CN107601439A - A kind of MnTe nano wires and preparation method thereof - Google Patents
A kind of MnTe nano wires and preparation method thereof Download PDFInfo
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- CN107601439A CN107601439A CN201710724655.7A CN201710724655A CN107601439A CN 107601439 A CN107601439 A CN 107601439A CN 201710724655 A CN201710724655 A CN 201710724655A CN 107601439 A CN107601439 A CN 107601439A
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Abstract
The invention provides a kind of MnTe nano wires, the MnTe nano wires that preparation method disclosed by the invention is prepared have good pattern and monodispersity by scanning electron microscope (SEM) photograph observation, and its diameter regulates and controls in 50 200nm, longitudinal length between 2 10 μm；By X-ray diffraction, show that MnTe nano wires prepared by the present invention are hexagonal crystallographic texture, show that antiferromagnetic characteristic is presented in MnTe nano wires by Magnetic Measurement.
Description
Technical field
The present invention relates to antiferromagnetic field of nanometer material technology, and in particular to a kind of preparation method of MnTe nano wires.
Background technology
An important component of the nano wire as nanometer technology, refers to be limited in below 100nm on transversary
One-dimentional structure.Nano wire has the unexistent unique physico-chemical performance of other bulk materials, such as quantum size effect, table
Face effect, macro quanta tunnel effect etc., due to these unique performances so that nano wire optical sensor, temperature sensor,
Had a wide range of applications in rectifier, copying machines, inorganic coating and pressure electric actuator etc..Since particularly 20th century,
The research of nano wire is even more to be rapidly developed, and deepening continuously with nano wire research, and the nano wire of new material is not yet
It is disconnected to emerge in large numbers.For example, the Lieber professors research group of Harvard University is prepared for selenizing molybdenum nano wire, and it is micro- by tunnel
Mirror have studied its structure and characteristic electron (L.Venkataraman, C.M.Lieber.Phys.Rev.Lett., 1999,83
(25):5334-5337)；(the Fe that Yang et al. is developed1-xCox)2P magnetic nanometers, the coercivity in 10K reach
5.74kOe, but the nanowire length is shorter, only 2-4 μm or so, this make its application receive greatly limitation (W.W.Yang,
X.M.Wu,Y.S.Yu,et al.Nancosale,2016,8(36):16187-16191)；Chen et al. passes through in MoS2In mix
Miscellaneous CdS and Cu2-xS forms the MoSe of composite2-CdS、Cu2-xS-MoSe2Nano wire, ensureing CdS and Cu2-xS nanometer chi
Its longitudinal length (J.Z.Chen, X.J.Wu, et al.J.Am.Chem.Soc., 2017,139 (25) is added while very little:
8653-8660)。
With the continuous development of semi-conducting material and storage material, the demand of antiferromagnet is also on the increase.But
It is to concentrate on the research to ferromagnetic nanowires mostly, the research to antiferromagnetic nano wire is less at present to the research of nano wire.And
And pattern and the monodispersity for the antiferromagnetic nano wire prepared at present are nor very well, limiting it in semi-conducting material and depositing
The application of material is stored up, therefore, it is most important to prepare the antiferromagnetic nano wire that pattern is homogeneous, monodispersity is good.
The content of the invention
The invention discloses a kind of MnTe nano wires with good pattern and monodispersity and preparation method thereof.
A kind of preparation method of MnTe nano wires, comprises the following steps：
Solution containing Mn and the suspension containing Te are mixed to get reaction solution, are at the uniform velocity warming up under inert gas shielding
350-400 DEG C of reaction, obtains MnTe nano wires；
Wherein, in the reaction solution, the ratio between Mn and Te amount of material is 1:(0.5-1.8).
Preferably, in described preparation method, the reaction solution is at the uniform velocity warming up to (2-5) DEG C/min heating rate
After 350-400 DEG C, insulation reaction 1-3h.
Preferably, in described preparation method, Te sources are dissolved in tri octyl phosphine, ultrasound obtains described outstanding containing Te
Supernatant liquid；Mn sources are dissolved in oleyl amine, stirred, obtain the solution containing Mn.
Preferably, in described preparation method, the solution containing Mn, 100- is warming up under inert gas shielding
After 120 DEG C, 20-30min is incubated, the suspension containing Te is added to wherein mixing, obtains the reaction solution.
Preferably, in described preparation method, in addition to the step washed and dried to the MnTe nano wires.
Preferably, in described preparation method, the inert gas is nitrogen or argon gas.
Preferably, in described preparation method, the Mn sources are manganese acetylacetonate；The Te sources are tellurium powder.
A kind of MnTe nano wires, its crystal formation are hexagonal crystallographic texture..
Technical solution of the present invention, have the following advantages that：
1. the invention provides a kind of MnTe nano wires, the MnTe being prepared by preparation method disclosed by the invention receives
Rice noodles have good a pattern and monodispersity by scanning electron microscope (SEM) photograph observation, and its diameter is in 50-300nm, and longitudinal length is in 2-
Regulate and control between 10 μm；
By X-ray diffraction, it is hexagonal crystallographic texture to obtain the MnTe nano wires that the present invention is prepared.
2. the invention provides a kind of preparation method of MnTe nano wires, including by the solution containing Mn and the suspension containing Te
Liquid is mixed to get reaction solution, and 350-400 DEG C of reaction is at the uniform velocity warming up under inert gas shielding, obtains MnTe nano wires；Its technique
Simply, it is easy to accomplish, have a good application prospect.
Brief description of the drawings
, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art
The required accompanying drawing used is briefly described in embodiment or description of the prior art, it should be apparent that, in describing below
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before creative work is not paid
Put, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1-3 is the X ray diffracting spectrum of the MnTe nano wires obtained by embodiment 1-3 respectively；
Fig. 4 and 7 is the scanning electron microscope (SEM) photograph of the MnTe nano wires of the gained of embodiment 1 and 3 respectively；
Fig. 5 and 6 is scanning electron microscope (SEM) photograph of the MnTe nano wires of the gained of embodiment 2 under different resolution respectively；
Fig. 8-10 is hysteresis curve figure of the MnTe nano wires in low temperature 5K obtained by embodiment 1-3 respectively.
Embodiment
Technical scheme will be clearly and completely described below, it is clear that described embodiment is this hair
Bright part of the embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not having
There is the every other embodiment made and obtained under the premise of creative work, belong to the scope of protection of the invention.In addition, below
As long as it is mutual not form conflict can each other for involved technical characteristic in described different embodiments of the present invention
With reference to.
Embodiment 1
A kind of MnTe nano wires are present embodiments provided, are obtained by following preparation process：
(1) by 2.8mmol Mn (acac)2Four equipped with thermoregulator and magnetic stirring apparatus are added to 30mL oleyl amines
In mouth flask, 20min is stirred, the solution containing Mn is obtained, in N2100 DEG C are warming up under protection, is incubated 30min；
(2) 1.4mmol Te elemental powders are dissolved in 5mL trioctylphosphine phosphorus (TOP), ultrasonic 30min, obtained containing Te
Aaerosol solution；
(3) aaerosol solution containing Te is expelled in the solution containing Mn, under nitrogen protection with 5 DEG C/min heating
Speed is warming up to 400 DEG C, insulation reaction 1h, closes thermal source, and its product passes through absolute ethyl alcohol and n-hexane centrifuge washing three times, then
MnTe nano wires are can obtain through spontaneously drying.
Embodiment 2
A kind of MnTe nano wires are present embodiments provided, are obtained by following preparation process：
(1) by 2.8mmol Mn (acac)2Four equipped with thermoregulator and magnetic stirring apparatus are added to 30mL oleyl amines
In mouth flask, 30min is stirred, the solution containing Mn is obtained, in N2100 DEG C are warming up under protection, is incubated 20min；
(2) 2.4mmol Te elemental powders are dissolved in 5mL trioctylphosphine phosphorus (TOP), ultrasonic 30min, obtained containing Te
Aaerosol solution；
(3) aaerosol solution containing Te is expelled in the solution containing Mn, under nitrogen protection with 2 DEG C/min heating
Speed is warming up to 400 DEG C, insulation reaction 2h, closes thermal source, and its product passes through absolute ethyl alcohol and n-hexane centrifuge washing three times, then
MnTe nano wires are can obtain through spontaneously drying.
Embodiment 3
A kind of MnTe nano wires are present embodiments provided, are obtained by following preparation process：
(1) by 2.8mmol Mn (acac)2Four equipped with thermoregulator and magnetic stirring apparatus are added to 30mL oleyl amines
In mouth flask, 20min is stirred, the solution containing Mn is obtained, in N2120 DEG C are warming up under protection, is incubated 20min；
(2) 3.6mmol Te elemental powders are dissolved in 5mL trioctylphosphine phosphorus (TOP), ultrasonic 30min, obtained containing Te
Aaerosol solution；
(3) aaerosol solution containing Te is expelled in the solution containing Mn, is first warming up to 120 DEG C under nitrogen protection,
Then 350 DEG C, insulation reaction 3h are at the uniform velocity warming up to 5 DEG C/min heating rate, close thermal source, its product passes through absolute ethyl alcohol
With n-hexane centrifuge washing three times, then through spontaneously drying MnTe nano wires be can obtain.
Compliance test result example
1. structural characterization detects
Structural characterization detection is carried out to the MnTe nano wires prepared by embodiment 1-3 using x-ray diffractometer (XRD).
Fig. 1-3 gives the X ray diffracting spectrum of MnTe nano wires obtained by embodiment 1-3；
The XRD spectrum of MnTe nano wires and MnTe (labels in standard card valut in above-described embodiment：JCPDS18-0814)
Peak shape it is consistent, illustrate prepare MnTe nano wires be hexagonal crystallographic texture；Illustrate that the formation of MnTe nano wires can low, Mn and Te
Different proportion generate MnTe phases.
2. elemental composition and content detection
The elemental composition for the MnTe nano wires that embodiment 1-3 is prepared using energy dispersion X-ray spectrometer (EDX)
And content is tested.
Detected through X-ray energy spectrum：The molar content of Mn elements is 54.38% in the nano wire prepared by embodiment 1,
Te molar content is 45.62%；
The molar content of Mn elements is 50.26%, Te molar content in the nano wire prepared by embodiment 2
For 49.74%；
The molar content of Mn elements is 51.65%, Te molar content in the nano wire prepared by embodiment 3
For 48.35%.
3. morphology characterization detects
The pattern for the MnTe nano wires that embodiment 1-3 is prepared using ESEM (SEM) is tested.
Fig. 4 and 7 sets forth the scanning electron microscope (SEM) photograph of the gained MnTe nano wires of embodiment 1 and 3；It is prepared into embodiment 1
The MnTe nano wires arrived, a diameter of 80-120nm, length are 2-5 μm；The MnTe nano wires being prepared in embodiment 3, diameter
For 100-200nm, length is 3-7 μm；
Fig. 5 and 6 is scanning electron microscope (SEM) photograph of the gained MnTe nano wires of embodiment 2 under different resolution respectively；In embodiment 2
The MnTe nano wires being prepared, a diameter of 50-100nm, length are 8-10 μm；
The average length of MnTe nano wires prepared by embodiment 1-3 is all higher than 5 μm, and diameter is in 100nm or so.
Can also clearly it find out from Fig. 4-7 simultaneously, the thickness by the embodiment 1-3 MnTe nano wires prepared is equal
It is even, there is good pattern and monodispersity.Wherein, the nanowire length of embodiment 2 is more than 10 μm.
4. magnetic detection
Magnetic hysteresis of the MnTe nano wires in 5K prepared by embodiment 1-3 is returned using superconducting quantum interference device (SQUID) (SQUID)
Line is characterized.
Fig. 8-10 sets forth hysteresis curve figures of the nano wire MnTe in low temperature 5K obtained by embodiment 1-3；Pass through magnetic
Hysteresis curves show that MnTe nano wires prepared by embodiment 1-3 show antiferromagnetic behavior.
Obviously, above-described embodiment is only intended to clearly illustrate example, and is not the restriction to embodiment.For
For those of ordinary skill in the art, other various forms of changes or change can also be made on the basis of the above description
It is dynamic.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change or change thus extended out
Among moving still in the protection domain of the invention.
Claims (8)
1. a kind of preparation method of MnTe nano wires, comprises the following steps：
Solution containing Mn and the suspension containing Te are mixed to get reaction solution, 350- is at the uniform velocity warming up under inert gas shielding
400 DEG C of reactions, obtain MnTe nano wires；
Wherein, in the reaction solution, the ratio between Mn and Te amount of material is 1:(0.5-1.8).
2. preparation method as claimed in claim 1, it is characterised in that the reaction solution is with (2-5) DEG C/min heating rate
After being at the uniform velocity warming up to 350-400 DEG C, insulation reaction 1-3h.
3. the preparation method as described in claim any one of 1-2, it is characterised in that Te sources are dissolved in tri octyl phosphine, ultrasound
Obtain the suspension containing Te；Mn sources are dissolved in oleyl amine, stirred, obtain the solution containing Mn.
4. the preparation method as described in claim any one of 1-3, it is characterised in that the solution containing Mn, in indifferent gas
After being warming up to 100-120 DEG C under body protection, 20-30min is incubated, the suspension containing Te is added to wherein mixing, obtained
To the reaction solution.
5. the preparation method as described in claim any one of 1-4, it is characterised in that also include washing the MnTe nano wires
With dry step.
6. the preparation method as described in claim any one of 1-5, it is characterised in that the inert gas is nitrogen or argon gas.
7. the preparation method as described in claim any one of 1-6, it is characterised in that the Mn sources are manganese acetylacetonate；It is described
Te sources are tellurium powder.
8. a kind of MnTe nano wires, it is characterised in that the crystal formation of the MnTe nano wires is hexagonal crystallographic texture.
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| CN104538145A (en) * | 2014-12-08 | 2015-04-22 | 浙江师范大学 | Multi-scale uniform and single-dispersion magnetic microsphere and preparation method thereof |
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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 |
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| WO2010124212A2 (en) * | 2009-04-23 | 2010-10-28 | The University Of Chicago | Materials and methods for the preparation of nanocomposites |
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| CN104787733A (en) * | 2015-04-09 | 2015-07-22 | 复旦大学 | Preparation method of MnTe2 nano-particles |
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