CN110624572A - Flaky semimetal MoTe2And flaky semi-metal MoTe2Preparation method of/RGO - Google Patents

Flaky semimetal MoTe2And flaky semi-metal MoTe2Preparation method of/RGO Download PDF

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CN110624572A
CN110624572A CN201910934298.6A CN201910934298A CN110624572A CN 110624572 A CN110624572 A CN 110624572A CN 201910934298 A CN201910934298 A CN 201910934298A CN 110624572 A CN110624572 A CN 110624572A
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贺海燕
贺祯
沈清
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Shaanxi University of Science and Technology
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    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
    • C25B1/01Products
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    • C25B1/04Hydrogen or oxygen by electrolysis of water
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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    • C25B11/051Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/091Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/36Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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Abstract

The invention discloses a flaky semi-metal MoTe2And flaky semi-metal MoTe2The preparation method of/RGO comprises adding tellurium powder and potassium borohydride into deionized water, and reacting in sealed environment to obtain Te2‑A precursor aqueous solution; dissolving ammonium paramolybdate in a solvent, and adding citric acid to obtain a precursor solution of a molybdenum ion source; mixing Te2‑Placing the precursor aqueous solution and the molybdenum ion source precursor solution into a reaction kettle, keeping the solution at room temperature, performing gradient heating to 155-165 ℃ for hydrothermal reaction, cooling to room temperature, filtering, cleaning the filtered substance, and drying to obtain sheet-shaped semi-metal MoTe2And flaky semi-metal MoTe2and/RGO. The preparation process is simple.

Description

Flaky semimetal MoTe2And flaky semi-metal MoTe2Preparation method of/RGO
Technical Field
The invention belongs to the technical field of electrocatalysts, and relates to a flaky semi-metal MoTe2And flaky semi-metal MoTe2A process for the preparation of RGO.
Background
Hydrogen is a clean energy source and is currently receiving wide attention. Electrocatalytic water is currently one of the most efficient methods for producing hydrogen. MoTe2The catalyst is an ideal electrocatalyst due to excellent photoelectric properties. MoTe2Generally, there are three structures of semiconductor, metal and semimetal. Wherein the semiconductor and the semi-metal are stable, and the semi-metal structure and the metal junction are stableThe structure has excellent photoelectric properties, particularly high conductivity; in order to meet the requirements of higher hydrogen production performance and long-term stability of electrocatalysis, MoTe with a semi-metal structure is selected at present2MoTe of current single-layer semi-metal structure2It is generally necessary to first synthesize a bulk semiconductor structure MoTe2Then layered into the semi-metal MoTe by applying various complicated chemical and physical layering methods2. However, the currently used delamination methods mostly result in lamellar single-layer MoTe2Is a semiconductor structure or a mixed semiconductor and semi-metal structure.
Disclosure of Invention
The invention aims to provide a flaky semimetal MoTe with simple process2And flaky semi-metal MoTe2A process for the preparation of RGO.
The invention is realized by the following technical scheme:
flaky semimetal MoTe2And flaky semi-metal MoTe2A method for preparing/RGO, comprising the following steps:
step 1: adding 0.002-0.004 mol of tellurium powder and 0.004-0.008 mol of potassium borohydride into 10ml of deionized water, placing the mixture in a sealed environment for reaction to obtain Te2-A precursor aqueous solution;
step 2: dissolving 0.001/7-0.002/7 mol of ammonium paramolybdate in 10ml of solvent, and adding 0.0025-0.005 mol of citric acid to obtain a precursor solution of the molybdenum ion source;
and step 3: mixing Te2-Placing the precursor aqueous solution and the molybdenum ion source precursor solution into a reaction kettle, keeping the solution at room temperature, performing gradient heating to 155-165 ℃ for hydrothermal reaction, cooling to room temperature, filtering, cleaning the filtered substance, and drying to obtain sheet-shaped semi-metal MoTe2And flaky semi-metal MoTe2/RGO。
Further, in the step 1, the weight ratio of the tellurium powder to the potassium borohydride is 1: 2.
Furthermore, the reaction time in the step 1 is 40-50 h.
Further, the solvent in step 2 is deionized water.
Further, the solvent in the step 2 is 1mg/ml graphene oxide aqueous solution.
Further, the time for keeping at room temperature in the step 3 is 10-12 hours.
Further, in the step 3, the temperature is raised to 45-55 ℃ and kept for 4-5 h, then raised to 95-105 ℃ and kept for 3-4 h, and then raised to 155-165 ℃ for hydrothermal reaction for 15-17 h.
Further, the heating rate of the gradient temperature rise in the step 3 is 10-40 ℃/min.
Further, deionized water and ethanol are adopted for cleaning in the step 3.
Further, the drying in the step 3 is carried out at the temperature of 50-60 ℃ for 12-14 h.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention provides flaky semimetal MoTe2And flaky semi-metal MoTe2The preparation method of/RGO, citric acid plays a role in dispersing and chelating in the course of preparation, adopt the ladder hydrothermal temperature to carry on the hydrothermal reaction separately, thus produce the flaky semimetal ditelluride molybdenum, it does not need to synthesize the massive semimetal ditelluride molybdenum first and then apply various complicated chemistry and physical stratification method to stratify, the reaction process adopted in this method only involves the hydrothermal reaction, the process for its preparation is simple, and the apparatus cost involved in the reaction is low, with low consumption of energy.
Further, the solvent is graphene oxide aqueous solution, ammonium paramolybdate is dissolved in the graphene oxide aqueous solution, and then Te is added2-The precursor aqueous solution generates RGO which plays a role of a template in the later stage of step temperature rise, heat preservation and hydrothermal reaction, so that the generated semimetal molybdenum ditelluride is better formed into a sheet shape and is compounded with the RGO; the flaky molybdenum ditelluride and graphene oxide are compounded, and the introduction of the graphene increases the conductivity of the molybdenum ditelluride and generates an interface effect, so that the hydrogen evolution catalytic performance of the molybdenum ditelluride with a semimetal structure is enhanced.
Drawings
FIG. 1 shows the medium half metal MoTe prepared in examples 1 and 2 of the present invention2And half-metal MoTe2/TEM of RGOA drawing;
FIG. 2 shows the medium half metal MoTe prepared in examples 1 and 2 of the present invention2And half-metal MoTe2/XRD pattern of RGO;
FIG. 3 shows the medium half metal MoTe prepared in examples 1 and 2 of the present invention2And half-metal MoTe2/Raman spectrum of RGO;
FIG. 4 shows the medium half metal MoTe2 and the half metal MoTe prepared in examples 1 and 2 of the present invention2/Infrared spectroscopy of RGO;
FIG. 5 shows the medium half metal MoTe prepared in examples 1 and 2 of the present invention2And half-metal MoTe2/Fluorescence spectrum of RGO.
Detailed Description
Specific examples are given below.
Example 1
Flaky semimetal MoTe2And flaky semi-metal MoTe2A method for preparing/RGO, comprising the following steps:
step 1: adding 0.004mol of tellurium powder and 0.008mol of potassium borohydride into 10ml of deionized water, and reacting for 48 hours in a sealed environment until the reaction is completed to obtain Te2-Te at a concentration of 0.4mol/L2-A precursor aqueous solution;
step 2: dissolving 0.002/7mol of ammonium paramolybdate in 10ml of deionized water, and adding 0.005mol of citric acid to obtain a precursor solution of the molybdenum ion source;
and step 3: mixing Te2-Placing the precursor aqueous solution and the molybdenum ion source precursor solution into a reaction kettle, keeping the solution at room temperature for 12h, sequentially heating to 50 ℃ at a heating rate of 10 ℃/min, keeping the solution at 4h, heating to 100 ℃ and keeping the solution at 4h, heating to 160 ℃ for hydrothermal reaction for 16h, cooling to room temperature, filtering, washing filtrate deionized water and ethanol for 5 times, and drying at 60 ℃ for 12h to obtain flaky semi-metal MoTe2
Example 2
Flaky semimetal MoTe2And flaky semi-metal MoTe2A method for preparing/RGO, comprising the following steps:
step 1: 0.004mol of tellurium powder and 0.008mol of potassium borohydride are added into 10ml of deionized waterReacting for 48 hours in water in a sealed environment until the reaction is complete to obtain Te2-Te at a concentration of 0.4mol/L2-A precursor aqueous solution;
step 2: dissolving 0.002/7mol of ammonium paramolybdate in 10ml of graphene oxide aqueous solution, and adding 0.005mol of citric acid to obtain a precursor solution of a molybdenum ion source; wherein the concentration of the graphene oxide aqueous solution is 1 mg/ml;
and step 3: mixing Te2-Placing the precursor aqueous solution and the molybdenum ion source precursor solution into a reaction kettle, keeping the solution at room temperature for 12h, sequentially heating to 50 ℃ at a heating rate of 20 ℃/min, keeping the solution at 4h, heating to 100 ℃ and keeping the solution at 4h, heating to 160 ℃ for hydrothermal reaction for 16h, cooling to room temperature, filtering, washing filtrate deionized water and ethanol for 5 times, and drying at 60 ℃ for 12h to obtain flaky semi-metal MoTe2/RGO。
Samples prepared in examples 1 and 2 were taken, wherein a is the semimetal MoTe2Powder b is half-metal MoTe2/RGO; as shown in fig. 1, 2 samples prepared were all sheet-like structures; as shown in FIG. 2, MoTe in 2 samples prepared2All have a hexagonal structure; as shown in FIG. 3, the prepared 2 samples are all semimetal structures, but semiconductor structures are formed when citric acid is not added, and the thickness of the semiconductor structure ranges from 1200 cm to 1650cm in FIG. 3-1A higher peak D than peak G in between also indicates sufficient reduction of GO to RGO; as shown in FIG. 4, 4000-3438 cm of infrared spectrum of the prepared 2 samples-1The peaks at wave number indicate that the synthesized powders are all hydrophilic, and RGO leads to increased hydrophilicity; as shown in FIG. 5, peaks at 760nm in the prepared 2 sample fluorescence spectra correspond to MoTe2RGO causes the peak to increase, indicating that recombination of RGO causes electrons to move from RGO to MoTe2Transfer, and Cu doping causes the peak to weaken, indicating that electrons in the conduction band are transferred to the Cu impurity level. MoTe2Semi-metal structure of (A), hydrophilicity enhancement by RGO and electron transfer from RGO to MoTe2The transfer indicates that the composite powder has excellent hydrogen evolution catalytic activity.
Example 3
Flaky semimetal MoTe2And flaky semi-metal MoTe2A method for preparing/RGO, comprising the following steps:
step 1: adding 0.002mol of tellurium powder and 0.004mol of potassium borohydride into 10ml of deionized water, and reacting for 48 hours in a sealed environment until complete reaction is achieved to obtain Te2-Te at a concentration of 0.2mol/L2-A precursor aqueous solution;
step 2: dissolving 0.001/7mol of ammonium paramolybdate in 10ml of deionized water, and adding 0.0025mol of citric acid to obtain a precursor solution of a molybdenum ion source;
and step 3: mixing Te2-Placing the precursor aqueous solution and the molybdenum ion source precursor solution into a reaction kettle, keeping the temperature at room temperature for 11h, sequentially heating to 50 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 5h, heating to 100 ℃ and keeping the temperature for 3h, heating to 160 ℃ for hydrothermal reaction for 16h, cooling to room temperature, filtering, washing the filtrate with deionized water and ethanol for 5 times, and drying at 50 ℃ for 14h to obtain sheet-shaped half-metal MoTe2。。
Example 4
Flaky semimetal MoTe2And flaky semi-metal MoTe2A method for preparing/RGO, comprising the following steps:
step 1: adding 0.002mol of tellurium powder and 0.004mol of potassium borohydride into 10ml of deionized water, and reacting for 48 hours in a sealed environment until complete reaction is achieved to obtain Te2-Te at a concentration of 0.2mol/L2-A precursor aqueous solution;
step 2: dissolving 0.001/7mol of ammonium paramolybdate in 10ml of graphene oxide aqueous solution, and adding 0.0025mol of citric acid to obtain a precursor solution of a molybdenum ion source; wherein the concentration of the graphene oxide aqueous solution is 1 mg/ml;
and step 3: mixing Te2-Placing the precursor aqueous solution and the molybdenum ion source precursor solution into a reaction kettle, keeping the solution at room temperature for 11h, sequentially heating to 50 ℃ at a heating rate of 20 ℃/min, keeping the solution at 5h, heating to 100 ℃ and keeping the solution at 3h, heating to 160 ℃ for hydrothermal reaction for 16h, cooling to room temperature, filtering, washing the filtrate with deionized water and ethanol for 5 times, and drying at 50 ℃ for 14h to obtain sheet-shaped half-metal MoTe2/RGO。
Example 5
Flaky semimetal MoTe2And flaky semi-metal MoTe2A process for the preparation of/RGO comprisingThe following steps:
step 1: adding 0.003mol of tellurium powder and 0.006mol of potassium borohydride into 10ml of deionized water, and reacting for 48 hours in a sealed environment until the reaction is completed to obtain Te2-Te at a concentration of 0.3mol/L2-A precursor aqueous solution;
step 2: dissolving 0.0015/7mol of ammonium paramolybdate in 10ml of deionized water, and adding 0.00375mol of citric acid to obtain a precursor solution of the molybdenum ion source;
and step 3: mixing Te2-Placing the precursor aqueous solution and the molybdenum ion source precursor solution into a reaction kettle, keeping the solution at room temperature for 12h, sequentially heating to 50 ℃ at a heating rate of 20 ℃/min, keeping the solution at 4h, heating to 100 ℃ and keeping the solution at 4h, heating to 160 ℃ for hydrothermal reaction for 16h, cooling to room temperature, filtering, washing filtrate deionized water and ethanol for 5 times, and drying at 55 ℃ for 13h to obtain flaky semi-metal MoTe2
Example 6
Flaky semimetal MoTe2And flaky semi-metal MoTe2A method for preparing/RGO, comprising the following steps:
step 1: adding 0.003mol of tellurium powder and 0.006mol of potassium borohydride into 10ml of deionized water, and reacting for 48 hours in a sealed environment until the reaction is completed to obtain Te2-Te at a concentration of 0.3mol/L2-A precursor aqueous solution;
step 2: dissolving 0.0015/7mol of ammonium paramolybdate in 10ml of graphene oxide aqueous solution, and adding 0.00375mol of citric acid to obtain a precursor solution of the molybdenum ion source; wherein the concentration of the graphene oxide aqueous solution is 1 mg/ml;
and step 3: mixing Te2-Placing the precursor aqueous solution and the molybdenum ion source precursor solution into a reaction kettle, keeping the solution at room temperature for 12h, sequentially heating to 50 ℃ at a heating rate of 30 ℃/min, keeping the solution at 4h, heating to 100 ℃ and keeping the solution at 4h, heating to 160 ℃ for hydrothermal reaction for 16h, cooling to room temperature, filtering, washing filtrate deionized water and ethanol for 5 times, and drying at 55 ℃ for 13h to obtain flaky semi-metal MoTe2/RGO。
Example 7
Flaky semimetal MoTe2And flaky semi-metal MoTe2Preparation of/RGOThe method comprises the following steps:
step 1: adding 0.002mol of tellurium powder and 0.004mol of potassium borohydride into 10ml of deionized water, and reacting for 40h in a sealed environment until the reaction is complete to obtain Te2-Te at a concentration of 0.2mol/L2-A precursor aqueous solution;
step 2: dissolving 0.001/7mol of ammonium paramolybdate in 10ml of deionized water, and adding 0.0025mol of citric acid to obtain a precursor solution of a molybdenum ion source;
and step 3: mixing Te2-Placing the precursor aqueous solution and the molybdenum ion source precursor solution into a reaction kettle, keeping the solution at room temperature for 10h, sequentially heating to 50 ℃ at a heating rate of 30 ℃/min, keeping the solution at 5h, heating to 100 ℃ and keeping the solution at 3h, heating to 160 ℃ for hydrothermal reaction for 17h, cooling to room temperature, filtering, washing filtrate deionized water and ethanol for 5 times, and drying at 60 ℃ for 12h to obtain flaky semi-metal MoTe2。。
Example 8
Flaky semimetal MoTe2And flaky semi-metal MoTe2A method for preparing/RGO, comprising the following steps:
step 1: adding 0.002mol of tellurium powder and 0.004mol of potassium borohydride into 10ml of deionized water, and reacting for 40h in a sealed environment until the reaction is complete to obtain Te2-Te at a concentration of 0.2mol/L2-A precursor aqueous solution;
step 2: dissolving 0.001/7mol of ammonium paramolybdate in 10ml of graphene oxide aqueous solution, and adding 0.0025mol of citric acid to obtain a precursor solution of a molybdenum ion source; wherein the concentration of the graphene oxide aqueous solution is 1 mg/ml;
and step 3: mixing Te2-Placing the precursor aqueous solution and the molybdenum ion source precursor solution into a reaction kettle, keeping the solution at room temperature for 10h, sequentially heating to 50 ℃ at a heating rate of 30 ℃/min, keeping the solution at 5h, heating to 100 ℃ and keeping the solution at 3h, heating to 160 ℃ for hydrothermal reaction for 17h, cooling to room temperature, filtering, washing filtrate deionized water and ethanol for 5 times, and drying at 60 ℃ for 12h to obtain flaky semi-metal MoTe2/RGO。
Example 9
Flaky semimetal MoTe2And flaky semi-metal MoTe2A method for preparing/RGO, comprising the following steps:
step 1: adding 0.003mol of tellurium powder and 0.006mol of potassium borohydride into 10ml of deionized water, and reacting for 50h in a sealed environment until the reaction is completed to obtain Te2-Te at a concentration of 0.3mol/L2-A precursor aqueous solution;
step 2: dissolving 0.0015/7mol of ammonium paramolybdate in 10ml of deionized water, and adding 0.00375mol of citric acid to obtain a precursor solution of the molybdenum ion source;
and step 3: mixing Te2-Placing the precursor aqueous solution and the molybdenum ion source precursor solution into a reaction kettle, keeping the solution at room temperature for 12h, sequentially heating to 50 ℃ at a heating rate of 30 ℃/min, keeping the solution at 4h, heating to 100 ℃ and keeping the solution at 4h, heating to 160 ℃ for hydrothermal reaction for 15h, cooling to room temperature, filtering, washing filtrate deionized water and ethanol for 5 times, and drying at 55 ℃ for 13h to obtain flaky semi-metal MoTe2
Example 10
Flaky semimetal MoTe2And flaky semi-metal MoTe2A method for preparing/RGO, comprising the following steps:
step 1: adding 0.003mol of tellurium powder and 0.006mol of potassium borohydride into 10ml of deionized water, and reacting for 50h in a sealed environment until the reaction is completed to obtain Te2-Te at a concentration of 0.3mol/L2-A precursor aqueous solution;
step 2: dissolving 0.0015/7mol of ammonium paramolybdate in 10ml of graphene oxide aqueous solution, and adding 0.00375mol of citric acid to obtain a precursor solution of the molybdenum ion source; wherein the concentration of the graphene oxide aqueous solution is 1 mg/ml;
and step 3: mixing Te2-Placing the precursor aqueous solution and the molybdenum ion source precursor solution into a reaction kettle, keeping the solution at room temperature for 12h, sequentially heating to 50 ℃ at a heating rate of 30 ℃/min, keeping the solution at 4h, heating to 100 ℃ and keeping the solution at 4h, heating to 160 ℃ for hydrothermal reaction for 15h, cooling to room temperature, filtering, washing filtrate deionized water and ethanol for 5 times, and drying at 55 ℃ for 13h to obtain flaky semi-metal MoTe2/RGO。

Claims (10)

1. Flaky semimetal MoTe2And flaky semi-metal MoTe2A method for producing/RGO, characterized by comprising the steps of:
step 1: adding 0.002-0.004 mol of tellurium powder and 0.004-0.008 mol of potassium borohydride into 10ml of deionized water, placing the mixture in a sealed environment for reaction to obtain Te2-A precursor aqueous solution;
step 2: dissolving 0.001/7-0.002/7 mol of ammonium paramolybdate in 10ml of solvent, and adding 0.0025-0.005 mol of citric acid to obtain a precursor solution of the molybdenum ion source;
and step 3: mixing Te2-Placing the precursor aqueous solution and the molybdenum ion source precursor solution into a reaction kettle, keeping the solution at room temperature, performing gradient heating to 155-165 ℃ for hydrothermal reaction, cooling to room temperature, filtering, cleaning the filtered substance, and drying to obtain sheet-shaped semi-metal MoTe2And flaky semi-metal MoTe2/RGO。
2. The method for preparing the sheet-shaped half-metal MoTe2 and the sheet-shaped half-metal MoTe2/RGO according to claim 1, wherein the weight ratio of the tellurium powder to the potassium borohydride in the step 1 is 1: 2.
3. Sheet-like semimetal MoTe according to claim 12And flaky semi-metal MoTe2The preparation method of/RGO is characterized in that the reaction time in the step 1 is 40-50 h.
4. Sheet-like semimetal MoTe according to claim 12And flaky semi-metal MoTe2The preparation method of/RGO is characterized in that the solvent in the step 2 is deionized water.
5. Sheet-like semimetal MoTe according to claim 12And flaky semi-metal MoTe2The preparation method of/RGO is characterized in that the solvent in the step 2 is 1mg/ml graphene oxide aqueous solution.
6. Sheet-like semimetal MoTe according to claim 12And flaky semi-metal MoTe2The preparation method of/RGO is characterized in that the time of keeping at room temperature in the step 3 is 10-12 h.
7. Sheet-like semimetal MoTe according to claim 12And flaky semi-metal MoTe2The preparation method of/RGO is characterized in that in the step 3, the temperature is raised to 45-55 ℃ and kept for 4-5 h, then raised to 95-105 ℃ and kept for 3-4 h, and then raised to 155-165 ℃ for hydrothermal reaction for 15-17 h.
8. Sheet-like semimetal MoTe according to claim 12And flaky semi-metal MoTe2The preparation method of/RGO is characterized in that the heating rate of the gradient temperature rise in the step 3 is 10-40 ℃/min.
9. Sheet-like semimetal MoTe according to claim 12And flaky semi-metal MoTe2The preparation method of/RGO is characterized in that deionized water and ethanol are adopted for cleaning in the step 3.
10. Sheet-like semimetal MoTe according to claim 12And flaky semi-metal MoTe2The preparation method of/RGO is characterized in that the drying in the step 3 is drying at 50-60 ℃ for 12-14 h.
CN201910934298.6A 2019-09-29 2019-09-29 Flaky semimetal MoTe2And flaky semi-metal MoTe2Preparation method of/RGO Pending CN110624572A (en)

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Application publication date: 20191231