CN111792669B - TiO 22Nano-rod/multilayer graphene composite material and preparation method thereof - Google Patents
TiO 22Nano-rod/multilayer graphene composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a TiO 22The nano-rod/multilayer graphene composite material takes multilayer graphene as a carbon substrate, and TiO is uniformly distributed on the surface of the composite material2A nanorod; TiO 22The diameter of the nanorod is less than 100 nanometers, the length of the nanorod is less than 500nm, and the length-diameter ratio of the nanorod is about 3-7. The nano rods are uniformly distributed on the surface of the multilayer graphene, and a part of the nano rods are overlapped, so that larger pores are formed among the nano rods. The preparation process of the composite material comprises the following steps: 1. adding expanded graphite into a mixed solution of DMF and distilled water, and ultrasonically treating to obtain a multilayer graphene sheet; 2. adding titanium powder, concentrated hydrochloric acid and alkene nitric acid solution into multilayer graphene; 3. and putting the mixed solution into a water bath kettle at the temperature of 90 ℃ for magnetic stirring reaction for a certain hour. 4. And washing the reaction product with deionized water and alcohol, and drying to obtain the final composite material. TiO prepared by the method2The nanorod/multilayer graphene composite material has potential application in the fields of lithium ion battery cathode materials, lithium sulfur battery anode materials, photocatalysis and the like.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to TiO2A nano-rod/multi-layer graphene composite material and a preparation method thereof. The prepared material has potential application in the fields of lithium ion battery cathode materials, lithium sulfur battery anode materials, photocatalysis and the like.
Background
The titanium dioxide material has wide application in the fields of pigments, catalyst carriers, photocatalysis, lithium ion batteries, lithium sulfur batteries and the like. The nano-scale titanium dioxide has more excellent performance due to size effect, quantum effect and the like. The nanometer titanium dioxide is easy to agglomerate and the nanometer titanium dioxide has poor self-conductivity. Therefore, in application as an electrode material, nano titanium dioxide is often compounded with a conductive material such as a carbon material. At present, the most studied is the compounding of nano titanium oxide and graphene and the study of various properties.
However, graphene and nanodioxos are currently availableThe titanium composite material has the following characteristics in preparation technology. 1. The titanium source is mainly TiCl4And titanium organic compounds such as butyl titanate. These titanium sources are very susceptible to hydrolysis due to hydrolysis to TiO2Too fast, the titanium dioxide produced is prone to agglomeration. Therefore, the concentration of the titanium precursor in the solution cannot be too high, resulting in low distribution density of the nano titanium dioxide on the surface of the graphene. 2. At present, the composite material is prepared mainly by a hydrothermal method or a microwave heating method. These methods are not suitable for large-scale production. 3. The preparation on the surface of graphene is mainly nano-particles. Few reports are related to the preparation of nanorods on the surface of multilayer graphene. The nanorod is easy to form a three-dimensional porous structure on the surface of graphene, and can improve the excellent electrochemical performance of the arch material.
In view of the deficiencies of the prior art, a technical solution is needed to solve the technical problems in the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides TiO2The nano-rod/multilayer graphene composite material is prepared by adopting titanium powder as a titanium source, stirring and reacting in water bath and preparing TiO by a one-step method2The nano-rod/multilayer graphene composite material has simple preparation process and is beneficial to industrial preparation.
In order to solve the technical problems in the prior art, the invention discloses TiO2Nanorod/multilayer graphene composite, TiO2The crystallized nano rods are in the shape and are uniformly distributed on the surface of the multilayer graphene, and part of the nano rods are overlapped to form pores; wherein, TiO2The nano rod and the multilayer graphene are combined by molecular force, and TiO2The crystal is rutile TiO2The length-diameter ratio of the nanorod is 3-7, the diameter of the nanorod is less than 100nm, and the length of the nanorod is less than 500 nm; the number of the layers of the multilayer graphene is less than 100.
The invention also discloses the TiO2The preparation method of the nanorod/multilayer graphene composite material comprises the following steps:
step S10, measuring DMF and deionized water in a volume ratio of 4:1, and uniformly mixing the DMF and the deionized water to obtain a mixed solvent A;
step S20, weighing a certain amount of expanded graphite, adding the expanded graphite into the mixed solvent A, and performing ultrasonic treatment for 5 hours to obtain a multilayer graphene dispersion liquid, wherein the concentration of the expanded graphite relative to the solvent A is 2-4 mg/mL;
step S30, measuring nitric acid and deionized water to prepare a dilute nitric acid solution of 2mol/L, which is called as a B solution;
step S40, weighing titanium powder and adding the titanium powder into the graphene dispersion liquid, wherein the particle size of the titanium powder is 10-50 microns; measuring hydrochloric acid with the concentration of 36% and a solution B, and adding the hydrochloric acid and the solution B into the graphene dispersion liquid; then putting the mixture into a water bath at 90 ℃ for magnetic stirring reaction for 36-60 hours, wherein the magnetic stirring speed is 300 revolutions per minute; the concentration of the titanium powder relative to the solution A is 4-6 mg/mL, the volume ratio of the hydrochloric acid to the solution A is 1.2: 1-1.4: 1, and the volume ratio of the solution B to the solution A is 0.02: 1-0.03: 1.
Step S50, after cooling, collecting black products through centrifugal cleaning, wherein the centrifugal cleaning adopts 3 times of deionized water and 3 times of alcohol centrifugal cleaning, and the speed of a centrifugal machine is 6000 r/min; drying the mixture in an oven at 70 ℃ for 24 hours to obtain the TiO of the invention2A nanorod/multilayer graphene composite.
The technical scheme is realized based on the combined action of hydrochloric acid, nitric acid and DMF. The main purpose of the hydrochloric acid with higher concentration is to dissolve metal titanium powder, and the titanium powder is gradually dissolved into Ti under the action of the hydrochloric acid3+Ions. In the absence of alkene nitric acid, contains Ti3+The purple solution of (A) remains and is not further oxidized to Ti4+. And the dilute nitric acid can be added to react with Ti3+Further oxidized to Ti4+. The function of DMF is to react with Ti4+Form a complex with Ti4+The formed complex is adsorbed by the multilayer graphene by the action of molecular force, and then hydrolysis is generated to form titanium dioxide. Due to the slow rate of titanium dioxide formation, the subsequently produced titanium dioxide preferentially grows on the surface of the titanium dioxide nanocrystal formed first, thus forming a rod shape.
Compared with the prior art, the invention has the following characteristics:
(1) the metal titanium powder is used as a raw material, and titanium does not need to be prepared into organic titanium salt, so that the cost is saved. The metal titanium is used as a titanium source, and the dissolution and deposition speed of titanium dioxide can be controlled through the acid concentration, so that the nano rod is prepared.
(2) According to the preparation method, the surface of the multilayer graphene does not need to be subjected to activation treatment, and titanium dioxide is deposited under the action of molecular force, so that the distribution of the titanium dioxide on the surface of the multilayer graphene is more uniform.
(3) The titanium dioxide nanorods prepared by the method are uniformly distributed on the surface of the multilayer graphene, and a part of the nanorods are overlapped, so that larger pores are formed among the nanorods.
(4) The invention adopts water bath stirring reaction and one-step preparation process, has low preparation temperature and simple preparation equipment, and is beneficial to industrial preparation.
(5) The composite material takes multilayer graphene as a carbon material substrate. The multilayer graphene is prepared by a simple ultrasonic method, and the preparation cost is lower than that of single-layer graphene and graphene oxide. The multilayer graphene also has good conductivity, large specific surface area and strong TiO loading2The capacity of the nano-rod.
Drawings
FIG. 1 shows TiO of example 1 of the present invention2A flow chart of the steps of the method for preparing the nanorod/multilayer graphene composite material;
FIG. 2 shows TiO of example 2 of the present invention2XRD pattern of nanorod/multilayer graphene composite;
FIG. 3 shows TiO of example 2 of the present invention2A low-power scanning electron microscope image of the nanorod/multilayer graphene composite material;
FIG. 4 shows TiO of example 2 of the present invention2A high-power scanning electron microscope image of the nanorod/multilayer graphene composite material;
Detailed Description
The technical solution provided by the present invention will be further explained with reference to the accompanying drawings.
Referring to FIG. 1, there is shown TiO of the present invention2Process for preparing nano-rod/multi-layer graphene composite materialA block diagram comprising the steps of:
step S10, measuring DMF and deionized water in a volume ratio of 4:1, and uniformly mixing the DMF and the deionized water to obtain a mixed solvent A;
step S20, weighing a certain amount of expanded graphite, adding the expanded graphite into the mixed solvent A, and performing ultrasonic treatment for 5 hours to obtain a multilayer graphene dispersion liquid, wherein the concentration of the expanded graphite relative to the solvent A is 2-4 mg/mL;
step S30, measuring nitric acid and deionized water to prepare a dilute nitric acid solution of 2mol/L, which is called as a B solution;
step S40, weighing titanium powder and adding the titanium powder into the graphene dispersion liquid, wherein the particle size of the titanium powder is 10-50 microns; measuring hydrochloric acid with the concentration of 36% and a solution B, and adding the hydrochloric acid and the solution B into the graphene dispersion liquid; then putting the mixture into a water bath at 90 ℃ for magnetic stirring reaction for 36-60 hours, wherein the magnetic stirring speed is 300 revolutions per minute; the concentration of the titanium powder relative to the solution A is 4-6 mg/mL, the volume ratio of the hydrochloric acid to the solution A is 1.2: 1-1.4: 1, and the volume ratio of the solution B to the solution A is 0.02: 1-0.03: 1.
Step S50, after cooling, collecting black products through centrifugal cleaning, wherein the centrifugal cleaning adopts 3 times of deionized water and 3 times of alcohol centrifugal cleaning, and the speed of a centrifugal machine is 6000 r/min; drying the mixture in an oven at 70 ℃ for 24 hours to obtain the TiO of the invention2A nanorod/multilayer graphene composite.
TiO prepared by the above method2Nanorod/multilayer graphene composite, TiO2The crystallized nano rods are in the shape and are uniformly distributed on the surface of the multilayer graphene, and part of the nano rods are overlapped to form pores; wherein, TiO2The nano rod and the multilayer graphene are combined by molecular force, and TiO2The crystal is rutile-shaped TiO2The length-diameter ratio of the nanorod is 3-7, the diameter of the nanorod is less than 100nm, and the length of the nanorod is less than 500 nm; the number of the layers of the multilayer graphene is less than 100.
The preparation process and experimental results of the present invention are further described below by way of examples.
Instantiation 1
4ml DMF and 1ml distilled water are mixed evenly as a mixed solvent, and 10mg of swelling stone is weighedAdding the ink into a mixed solvent, and after ultrasonic oscillation is carried out for 5 hours, stripping the expanded graphite into multilayer graphene which is uniformly dispersed in the solvent, thereby obtaining the multilayer graphene dispersion liquid. To the multilayer graphene dispersion, 20mg of titanium powder and 6ml of concentrated hydrochloric acid (36%) and 150ul of dilute nitric acid with a concentration of 2mol/L were added. Then stirred in a water bath at 90 ℃ and 300 rpm for 36 hours. Cooling, centrifugally cleaning to collect black product, centrifugally cleaning with deionized water for 3 times and alcohol for 3 times, drying in an oven at 70 deg.C for 24 hr to obtain nanometer TiO powder2A nanorod/multilayer graphene composite.
Uniformly mixing 4ml of DMF (dimethyl formamide) and 1ml of distilled water to obtain a mixed solvent A, weighing 15mg of expanded graphite, adding the expanded graphite into the mixed solvent A, and carrying out ultrasonic oscillation for 5 hours to ensure that the expanded graphite is stripped into multilayer graphene which is uniformly dispersed in the solvent, thereby obtaining the multilayer graphene dispersion liquid. 23mg of titanium powder and 6ml of concentrated hydrochloric acid (36%) and 120ul of dilute nitric acid with a concentration of 2mol/L were added to the multilayer graphene dispersion. Then stirred in a water bath at 90 ℃ and 300 rpm for 48 hours. Cooling, centrifugally cleaning to collect black product, centrifugally cleaning with deionized water for 3 times and alcohol for 3 times, drying at 70 deg.C for 24 hr in oven, and drying to obtain nanometer TiO2A rod/multilayer graphene composite.
Instantiation 3
Uniformly mixing 4ml of DMF (dimethyl formamide) and 1ml of distilled water to obtain a mixed solvent A, weighing 20mg of expanded graphite, adding the expanded graphite into the mixed solvent A, and carrying out ultrasonic oscillation for 5 hours to ensure that the expanded graphite is stripped into multilayer graphene which is uniformly dispersed in the solvent, thereby obtaining the multilayer graphene dispersion liquid. 30mg of titanium powder and 7ml of concentrated hydrochloric acid (36%) and 150ul of dilute nitric acid with a concentration of 2mol/L were added to the multilayer graphene dispersion. Then stirred in a water bath at 90 ℃ and 300 rpm for 60 hours. Cooling, centrifugally cleaning to collect black product, centrifugally cleaning with deionized water for 3 times and alcohol for 3 times, drying at 70 deg.C for 24 hr in oven, and drying to obtain nanometer TiO2A rod/multilayer graphene composite.
Instantiation 4
Uniformly mixing 4ml of DMF (dimethyl formamide) and 1ml of distilled water to obtain a mixed solvent A, weighing 17mg of expanded graphite, adding the expanded graphite into the mixed solvent A, and carrying out ultrasonic oscillation for 5 hours to ensure that the expanded graphite is stripped into multilayer graphene which is uniformly dispersed in the solvent, thereby obtaining the multilayer graphene dispersion liquid. 25mg of titanium powder and 6.5ml of concentrated hydrochloric acid (36%) and 130ul of dilute nitric acid with a concentration of 2mol/L were added to the multilayer graphene dispersion. Then stirred in a water bath at 90 ℃ and 300 rpm for 50 hours. Cooling, centrifugally cleaning to collect black product, centrifugally cleaning with deionized water for 3 times and alcohol for 3 times, drying at 70 deg.C for 24 hr in oven, and drying to obtain nanometer TiO2A rod/multilayer graphene composite.
XRD detection is carried out on the composite material prepared in example 1, and as shown in figure 2, multilayer graphene and TiO can be seen from the figure2The diffraction peak of (1). TiO 22Has a broad diffraction peak, indicating that TiO2The rod of (a) is small. No other phases were found, indicating that the phases obtained were very pure.
The composite material prepared in example 1 was subjected to SEM observation, and fig. 3 is a low power electron microscope image thereof, and fig. 4 is a high power electron microscope image thereof. TiO can be observed by low-power SEM picture2The nanorods are very uniformly distributed on the surface of the multilayer graphene. TiO can be observed by high-power SEM picture2The nanorod has the diameter less than 100 nanometers, the length less than 500nm and the length-diameter ratio of about 3-7. The nano rods are uniformly distributed on the surface of the multilayer graphene, and a part of the nano rods are overlapped, so that larger pores are formed among the nano rods.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. TiO 22The nano-rod/multi-layer graphene composite material is characterized in that TiO2The crystallized nano rods are in the shape and are uniformly distributed on the surface of the multilayer graphene, and part of the nano rods are overlapped to form pores; wherein, TiO2The nano rod and the multilayer graphene are combined by molecular force, and TiO2The crystal is rutile TiO2The length-diameter ratio of the nanorod is 3-7, the diameter of the nanorod is less than 100nm, and the length of the nanorod is less than 500 nm;
the composite material is prepared by taking titanium powder as a titanium source through a one-step method of water bath stirring reaction, and the preparation method comprises the following steps:
step S10, measuring DMF and deionized water in a volume ratio of 4:1, and uniformly mixing the DMF and the deionized water to obtain a mixed solvent A;
step S20, weighing a certain amount of expanded graphite, adding the weighed expanded graphite into a mixed solvent A, and obtaining a multilayer graphene dispersion liquid through ultrasound, wherein the concentration of the expanded graphite relative to the solvent A is 2-4 mg/mL;
step S30, measuring nitric acid and deionized water to prepare a dilute nitric acid solution of 2mol/L, which is called as a B solution;
step S40, weighing titanium powder and adding the titanium powder into the graphene dispersion liquid, wherein the particle size of the titanium powder is 10-50 microns; measuring hydrochloric acid with the concentration of 36% and a solution B, and adding the hydrochloric acid and the solution B into the graphene dispersion liquid; then putting the mixture into a water bath with the temperature of 90 ℃ for stirring reaction for 36-60 hours, wherein the stirring speed is 300 r/min; wherein the concentration of the titanium powder relative to the solution A is 4-6 mg/mL, the volume ratio of the hydrochloric acid to the solution A is 1.2: 1-1.4: 1, and the volume ratio of the solution B to the solution A is 0.02: 1-0.03: 1;
step S50, cooling, centrifugally cleaning, collecting reaction products, centrifugally cleaning, and drying to obtain TiO2A nanorod/multilayer graphene composite.
2. The TiO of claim 12The nanorod/multilayer graphene composite material is characterized in that the number of the multilayer graphene layers is less than 100.
3. The TiO of claim 12The nanorod/multilayer graphene composite material is characterized in that in step S40, titanium powder is gradually dissolved into Ti under the action of hydrochloric acid3+Ionic, dilute nitric acid to Ti3+Further oxidized to Ti4+DMF and Ti4+Forming a complex, adsorbing the complex by the multilayer graphene through the action of molecular force, and then hydrolyzing to form titanium dioxide; the forming speed of the titanium dioxide is controlled by water bath stirring, so that the subsequently generated titanium dioxide preferentially grows on the surface of the titanium dioxide nanocrystal which is firstly formed to form a rod shape.
4. The TiO of claim 12The nanorod/multilayer graphene composite material is characterized in that a reaction product is centrifugally cleaned and then placed in an oven to be dried for 24 hours at 70 ℃.
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