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Preparing method of metal chalcogenide nanomesh material

A metal sulfide, metal selenide technology, applied in binary selenium/tellurium compounds, molybdenum sulfide, nanotechnology and other directions, can solve problems such as inability to prepare in large quantities, low yield of nanosieves, and restrictions on large-scale production

Inactive Publication Date: 2014-07-09
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of method needs to first prepare a planar substrate with a regular pore structure, and the thickness of the nanosieve prepared on the planar substrate is also controlled between several nanometers to tens of nanometers, so the nanosieve prepared by this method has the same yield. Very low, cannot be prepared in large quantities
[0005] Generally speaking, the published preparation methods are to synthesize nanosieves on two-dimensional planar substrates. Due to the lack of large enough substrates and the extremely thin thickness of nanosieves deposited on each substrate, the possibility of large-scale production is limited. sex

Method used

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  • Preparing method of metal chalcogenide nanomesh material
  • Preparing method of metal chalcogenide nanomesh material
  • Preparing method of metal chalcogenide nanomesh material

Examples

Experimental program
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Effect test

Embodiment 1

[0068] Preparation of ordered mesoporous silica KIT-6 template material: Accurately weigh 20 grams of triblock copolymer P123 (polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, PEO- PPO-PEO), transferred into a 1000ml beaker, added 720ml of distilled water, 33.3ml of concentrated hydrochloric acid (36-38%). Stir in a water bath at 35 °C until the P123 is completely dissolved. 20 g of n-butanol were added and stirring was continued for 1 hour. Add 43 grams of tetraethyl orthosilicate, keep the temperature at 35 degrees Celsius, and continue to stir for 24 hours. The mixture in the beaker was transferred to a polytetrafluoroethylene hydrothermal kettle, and kept at a constant temperature of 100 degrees Celsius in an oven for 24 hours. After cooling, take it out, filter it with suction, wash the filter cake three times with distilled water, and wash it once with ethanol to obtain a white powder. After the white powder is completely dry, place it in ...

Embodiment 2

[0072] The ordered mesoporous silica KIT-6 material synthesized according to the method described in Example 1 was further heated in a muffle furnace to 900 degrees Celsius at a heating rate of 2 degrees Celsius / minute, kept for 5 hours and then cooled to room temperature to prepare A white powder was obtained. Weigh 10 grams of KIT-6 material after high-temperature treatment at 900 degrees Celsius, and its total pore volume value is calculated to be 5.3 cubic centimeters according to the nitrogen adsorption test results; add 100 ml of xylene and stir at room temperature for 1 hour to obtain a suspension . Ammonium tungstate ((NH 4 ) 10 W 12 o 41 ) and ammonium paramolybdate ((NH 4 ) 6 Mo 7 o 24 4H 2 O) the mixture was dissolved in 5 ml of a 5% by weight ammonia solution. The ammonia solution of the metal precursor was added to the above mixed suspension of mesoporous silica and xylene. Stirring was continued for 4 hours and then suction filtered. The white KIT-6 p...

Embodiment 3

[0075]2.0 g of phosphomolybdic acid was dissolved in 40 ml of ethanol, and 1 g of the KIT-6 template material prepared by the method described in Example 1 was added. Stir at room temperature until the ethanol is completely volatilized, and an ordered mesoporous silica material loaded with phosphomolybdic acid is obtained. Mix it with 10 grams of sulfur powder evenly, and put it into a quartz boat covered with a quartz plate. Place the quartz boat at the mouth of the tube furnace. A stream of pure hydrogen at a flow rate of 100 ml / min was introduced into the tube furnace. The tube furnace was raised to 400 °C. Use a quartz rod to quickly push the quartz boat into the center of the heating zone of the tube furnace for reaction, and hydrogen gas is continuously injected. After reacting for 600 minutes, it was cooled to room temperature under the protection of hydrogen to obtain a black powder. Put the black powder in a 500ml plastic beaker, add 200ml of distilled water, add ...

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Abstract

The invention discloses a preparing method of a metal chalcogenide nanomesh material. A mesoporous material is adopted as a template material. The metal chalcogenide nanomesh material is prepared by steps of: preparing a metal precursor into a solution, filling a pore channel space of the mesoporous template material with the solution so as to prepare a mesoporous material loading the metal precursor; mixing the mesoporous material loading the metal precursor with a chalcogenide precursor and putting the mixture into a heating space of a heating device, or putting the mesoporous material loading the metal precursor and the chalcogenide precursor side by side into the heating space of the heating device; raising the temperature rapidly to 300-900 DEG C under the protection of carrier gas and maintaining the temperature for 15-600 min; adding a template corroding agent into the obtained solid powder so that the mesoporous material is fully dissolved in the template corroding solution; and filtering and drying the filter cake. The metal chalcogenide nanomesh material is obtained by synthesis for the first time. The preparation method is free of use of precious metals, free of vacuum conditions, simple in synthetic process, and prone to large-scale production.

Description

technical field [0001] The invention relates to a preparation method of a metal chalcogenide nano-sieve material, in particular to a mass preparation method of a metal-chalcogenide nano-sieve material with adjustable pore size and controllable pore structure arrangement, and belongs to the field of chemical synthesis of inorganic nano-materials. Background technique [0002] Inorganic nanosieve (nanomesh) material refers to a kind of extremely thin (0.1 to 100 nanometers) two-dimensional sheet or film-like inorganic material, and its sheet is covered with uniformly distributed nanopores that open on both sides of the entire layer. Usually these pores are arranged in a regular structure with long-range order, and the size of the pores is generally larger than the thickness of the sheet. The special structure of this type of material makes it have important application potential in the fields of catalysis, molecular adsorption, separation, and thermoelectric conversion. [00...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04C01G39/06B82Y30/00B82Y40/00
Inventor 施益峰汪均姚朝华
Owner HANGZHOU NORMAL UNIVERSITY
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