A method for the controllable preparation of cobalt/cobalt oxide nanofilms using an ionic liquid water interface

A technology of ionic liquids and nano-membranes, applied in the field of nano-materials, can solve the problems of no large-scale application of nano-membranes, the inability of independent existence of thin films, poor energy conservation and environmental protection, and achieve excellent Co redox and catalytic hydrogenation performance, Avoid the use of complex organic stabilizers, the effect of mild reaction conditions

Inactive Publication Date: 2016-03-30
HENAN POLYTECHNIC UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Compared with the conventional techniques for preparing thin films by chemical methods, such as electrodeposition technology and liquid phase reduction method, electrodeposition technology can achieve the deposition of nanostructured films with different shapes, but the electrodeposition process relies on the deposition of metal atoms onto conductive substrates , the thin film cannot exist independently, and the conventional electrodeposition technology cannot realize the control of the nano-film structure (such as conventional aqueous solution electroplating), which requires high deposition conditions. In addition, the deposition process consumes a lot of power, which is poor in energy saving and environmental protection; conventional liquid phase reduction technology (such as Polyol method, protective agent method, etc.) are commonly used methods to prepare metal nanoparticles, but there is no soft template controlled by the two-dimensional membrane structure in the solution, and the membrane structure cannot be realized.
In the prior art, there is no related description and large-scale application method for preparing nano-membrane by using ionic liquid water interface

Method used

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  • A method for the controllable preparation of cobalt/cobalt oxide nanofilms using an ionic liquid water interface
  • A method for the controllable preparation of cobalt/cobalt oxide nanofilms using an ionic liquid water interface

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Experimental program
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Effect test

Embodiment 1

[0026] Embodiment 1: a kind of method that utilizes ionic liquid water interface to controllably prepare cobalt / cobalt oxide nano film, concrete steps are: put 6.00g ionic liquid (1 methyl-3 octylimidazolium salt hexafluorophosphoric acid [C 8 min]PF 6 , dosage can be adjusted) and KBH 4 (0.15mol / L, 20mL) aqueous solution was mixed in a three-necked flask and ultrasonically dispersed to form an ultra-fine dispersed microemulsion structure; then, under the conditions of Ar gas saturation, reflux and liquid seal, magnetic stirring and heating at 60 ° C as A solution; make cobalt acetate into a (30mmol / L, 20mL) aqueous solution as solution B; add solution B to solution A dropwise at a rate of 2 drops per second through a constant pressure funnel. Then, under the condition of magnetic stirring, the reaction was performed at a constant temperature of 60°C for 1 hour until a black colloidal solution was formed. The reaction flask was cooled to room temperature and allowed to stand...

Embodiment 2

[0027] Example 2: The ionic liquid in Example 1 is replaced by 1,3-dioctyl imidazolium hexafluorophosphate [OOIM]PF 6 , others are the same as in Example 1, the result is as figure 2 . figure 2 Shown in [OOIM]PF 6 Transmission electron microscopy (TEM) images of Co nanofilms synthesized on ionic liquid water interfaces with a scale of 500nm; TEM images show that Co nanofilms synthesized on different ionic liquid water interfaces can achieve structural adjustment, and cobalt / cobalt oxide forms a clean The nano film has a thickness of 1-2nm and curls into a tubular structure at the edge of the film. By changing the different substituents on the imidazole ring, changing the template properties on the interface and the adsorption of ionic liquids on the metal surface, the controllable preparation of Co metal nanofilms is achieved. Infrared spectroscopy was performed on pure ionic liquids, supernatants, liquid cobalt / cobalt oxide colloids, and centrifuged dried solids, showing...

Embodiment 3

[0029] Embodiment 3: Adjust the reaction temperature in Embodiment 1 and Embodiment 2 within the range of 60-100° C., and the others are the same as Scheme 1. Temperature has a great influence on the control of nanostructures. If the reaction temperature is too low, the reaction will not be complete; if the temperature is too high, the reaction speed will be too fast, the metal nucleation speed will be too fast, and the Co film structure will not form stably. The reaction temperature is controlled at 60-100°C, and the Co film structure can be adjusted by changing the reaction temperature. For example, the reaction temperature is 70°C for one hour at a constant temperature, and KBH is added 4 After that, the Co nucleation speed is accelerated, and the film formation time is shortened, but the area and integrity of the film will be reduced, and the nano-film can still be formed at a reaction temperature of 100 °C;

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Abstract

Disclosed is a method for utilizing controllability of an ionic liquid water interface to prepare a cobalt / cobalt oxide nanofilm. The method includes that KBH4 is utilized as a reducing agent, a transition metal cobalt / cobalt oxide nanofilm structure material is realized on the insoluble ionic liquid water interface, and water-insoluble imidazolyl cations and weak-coordination composite anions like PF-6 are selected for ionic liquid; infrared spectrometry is performed on pure ionic liquid, supernate, liquid cobalt / cobalt oxide colloid and centrifugally-dried solid, and preparation of a completely-clean cobalt / cobalt oxide nanofilm is realized if the ionic liquid is not adsorbed on the surface of cobalt / cobalt oxide before and after centrifugation. By the method, control on nanofilm structure can be realized by changing substituent groups on an imidazole ring and cations. Preparation of a clean and controllable cobalt / cobalt oxide nanofilm is realized on the ionic liquid water interface on the basis of selective weak adsorption effect and template effect of the ionic liquid on the metal surface.

Description

technical field [0001] The invention relates to the technical field of nanometer materials, in particular to a method for controllably preparing a cobalt / cobalt oxide nanofilm by using an ionic liquid water interface. Background technique [0002] Due to their unique physical and chemical properties, nanostructured materials show potential application prospects in scientific research and industrial applications. The controllable and continuous preparation of nanostructured materials through appropriate design is still a research hotspot in various fields. 80% of cobalt output is used to produce various alloys, which have better properties in terms of magnetism, hardness, heat resistance, wear resistance and corrosion resistance; the artificial radioactive isotope cobalt 60 can replace X-rays and is also used to treat cancer ; Cobalt compounds are used in medicine, pigments, driers, catalysts and ceramic glazes, such as vitamin B 12 It is a cobalt compound. Metal cobalt is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24B22F1/00C30B29/02C30B27/00C30B33/02B82Y40/00
Inventor 陈玉梅时建朝张利伟张大峰杨娟陈萌
Owner HENAN POLYTECHNIC UNIV
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