CN107159901A - A kind of magnetic alloy nanosphere body and the method for cube controllable preparation - Google Patents

A kind of magnetic alloy nanosphere body and the method for cube controllable preparation Download PDF

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Publication number
CN107159901A
CN107159901A CN201710327267.5A CN201710327267A CN107159901A CN 107159901 A CN107159901 A CN 107159901A CN 201710327267 A CN201710327267 A CN 201710327267A CN 107159901 A CN107159901 A CN 107159901A
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China
Prior art keywords
magnetic alloy
cube
acac
controllable preparation
nanosphere body
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CN201710327267.5A
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Inventor
成汉文
朱丽莹
沈悦
蒋婧
华中慧
罗谨
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Shanghai Institute of Technology
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Shanghai Institute of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • B22F1/0553Complex form nanoparticles, e.g. prism, pyramid, octahedron
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2201/00Treatment under specific atmosphere
    • B22F2201/02Nitrogen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2201/00Treatment under specific atmosphere
    • B22F2201/10Inert gases
    • B22F2201/11Argon

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention discloses a kind of magnetic alloy nanosphere body and the method for cube controllable preparation.The present invention is by first by Fe (acac)3、Mn(acac)2With Zn (acac)2Be dissolved in organic stabilizer, then under inert gas shielding pass through weak reductant heating means synthesis containing iron, manganese, zinc and oxygen element magnetic alloy nanometer son;In heating process, particle morphology develops into alloy cube with extending heating time from alloy spheroid.The beneficial effects of the present invention are:Application with magnetic alloy material in fields such as bio-separation, drug deliveries is more and more wider, and particle size, composition, the controllability synthetic method of pattern provide feasibility preferably to expand its application in more many body system.

Description

A kind of magnetic alloy nanosphere body and the method for cube controllable preparation
Technical field
The present invention relates to technical field of nanometer material preparation, specifically, be a kind of magnetic alloy nanosphere body with cube The method of body controllable preparation.
Background technology
Development functional nanoparticles are used to realize that the research of biomolecule intervention and detection is more and more.Such as, some light It is both that make use of nano material so as to the important tool as biochemical research to learn probe, and it, which is optimized, it is possessed Gao Ling Sensitivity and very strong spectral fingerprint characteristic.Such instrument can Molecular Detection, bacterium and cell imaging, organizational diagnosis and Applied in the multi-level chemistry and biology field such as bio-imaging.But, how optical probe is improving detection signal Reappearance, how to develop in terms of the biocompatibility of multi-functional combined probe and also there are many problems.
In recent years, biomolecule conjugation has been carried out to nano-particle or magnetic nano-particle, become with uniqueness The Nanoparticle labeling thing of biocompatibility, and it is used as the probe in field of bioanalysis and carrier is subject to the people's attention. And the magnetic nano-particle synthetic method continued to develop can realize magnet tuning, and volume can be controlled at several nanometers to tens In individual nanometer range, this is closely sized to or isometric less than virus, protein molecule and gene;In addition, with superparamagnetism Magnetic nano-particle, can be regulated and controled by external magnetic field, so formation and separation to immune structure and to tumor tissues Site-specific delivery of drugs provides possibility.
Although however, existing many research workers were carried out to the synthesis of metal magnetic nano-particle, sign and application Research, but the size for particle, shape, the understanding of the accurate control of composition and surface property also lack very much, and chi Very little and morphology controllable, the preparation method of the adjustable magnetic alloy nano-particle of magnetic are not set up.
The content of the invention
For above technical problem, it can control it is an object of the invention to provide a kind of magnetic alloy nanosphere body and cube Standby method, this method is simply controllable, and obtained nano-particles size is between 1~20 nanometer.
To achieve these goals, the technical solution adopted by the present invention is as follows.
The present invention provides a kind of magnetic alloy nanosphere body and the method for cube controllable preparation, first by Fe (acac)3、Mn (acac)2With Zn (acac)2It is dissolved in organic stabilizer, then closed under inert gas shielding by weak reductant heating means Into the magnetic alloy nano-particle containing iron, manganese, zinc and oxygen element;In weak reductant heating process, extending heating time, particle Pattern develops into cube from spheroid;Wherein:The organic stabilizer is the benzyl ethereal solution of oleic acid and oleyl amine;Weak reductant is Oleyl amine in organic stabilizer.
In the present invention, in organic stabilizer, oleic acid and oleyl amine mol ratio are 1:1;Heating-up temperature is 280 ± 2 DEG C, during heating Between be 20~80 minutes.
In the present invention, when the heat time is 20~35 minutes, magnetic alloy nano-particle is spherical in shape;Heat time be 35~ At 80 minutes, magnetic alloy nano-particle is in cubic type.
In the present invention, inert gas is nitrogen or argon gas.
In the present invention, weak reductant is simultaneously as the oleyl amine of component in stabilizer.
In the present invention, described magnetic alloy nano-particles size is between 1~20 nanometer.
In the present invention, Fe (acac)3、Mn(acac)2With Zn (acac)2Mol ratio be 4:1:1.
In the present invention, oleic acid, oleyl amine and Fe (acac)3Three's mol ratio be:8:8:(1~2).
Compared to the prior art, the beneficial effects of the present invention are:The inventive method can realize magnetic alloy nanosphere Body and cube controllable preparation:Application with magnetic alloy material in fields such as bio-separation, drug deliveries is more and more wider, grain Sub- size, composition, the controllability synthetic method of pattern provide feasibility preferably to expand its application in more many body system.
Brief description of the drawings
Fig. 1 for embodiment 1~7 nanometers of magnetic alloy nanosphere body electron microscope.
Fig. 2 for embodiment 2~15 nanometers of magnetic alloy nanosphere body electron microscope.
Embodiment
Technical scheme is further described with reference to specific embodiment, but the present invention is not limited to Following embodiments.
Various raw materials used, are commercially available unless otherwise specified in various embodiments of the present invention.
Embodiment 1
(~7 nanometers) controllable preparation of magnetic alloy nanosphere body and sign:
(1) preparation of reactant, stabilizer
Fe(acac)3、Mn(acac)2、Zn(acac)2Anabolic reaction agent, three's consumption be followed successively by 2.40 mMs, 0.60 MM, 0.60 mM;In addition, the benzyl ether solvents of 12.0 mMs of oleic acid and 12.0 mMs of oleyl amine at 80 milliliters In be mixed into stabilizer, under inert gas, reactant and stabilizer are stirred mixing in flask.
(2) the heating building-up process of magnetic alloy particle
Above-mentioned mixed liquor is heated using heater, under inert gas, is risen with 3 DEG C per minute of speed and added Hot temperature is until 280 DEG C.From the point of view of the result of test of many times:Particle morphology is different because of heating duration difference, 20~35 minutes Alloy spheroid can be obtained;Alloy cube was then obtained higher than 35 minutes;Higher than 80 minutes, then cube pattern tended to be random.Cause This, reaches after 280 DEG C of target temperature, a length of 32 minutes when maintaining to heat.
(3) the final pattern and size of magnetic alloy particle
Magnetic particle is shape characteristic nanosphere body as obtained by ESEM (Fig. 1) determines synthesis, and average grain diameter is 7.3 ± 0.8 nanometer.
(4) composition of magnetic alloy particle
Using x-ray photoelectron power spectrum (XPS) technical Analysis Mn 2p, Zn 2p, Fe 2p and determine magnetic alloy particle Final composition (%) is Mn:22.1、Zn:16.4、Fe:61.4.
Embodiment 2
(~15 nanometers) controllable preparation of magnetic alloy nanocube and sign:
(1) preparation of reactant, stabilizer
Fe(acac)3、Mn(acac)2、Zn(acac)2Anabolic reaction agent, three's consumption is followed successively by:6.0 mMs, 1.5 millis Mole, 1.5 mMs;In addition, 30 mMs of oleic acid and 30 mMs of oleyl amine are mixed in 200 milliliters of benzyl ether solvents Into stabilizer, under inert gas, reactant and stabilizer are stirred mixing in flask.
(2) the heating building-up process of magnetic alloy particle
Above-mentioned mixed liquor is heated using heater, under inert gas, is risen with 4 DEG C per minute of speed and added Hot temperature is until 281 DEG C.From the point of view of the result of test of many times:Particle morphology is different because of heating duration difference, 20~35 minutes Alloy spheroid can be obtained;Alloy cube was then obtained higher than 35 minutes;Higher than 80 minutes, then cube pattern tended to be random.Cause This, reaches after 281 DEG C of target temperature, a length of 65 minutes when maintaining to heat.
(3) the final pattern and size of magnetic alloy particle
Magnetic particle is shape characteristic nanocube as obtained by ESEM (Fig. 2) determines synthesis, and average grain diameter is 15.6 ± 1.1 nanometers.
(4) composition of magnetic alloy particle
Using x-ray photoelectron power spectrum (XPS) technical Analysis Mn 2p, Zn 2p, Fe 2p and determine magnetic alloy particle Final composition (%) is Mn:20.8、Zn:15.9、Fe:63.2.

Claims (8)

1. a kind of magnetic alloy nanosphere body and the method for cube controllable preparation, it is characterised in that first by Fe (acac)3、Mn (acac)2With Zn (acac)2It is dissolved in organic stabilizer, then closed under inert gas shielding by weak reductant heating means Into the magnetic alloy nano-particle containing iron, manganese, zinc and oxygen element;In weak reductant heating process, extending heating time, particle Pattern develops into cube from spheroid;Wherein:The organic stabilizer is the benzyl ethereal solution of oleic acid and oleyl amine;Weak reductant is Oleyl amine in organic stabilizer.
2. magnetic alloy nanosphere body according to claim 1 and the method for cube controllable preparation, it is characterised in that have In machine stabilizer, oleic acid and oleyl amine mol ratio are 1:1;Heating-up temperature is 280 ± 2 DEG C, and the heat time is 20~80 minutes.
3. magnetic alloy nanosphere body according to claim 2 and the method for cube controllable preparation, it is characterised in that plus When hot, heating rate is 3~6 DEG C per minute.
4. magnetic alloy nanosphere body according to claim 2 and the method for cube controllable preparation, it is characterised in that plus When the hot time is 20~35 minutes, magnetic alloy nano-particle is spherical in shape;When heat time is 35~80 minutes, magnetic alloy is received Rice corpuscles is in cubic type.
5. magnetic alloy nanosphere body according to claim 1 and the method for cube controllable preparation, it is characterised in that lazy Property gas be nitrogen or argon gas.
6. magnetic alloy nanosphere body according to claim 1 and the method for cube controllable preparation, it is characterised in that institute The magnetic alloy nano-particles size stated is between 1~20 nanometer.
7. magnetic alloy nanosphere body according to claim 1 and the method for cube controllable preparation, it is characterised in that Fe (acac)3、Mn(acac)2With Zn (acac)2Mol ratio be 4:1:1.
8. magnetic alloy nanosphere body according to claim 1 and the method for cube controllable preparation, it is characterised in that oil Acid, oleyl amine and Fe (acac)3The mol ratio of three is 8:8:(1~2).
CN201710327267.5A 2017-05-10 2017-05-10 A kind of magnetic alloy nanosphere body and the method for cube controllable preparation Pending CN107159901A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108806960A (en) * 2018-04-24 2018-11-13 沈阳工业大学 A kind of liquid phase chemical combination method preparing Nd-Fe-B permanent magnetic nano-particle
CN108856729A (en) * 2018-07-16 2018-11-23 东北大学 The nanometer grain preparation method of the simple substance of Ferrious material or its binary, ternary alloy three-partalloy

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101774027A (en) * 2010-03-15 2010-07-14 北京化工大学 Method for preparing nano-magnetic alloy wave-absorbing material
CN101817088A (en) * 2009-02-27 2010-09-01 天津商业大学 Preparation method of Pt-Ni alloy nano particle and colloidal dispersion system thereof
CN102744419A (en) * 2012-06-20 2012-10-24 中国科学院宁波材料技术与工程研究所 Morphology control method of magnetic nanometer particles
CN103192086A (en) * 2012-01-10 2013-07-10 中国科学院宁波材料技术与工程研究所 Preparation method for controllable duplex metal alloy nano particle
CN103667887A (en) * 2013-12-25 2014-03-26 南京航空航天大学 Preparation method of FeCo alloy absorbing material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101817088A (en) * 2009-02-27 2010-09-01 天津商业大学 Preparation method of Pt-Ni alloy nano particle and colloidal dispersion system thereof
CN101774027A (en) * 2010-03-15 2010-07-14 北京化工大学 Method for preparing nano-magnetic alloy wave-absorbing material
CN103192086A (en) * 2012-01-10 2013-07-10 中国科学院宁波材料技术与工程研究所 Preparation method for controllable duplex metal alloy nano particle
CN102744419A (en) * 2012-06-20 2012-10-24 中国科学院宁波材料技术与工程研究所 Morphology control method of magnetic nanometer particles
CN103667887A (en) * 2013-12-25 2014-03-26 南京航空航天大学 Preparation method of FeCo alloy absorbing material

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108806960A (en) * 2018-04-24 2018-11-13 沈阳工业大学 A kind of liquid phase chemical combination method preparing Nd-Fe-B permanent magnetic nano-particle
CN108806960B (en) * 2018-04-24 2020-07-17 沈阳工业大学 Liquid phase combination method for preparing neodymium iron boron permanent magnetic nano particles
CN108856729A (en) * 2018-07-16 2018-11-23 东北大学 The nanometer grain preparation method of the simple substance of Ferrious material or its binary, ternary alloy three-partalloy

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Application publication date: 20170915