CN103864066A

CN103864066A - Method for preparing graphene, MoS2 or WS2 microspheres

Info

Publication number: CN103864066A
Application number: CN201410093551.7A
Authority: CN
Inventors: 嵇天浩; 马楠; 邹利锋
Original assignee: Individual
Current assignee: Individual
Priority date: 2014-03-14
Filing date: 2014-03-14
Publication date: 2014-06-18

Abstract

The invention discloses a preparation method of graphene microspheres, MoS2 microspheres or WS2 microspheres. The preparation method comprises the following steps of mixing graphene nanosheets, MoS2 nanosheets or WS2 nanosheets with an organic solvent, for example, water, ethanol or a polyhydric alcohol, to form a suspension, next, heating above the boiling point of the solvent, and preserving a constant temperature for a while to obtain the graphene microspheres, the MoS2 microspheres or the WS2 microspheres. The preparation method is simple and environmental friendly, and large-scale production can be realized easily.

Description

One is prepared Graphene, MoS 2or WS 2the method of microballoon

Technical field

The present invention relates to technical field of nano material, particularly relate to Graphene, MoS ₂or WS ₂the preparation method of microballoon.

Background technology

Graphene, MoS ₂or WS ₂nanometer sheet is a kind of two-dimensional nano material, the Graphene, the MoS that are formed by their further self-assemblies ₂or WS ₂microballoon is with a wide range of applications, and will be applied in fields such as catalysis, stored energy and conversion, sensor, matrix material or biomedicines.At present, have about the patent report of being prepared Graphene microballoon by graphene nanometer sheet, but its process complexity, cost is high, is unfavorable for suitability for industrialized production; And for by MoS ₂or WS ₂nanometer sheet direct-assembling forms MoS ₂or WS ₂the preparation process of microballoon have not been reported.

Summary of the invention

In view of this, the object of the invention is to propose a kind of preparation method of microballoon, reduce production costs to reach, the object of large-scale industrial production.

Based on above-mentioned purpose, method for preparing microsphere provided by the invention comprises the following steps:

By Graphene, MoS ₂or WS ₂nanometer sheet suspension liquid carries out liquid phase heating, makes temperature at least more than the boiling point of solvent, processing after for some time, just can make Graphene, MoS ₂or WS ₂microballoon.

Alternatively, nanometer sheet had both dispersibled in water, also dispersibled in the organic solvent such as ethanol or polyvalent alcohol or their mixed solvent.

Alternatively, type of heating can be reflux, can be also to heat in reactor.

Alternatively, Heating temperature is to 100-300 ℃, and keeps 5-45 hour.

As can be seen from above, Graphene provided by the invention, MoS ₂or WS ₂the preparation method of microballoon is by Graphene, MoS ₂or WS ₂nanometer sheet is mixed with water or ethanol, and under reflux conditions or in reactor heats, and single nanometer sheet will occur curling, by nanometer sheet surface interaction, obtains corresponding microballoon.Visible, preparation method's tool provided by the invention has the following advantages: (1) operating process simply, easily control; (2) little to environment and people's hazardness; (3) proper scaleization preparation.

Accompanying drawing explanation

Fig. 1 is X-ray diffraction (XRD) spectrogram, scanning electronic microscope (SEM) photo and transmission electron microscope (TEM) photo of the Graphene microballoon that makes of embodiment 1.

Fig. 2 is the MoS that embodiment 4 makes ₂transmission electron microscope (TEM) photo of microballoon and X-ray diffraction (XRD) spectrogram.

Fig. 3 is the WS that embodiment 10 makes ₂transmission electron microscope (TEM) photo of microballoon and X-ray diffraction (XRD) spectrogram.

Embodiment

For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, the present invention is described in more detail.

Embodiment 1

First at room temperature, the 2.0% Graphene suspension liquid that 100mL is dispersed in diluted hydrochloric acid aqueous solution mixes with 20mL glycerol, then puts into reactor, keeps 20 hours at 200 ℃, and centrifugation after naturally cooling, obtains Graphene microballoon.

Embodiment 2

First at room temperature, the 2.0% Graphene suspension liquid that 100mL is dispersed in diluted hydrochloric acid aqueous solution mixes with the 30mL ethanolic soln that contains a small amount of glycerol, then puts into reactor, keeps 12 hours at 200 ℃, centrifugation after naturally cooling, obtains Graphene microballoon.

Embodiment 3

First at room temperature, the 2.0% Graphene suspension liquid that 100mL is dispersed in diluted hydrochloric acid aqueous solution mixes with 25mL ethylene glycol, then puts into reactor, keeps 20 hours at 180 ℃, and centrifugation after naturally cooling, obtains Graphene microballoon.

Embodiment 4

First the 2.5%MoS at room temperature, 100mL being dispersed in water ₂nanometer sheet suspension liquid mixes with 20mL glycerol, then puts into reactor, keeps 13 hours at 200 ℃, and centrifugation after naturally cooling, obtains MoS ₂microballoon.

Embodiment 5

First the 2.5%MoS at room temperature, 100mL being dispersed in water ₂nanometer sheet suspension liquid mixes with 20mL glycerol, then puts into reactor, keeps 20 hours at 160 ℃, and centrifugation after naturally cooling, obtains MoS ₂microballoon.

Embodiment 6

First the 2.5%MoS at room temperature, 100mL being dispersed in water ₂nanometer sheet suspension liquid mixes with 20mL glycerol, under reflux conditions heats 20 hours, and centrifugation after naturally cooling, obtains MoS ₂microballoon.

Embodiment 7

First the 2.5%MoS at room temperature, 100mL being dispersed in water ₂nanometer sheet suspension liquid mixes with 30mL ethylene glycol, under reflux conditions heats 20 hours, and centrifugation after naturally cooling, obtains MoS ₂microballoon.

Embodiment 8

First the 2.5%MoS at room temperature, 50mL being dispersed in water ₂nanometer sheet suspension liquid mixes with 10mL glycerol, then adds and put into reactor after 50mL ethanol and at 200 ℃, keep 20 hours, and centrifugation after naturally cooling, obtains MoS ₂microballoon.

Embodiment 9

First at room temperature, by the 2.5%WS being dispersed in water ₂nanometer sheet suspension liquid mixes with 20mL glycerol, then puts into reactor, keeps 10 hours at 200 ℃, and centrifugation after naturally cooling, obtains WS ₂microballoon.

Embodiment 10

First at room temperature, by the 2.5%WS being dispersed in water ₂nanometer sheet suspension liquid mixes with 20mL glycerol, then puts into reactor, keeps 18 hours at 150 ℃, and centrifugation after naturally cooling, obtains WS ₂microballoon.

Those of ordinary skill in the field are to be understood that: the foregoing is only specific embodiments of the invention; be not limited to the present invention; all any modifications of making within the spirit and principles in the present invention, be equal to replacement, improvement etc., within protection scope of the present invention all should be included in.

Claims

1. a Graphene, MoS ₂or WS ₂the preparation method of microballoon, is characterized in that, comprises the following steps:

By Graphene, MoS ₂or WS ₂nanometer sheet suspension liquid heats, and makes temperature more than the boiling point of solvent, processing after for some time, just can obtain Graphene, MoS ₂or WS ₂microballoon.

2. method for preparing microsphere according to claim 1, is characterized in that: Graphene, MoS ₂or WS ₂nanometer sheet is to be dispersed in the suspension liquid forming in the organic solvent such as water or ethanol or polyvalent alcohol and their mixed solution.

3. method for preparing microsphere according to claim 1, is characterized in that: under refluxing or heat suspension liquid to 100-300 ℃ in reactor, and keep 5-45 hour.

4. method for preparing microsphere according to claim 1, is characterized in that: Graphene, MoS ₂or WS ₂microballoon is by Graphene, MoS ₂or WS ₂the microballoon that nanometer sheet self-assembly forms.