CN104609479A - Method for preparing Co3O4 nanoribbon - Google Patents

Abstract

The invention discloses a method for preparing a Co3O4 nanoribbon. The method comprises the following steps: by taking water as a reaction medium, taking cobalt chloride hexahydrate and urea as raw materials, reacting under water bath conditions, centrifuging and washing the obtained product, and drying, thereby obtaining a controllable ribbon-shaped Co(CO3)0.5(OH).0.11H2O precursor with regular morphology; putting the dried precursor into a muffle furnace, heating to a certain temperature at a certain heating speed, preserving the temperature, and totally converting the precursor into Co3O4, wherein the ribbon structure is not damaged, and the morphology is kept good. The method disclosed by the invention has the advantages that the size, structure and morphology of the Co3O4 nanoribbon prepared by the method are easily controlled, and the prepared Co3O4 nanoribbon has good gas-sensitive and photodegradable performances; and moreover, the preparation method is simple, convenient, easy to operate, low in cost and high in yield, and industrial production is easily realized.

Description

A kind of Co 3o 4the preparation method of nano belt

Technical field

The present invention relates to field of inorganic nano-material preparation, be specifically related to a kind of Co ₃o ₄the preparation method of nano belt.

Background technology

Nano material, particularly monodimension nanometer material show many excellent novel performances relative to its block materials, play an important role, the interest that its study on the synthesis causes scientist increasing in fields such as electronics, photoelectronics and storing devices.Wherein, one dimension transition metal oxide nano-material, gets most of the attention because of its special optics, magnetics and electrology characteristic.

As a kind of important p-type semiconductor, Co ₃o ₄there is spinel structure, be widely used in lithium ion battery, ultracapacitor, information storage, catalysis and sensor numerous areas.In recent years, successively report and multiplely prepare one dimension Co ₃o ₄the method of nano material.Such as: the Co that utilized method of electrostatic spinning to prepare such as Lee ₃o ₄nano wire (Sens. Actuators B, 2012,161,570-577); Takehiko Sasaki etc. are tensio-active agent with palmityl trimethyl ammonium chloride, then add DMF and 30% H ₂o ₂, prepared Co (OH) based on hydrothermal method ₃nano belt, is converted into Co after roasting ₃o ₄nano belt (Nanotechnology, 2010,21,045605); Similar with it, Qiuming Gao etc. add 1,2-PD (Adv. Funct. Mater. 2010,20,617 – 623), and Jianyi Lin etc. add ethylene glycol (ACS Nano, 2010,4,3,1425-1432), through hydro-thermal reaction, roasting presoma, have also been obtained Co ₃o ₄nano belt.These preparation methods or need the equipment of complex and expensive, or with an organic solvent and tensio-active agent, or high-temperature high-voltage reaction.Therefore, low in the urgent need to cost of development, pollution-free, be convenient to industrialized method to prepare Co ₃o ₄nano material.

Summary of the invention

The object of the invention is the deficiency existed for above-mentioned prior art, propose that a kind of technique is simple, easy and simple to handle, morphology controllable, output are high, the Co of constant product quality ₃o ₄the preparation method of nano belt.

Technical scheme of the present invention:

A kind of Co ₃o ₄the preparation method of nano belt, adopt immersion method synthesis, step is as follows:

1) be dissolved in deionized water by cobalt chloride hexahydrate, room temperature lower magnetic force stirs until dissolve completely, then adds urea, and room temperature lower magnetic force stirs and makes it dissolve completely, obtains mixed solution;

2) by above-mentioned mixed solution water-bath 2-48 h at 70-100 DEG C of temperature, reaction solution is obtained;

3) left standstill after 10-120min by above-mentioned reaction soln, centrifugation under 500-10000 r/min rotating speed, reject supernatant liquor, the throw out obtained is used respectively water and absolute ethanol washing 3-6 time, at 60 DEG C of temperature, dry 6-24 h, obtains Co (CO ₃) _0.5(OH) 0.11H ₂o presoma;

4) above-mentioned precursor powder is put into retort furnace, rise to 300-400 DEG C with the temperature rise rate of 2-5 DEG C/min and be incubated 0.5-5 h, obtaining Co ₃o ₄nano belt.

In described mixed solution, cobalt chloride hexahydrate is with Co ²⁺the strength of solution of metering is 0.1-2 mol/L, and urea concentration is 1-20 mol/L.

Advantage of the present invention is: this preparation method's technique is simple, easy to operate, reaction conditions is gentle, with cobalt chloride and urea for reactant, and cheaper starting materials, economic and reliable; The Co of preparation ₃o ₄nano belt is separated easily, purity is higher, Co ₃o ₄nano belt specific surface area is comparatively large, can be widely used as gas sensitive, battery material, photochemical catalysis or support of the catalyst etc.; Co prepared by the present invention ₃o ₄nanostructure contributes to the absorption property of its novelty of development research, catalytic performance, electrical property and air-sensitive performance, significant to exploitation cobalt oxide base novel functional materials.

[accompanying drawing explanation]

Fig. 1 is the Co (CO of preparation ₃) _0.5(OH) 0.11H ₂o presoma and Co ₃o ₄x-ray diffraction (XRD) figure of nano belt.

Fig. 2 is the Co (CO of preparation ₃) _0.5(OH) 0.11H ₂scanning electronic microscope (SEM) photo of O presoma.

Fig. 3 is the Co of preparation ₃o ₄scanning electronic microscope (SEM) photo of nano belt.

[embodiment]

Below by specific embodiment, the present invention is described in further detail.

Embodiment:

A kind of Co ₃o ₄the preparation method of nano belt, adopt immersion method synthesis, step is as follows:

1) be dissolved in the deionized water of 60 mL by 0.01 mol cobalt chloride hexahydrate, room temperature lower magnetic force stirs until dissolve completely, then adds 0.1 mol urea, and room temperature lower magnetic force stirs and makes it dissolve completely, obtains mixed solution;

2) by above-mentioned mixed solution water-bath 24 h at 90 DEG C, reaction solution is obtained;

3) left standstill after 20 min by above-mentioned reaction solution, centrifugal 2 min under 2000 r/min rotating speeds, reject supernatant liquor, the throw out obtained is used respectively water and dehydrated alcohol repeated washing 4 times, at 60 DEG C, dry 12 h, obtain Co (CO ₃) _0.5(OH) 0.11H ₂o presoma;

Fig. 1 is the Co (CO of preparation ₃) _0.5(OH) 0.11H ₂o presoma and Co ₃o ₄xRD figure spectrum (JCPDS card No.48-0083), wherein: be Co (CO in Fig. 1 (a) ₃) _0.5(OH) 0.11H ₂the XRD figure spectrum of O presoma, Fig. 1 (b) obtains sample Co after thermal treatment ₃o ₄xRD figure spectrum, show in figure: Co (CO ₃) _0.5(OH) 0.11H ₂o presoma is converted into Co completely ₃o ₄, all diffraction peaks are all through contrasting with standard spectrogram (JCPDS card No.42-1467), and that coincide is fine.Therefore, can judge that gained sample is as pure Co ₃o ₄.

Fig. 2 is the SEM photo of presoma under different multiples of preparation.Show in figure: presoma presents zonal structure, thickness is about 100 nm, and width is about 200 nm length and is about 6 μm.

By controlling reaction conditions, the regulation and control to presoma pattern and microstructure can also be realized.

4) above-mentioned presoma is put into retort furnace, be warming up to 300 DEG C with the temperature rise rate of 3 DEG C/min and be incubated 30 min, obtaining Co ₃o ₄nano belt.

Fig. 3 is the Co of preparation ₃o ₄the SEM photo of nano belt under different multiples.As can be seen from photo: at Co (CO ₃) _0.5(OH) 0.11H ₂o presoma is to Co ₃o ₄in transition process, structure and morphology remains intact, and be still banded, its thickness is 60-120 nm, and width is 140-280 nm, and length is 4-8 μm.

Detection shows: Co ₃o ₄the air-sensitive performance of nano belt is good, at 300 DEG C, reach 12 to the sensitivity of 100 ppm ethanol.

Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; do not deviate from do under ultimate principle of the present invention and technological process other any change, substitute, simplification etc.; be the displacement of equivalence, all should be included within protection scope of the present invention.

Claims (2)

1. a Co ₃o ₄the preparation method of nano belt, it is characterized in that adopting immersion method synthesis, step is as follows:

1) be dissolved in deionized water by cobalt chloride hexahydrate, room temperature lower magnetic force stirs until dissolve completely, then adds urea, and room temperature lower magnetic force stirs and makes it dissolve completely, obtains mixed solution;

2) by above-mentioned mixed solution water-bath 2-48 h at 70-100 DEG C of temperature, reaction solution is obtained;

3) left standstill after 10-120min by above-mentioned reaction soln, centrifugation under 500-10000 r/min rotating speed, reject supernatant liquor, the throw out obtained is used respectively water and absolute ethanol washing 3-6 time, at 60 DEG C of temperature, dry 6-24 h, obtains Co (CO ₃) _0.5(OH) 0.11H ₂o presoma;

4) above-mentioned precursor powder is put into retort furnace, rise to 300-400 DEG C with the temperature rise rate of 2-5 DEG C/min and be incubated 0.5-5 h, obtaining Co ₃o ₄nano belt.

2. Co according to claim 1 ₃o ₄the preparation method of nano belt, is characterized in that: in described mixed solution, cobalt chloride hexahydrate is with Co ²⁺the strength of solution of metering is 0.1-2 mol/L, and urea concentration is 1-20 mol/L.