CN107601439B - MnTe nanowire and preparation method thereof - Google Patents
MnTe nanowire and preparation method thereof Download PDFInfo
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- CN107601439B CN107601439B CN201710724655.7A CN201710724655A CN107601439B CN 107601439 B CN107601439 B CN 107601439B CN 201710724655 A CN201710724655 A CN 201710724655A CN 107601439 B CN107601439 B CN 107601439B
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Abstract
The invention provides a MnTe nanowire, the MnTe nanowire prepared by the preparation method disclosed by the invention has good appearance and monodispersity through observation of a scanning electron microscope picture, the diameter of the MnTe nanowire is 50-200nm, and the longitudinal length of the MnTe nanowire is regulated and controlled between 2-10 mu m; the MnTe nanowire prepared by the invention is obtained to be of a hexagonal crystal structure through X-ray diffraction, and the MnTe nanowire is shown to have an antiferromagnetic characteristic through magnetic measurement.
Description
Technical Field
The invention relates to the field of antiferromagnetic nano materials, in particular to a preparation method of a MnTe nanowire.
Background
Nanowires, an important component of nanotechnology, refer to one-dimensional structures that are limited to less than 100nm in lateral structure. The nano-wire has unique physical and chemical properties such as quantum size effect, surface effect, macroscopic quantum tunneling effect and the like which are not possessed by other bulk materials, and due to the unique properties, the nano-wire has wide application in light sensors, temperature sensors, rectifiers, photocopiers, inorganic coatings, piezoelectric actuators and the like. Particularly, the research on the nano-wire has been rapidly developed since the 20 th century, and the nano-wire of a new material has been emerged with the continuous and deep research on the nano-wire. For example, molybdenum selenide nanowires were prepared by the professor Lieber research group of harvard university in the united states and their structural and electronic properties were studied by tunneling microscopy (l.venkataraman, c.m.lieber.phys.rev.lett.,1999,83(25): 5334-; developed by Yang et al (Fe)1-xCox)2P magnetic nanowires, which have a coercivity of 5.74kOe at 10K, but are short, only about 2-4 μm in length, have greatly limited applications (W.W.Yang, X.M.Wu, Y.S.Yu, et al.Nancosale,2016,8(36): 16187-; chen et al, by at MoS2Doped with CdS and Cu2-xS forms MoSe of composite material2-CdS、Cu2-xS-MoSe2Nanowire of CdS and Cu2-xThe nano-size of S increases its longitudinal length (J.Z.Chen, X.J.Wu, et al.J.am.chem.Soc.,2017,139(25): 8653-8660).
With the continuous development of semiconductor materials and memory materials, the demand for antiferromagnetic materials has also increased. However, the research on the nanowires is focused on the research on ferromagnetic nanowires, and the research on antiferromagnetic nanowires is less. And the morphology and monodispersity of the prepared antiferromagnetic nanowire are not very good, so that the application of the antiferromagnetic nanowire in semiconductor materials and storage materials is limited, and therefore, the preparation of the antiferromagnetic nanowire with uniform morphology and good monodispersity is very important.
Disclosure of Invention
The invention discloses a MnTe nanowire with good appearance and monodispersity and a preparation method thereof.
A preparation method of MnTe nanowires comprises the following steps:
mixing the Mn-containing solution with the Te-containing suspension to obtain a reaction solution, and heating to 350-400 ℃ at a constant speed under the protection of inert gas to react to obtain a MnTe nanowire;
wherein the mass ratio of Mn to Te in the reaction solution is 1 (0.5-1.8).
Preferably, in the preparation method, the reaction solution is heated to 350-400 ℃ at a constant speed at a heating rate of (2-5) ° c/min, and then is subjected to heat preservation reaction for 1-3 h.
Preferably, in the preparation method, a Te source is dissolved in trioctylphosphine, and the suspension containing Te is obtained by ultrasonic treatment; and dissolving a Mn source in oleylamine, and uniformly stirring to obtain the Mn-containing solution.
Preferably, in the preparation method, after the temperature of the Mn-containing solution is raised to 120 ℃ under the protection of inert gas, the temperature is kept for 20-30min, and the suspension containing Te is added into the solution and mixed to obtain the reaction solution.
Preferably, the preparation method further comprises the steps of washing and drying the MnTe nanowires.
Preferably, in the preparation method, the inert gas is nitrogen or argon.
Preferably, in the preparation method, the Mn source is manganese acetylacetonate; the Te source is tellurium powder.
The crystal form of the MnTe nano wire is a hexagonal crystal structure. .
The technical scheme of the invention has the following advantages:
1. the invention provides a MnTe nanowire, the MnTe nanowire prepared by the preparation method disclosed by the invention has good appearance and monodispersity through observation of a scanning electron microscope picture, the diameter of the MnTe nanowire is 50-300nm, and the longitudinal length of the MnTe nanowire is regulated and controlled between 2-10 mu m;
the MnTe nano-wire prepared by the invention is obtained to be of a hexagonal crystal structure through X-ray diffraction.
2. The invention provides a preparation method of a MnTe nanowire, which comprises the steps of mixing a Mn-containing solution with a Te-containing suspension to obtain a reaction solution, and heating to 350-400 ℃ at a constant speed under the protection of inert gas to react to obtain the MnTe nanowire; the method has the advantages of simple process, easy realization and good application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIGS. 1 to 3 are X-ray diffraction patterns of MnTe nanowires obtained in examples 1 to 3, respectively;
FIGS. 4 and 7 are scanning electron micrographs of MnTe nanowires obtained in examples 1 and 3, respectively;
FIGS. 5 and 6 are SEM images of MnTe nanowires obtained in example 2 at different resolutions, respectively;
FIGS. 8 to 10 are hysteresis curves of the MnTe nanowires obtained in examples 1 to 3 at a low temperature of 5K, respectively.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
The embodiment provides a MnTe nanowire, which is obtained by the following preparation steps:
(1) 2.8mmol of Mn (acac)2And 30mL oleylamine were added to a four-necked flask equipped with a temperature regulator and a magnetic stirrer, and stirred for 20min to obtain a Mn-containing solution in N2Heating to 100 deg.C under protection, and keeping the temperature for 30 min;
(2) dissolving 1.4mmol of Te simple substance powder in 5mL of Trioctylphosphine (TOP), and performing ultrasonic treatment for 30min to obtain a suspension solution containing Te;
(3) injecting the suspension solution containing Te into the solution containing Mn, heating to 400 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen, carrying out heat preservation reaction for 1h, turning off a heat source, carrying out centrifugal washing on the product of the reaction for three times by using anhydrous ethanol and n-hexane, and naturally drying to obtain the MnTe nanowire.
Example 2
The embodiment provides a MnTe nanowire, which is obtained by the following preparation steps:
(1) 2.8mmol of Mn (acac)2And 30mL oleylamine were added to a four-necked flask equipped with a temperature regulator and a magnetic stirrer, and stirred for 30min to obtain a Mn-containing solution in N2Heating to 100 deg.C under protection, and maintaining the temperature for 20 min;
(2) dissolving 2.4mmol of Te simple substance powder in 5mL of Trioctylphosphine (TOP), and performing ultrasonic treatment for 30min to obtain a suspension solution containing Te;
(3) injecting the suspension solution containing Te into the solution containing Mn, heating to 400 ℃ at the heating rate of 2 ℃/min under the protection of nitrogen, carrying out heat preservation reaction for 2h, turning off a heat source, carrying out centrifugal washing on the product of the reaction for three times by using anhydrous ethanol and n-hexane, and naturally drying to obtain the MnTe nanowire.
Example 3
The embodiment provides a MnTe nanowire, which is obtained by the following preparation steps:
(1) 2.8mmol of Mn (acac)2And 30mL oleylamine were added to a four-necked flask equipped with a temperature regulator and a magnetic stirrer, and stirred for 20min to obtain a Mn-containing solution in N2Heating to 120 deg.C under protection, and maintaining the temperature for 20 min;
(2) dissolving 3.6mmol of Te simple substance powder in 5mL of Trioctylphosphine (TOP), and performing ultrasonic treatment for 30min to obtain a suspension solution containing Te;
(3) injecting the suspension solution containing Te into the solution containing Mn, heating to 120 ℃ under the protection of nitrogen, then heating to 350 ℃ at a constant speed at a heating rate of 5 ℃/min, carrying out heat preservation reaction for 3h, turning off a heat source, carrying out centrifugal washing on the product three times by using anhydrous ethanol and n-hexane, and naturally drying to obtain the MnTe nanowire.
Example of Effect verification
1. Structural characterization detection
The MnTe nanowires prepared in examples 1 to 3 were subjected to structural characterization and detection by means of an X-ray diffractometer (XRD).
FIGS. 1 to 3 show X-ray diffraction patterns of MnTe nanowires obtained in examples 1 to 3;
the XRD pattern of the MnTe nanowire in the embodiment is consistent with the peak shape of MnTe (label: JCPDS18-0814) in a standard card library, which indicates that the prepared MnTe nanowire has a hexagonal crystal structure; the formation energy of the MnTe nano-wire is low, and MnTe phases are generated by different proportions of Mn and Te.
2. Detection of element composition and content
The elemental compositions and contents of the MnTe nanowires prepared in examples 1 to 3 were measured by an energy dispersive X-ray spectrometer (EDX).
And (3) detecting by an X-ray energy spectrum: the nanowire prepared in example 1 had a Mn element content of 54.38 mol% and a Te content of 45.62 mol%;
the nanowires prepared in example 2 had a Mn element content of 50.26 mol% and a Te content of 49.74 mol%;
the nanowires prepared in example 3 had a Mn element content of 51.65 mol% and a Te content of 48.35 mol%.
3. Topography characterization detection
The morphology of the MnTe nanowires prepared in examples 1-3 was tested using a Scanning Electron Microscope (SEM).
FIGS. 4 and 7 show scanning electron micrographs of MnTe nanowires obtained in examples 1 and 3, respectively; the MnTe nanowire prepared in the embodiment 1 has a diameter of 80-120nm and a length of 2-5 μm; the MnTe nanowire prepared in the embodiment 3 has a diameter of 100-200nm and a length of 3-7 μm;
FIGS. 5 and 6 are SEM images of MnTe nanowires obtained in example 2 at different resolutions, respectively; the MnTe nanowire prepared in the embodiment 2 has a diameter of 50-100nm and a length of 8-10 μm;
the MnTe nanowires prepared in examples 1 to 3 each had an average length of more than 5 μm and a diameter of about 100 nm.
Meanwhile, as is clear from fig. 4 to 7, the MnTe nanowires prepared in examples 1 to 3 have uniform thickness, good morphology and monodispersity. Wherein the nanowire length of example 2 exceeds 10 μm.
4. Magnetic detection
The hysteresis loops at 5K of the MnTe nanowires prepared in examples 1-3 were characterized using a superconducting quantum interferometer (SQUID).
FIGS. 8 to 10 respectively show the magnetic hysteresis curves of the MnTe nanowires obtained in examples 1 to 3 at a low temperature of 5K; as can be seen from the hysteresis loop, the MnTe nanowires prepared in examples 1-3 show antiferromagnetic behavior.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (4)
1. A preparation method of MnTe nanowires comprises the following steps:
dissolving a Te source in trioctylphosphine, and performing ultrasonic treatment to obtain a suspension containing Te; dissolving a Mn source in oleylamine, stirring uniformly to obtain a Mn-containing solution, heating the Mn-containing solution to 120 ℃ under the protection of inert gas, preserving heat for 20-30min, adding the suspension containing Te into the solution, mixing to obtain a reaction solution, uniformly heating the reaction solution to 400 ℃ under the protection of inert gas at a heating rate of (2-5) DEG C/min, and preserving heat for reaction for 1-3h to obtain a MnTe nanowire;
wherein the mass ratio of Mn to Te in the reaction solution is 1 (0.5-1.8).
2. The method of claim 1, further comprising the step of washing and drying the MnTe nanowires.
3. The method according to claim 1 or 2, wherein the inert gas is nitrogen or argon.
4. The method of claim 1, wherein the Mn source is manganese acetylacetonate; the Te source is tellurium powder.
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| EP1855336A1 (en) * | 2006-05-12 | 2007-11-14 | Samsung SDI Co., Ltd. | Catalyst, method for preparing the same, and membrane-electrode assembly and fuel cell system including the same |
| CN101132028A (en) * | 2006-08-25 | 2008-02-27 | 通用电气公司 | Single conformal junction nanowire photovoltaic devices |
| WO2010124212A2 (en) * | 2009-04-23 | 2010-10-28 | The University Of Chicago | Materials and methods for the preparation of nanocomposites |
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| CN104538145B (en) * | 2014-12-08 | 2017-02-22 | 浙江师范大学 | Multi-scale uniform and single-dispersion magnetic microsphere and preparation method thereof |
| CN104787733B (en) * | 2015-04-09 | 2017-01-18 | 复旦大学 | Preparation method of MnTe2 nano-particles |
| DE102015218560A1 (en) * | 2015-09-28 | 2017-03-30 | Robert Bosch Gmbh | Hard magnetic phase, process for its preparation and magnetic material |
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| EP1855336A1 (en) * | 2006-05-12 | 2007-11-14 | Samsung SDI Co., Ltd. | Catalyst, method for preparing the same, and membrane-electrode assembly and fuel cell system including the same |
| CN101132028A (en) * | 2006-08-25 | 2008-02-27 | 通用电气公司 | Single conformal junction nanowire photovoltaic devices |
| WO2010124212A2 (en) * | 2009-04-23 | 2010-10-28 | The University Of Chicago | Materials and methods for the preparation of nanocomposites |
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