometer grain preparation method of a kind of simple substance of Ferrious material or its binary, ternary alloy three-partalloy, which is characterized in that including with
Lower step：
S1, molysite and/or nickel salt and/or cobalt salt are weighed, be added in organic solvent of the boiling point higher than 250 DEG C, under protective gas
It is heated to reflux to obtain precursor solution；
S2, so that the precursor solution temperature is down to 150-250 DEG C, and organic reducing agent is added, insulation reaction 15-60 minutes,
Obtain the reaction solution containing nano particle；
S3, separation generates product from the reaction solution containing nano particle, obtains nano particle；
The organic reducing agent includes organolithium and/or Grignard Reagent.
2. the nanometer grain preparation method of the simple substance of Ferrious material as described in claim 1 or its binary, ternary alloy three-partalloy, special
Sign is：The organic solvent includes diphenyl ether and/or benzyl ether.
3. the nanometer grain preparation method of the simple substance of Ferrious material as described in claim 1 or its binary, ternary alloy three-partalloy, special
Sign is：
The molysite includes the chloride, sulfate or acetylacetonate compound of iron；
The nickel salt includes the chloride, sulfate or acetylacetonate compound of nickel；
The cobalt salt includes the chloride, sulfate or acetylacetonate compound of cobalt.
4. the nanometer grain preparation method of the simple substance of Ferrious material as described in claim 1 or its binary, ternary alloy three-partalloy, special
Sign is：The volume ratio mol/V of the integral molar quantity and organic solvent of the molysite and/or nickel salt and/or cobalt salt is 0.02-
1.0mol/100ml。
5. the nanometer grain preparation method of the simple substance of Ferrious material as described in claim 1 or its binary, ternary alloy three-partalloy, special
Sign is：In step S1, the molysite and/or nickel salt and/or cobalt salt is added in organic solvent of the boiling point higher than 250 DEG C
After add surfactant.
6. the nanometer grain preparation method of the simple substance of Ferrious material as claimed in claim 5 or its binary, ternary alloy three-partalloy, special
Sign is：The surfactant is oleic acid, and the dosage of the oleic acid is the 0.01-1% of gross mass.
7. the nanometer grain preparation method of the simple substance of Ferrious material as described in claim 1 or its binary, ternary alloy three-partalloy, special
Sign is：The dosage of the organic reducing agent is 2-100 times of real reaction dosage.
8. the nanometer grain preparation method of the simple substance of Ferrious material as described in claim 1 or its binary, ternary alloy three-partalloy, special
Sign is：In step S3, the generation product is cleaned three times with hexane and ethyl alcohol respectively, finally with being dried with nitrogen, is obtained described
Nano particle.
9. the nano particle preparation of the simple substance of Ferrious material as claimed in any one of claims 1 to 8 or its binary, ternary alloy three-partalloy
Method, it is characterised in that：In step S3, the separation includes being separated in the space of starvation with magnet.
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Cited By (1)
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| CN110592606A (en) * | 2019-09-25 | 2019-12-20 | 哈尔滨工业大学 | Preparation method and application of gold-iron nano alloy catalyst |
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Application publication date: 20181123 |