Preparation method of high-purity and high-crystallinity titanium disulfide nanometer plates

A titanium disulfide, high crystallinity technology, applied in the field of nanomaterials, can solve the problems of uneven size and shape of nanosheets, no two-dimensional sheet material characteristics, poor crystallinity of nanocrystals, etc. Uniform appearance, large-scale adjustment of size, easy-to-control effect

Active Publication Date: 2014-08-20
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The literature (Well-Defined Colloidal 2-D Layered Transition-Metal Chalcogenide Nanocrystals via Generalized Synthetic protocols, J. Am. Chem. Soc. 2012, 134, 18233-18236) adopts the liquid-phase colloid synthesis method, using TiCl 4 , oleylamine and CS 2 Small-sized TiS was prepared for the reaction reagent 2 Nanocrystalline, and the size range is only 40nm to 150nm, the prepared TiS 2 Nanocrystals have poor crystallinity, low purity, and no obvious characteristics of two-dimensional sheet materials
Literature (Synthetic Strategy and Structural and Optical Characterization of Thin Highly Crystalline Titanium Disulfide Nanosheets, J. Phys. Chem. Lett. 2012, 3, 1554? 1558) adopts liquid phase method, with sulfur powder, TiCl 4 React with oleylamine as raw material to prepare TiS with larger area 2 Nanosheets, but the size and shape of the nanosheets prepared by this method are not uniform, the size is uncontrollable, and the purity is not high, containing obvious acicular TiO 2 Impurities
At present, there is no existing liquid-phase synthesis technology that can prepare TiS2 nanosheets with uniform size and shape, good dispersion, large-scale controllable size, high crystallinity and purity. Preparation technology

Method used

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  • Preparation method of high-purity and high-crystallinity titanium disulfide nanometer plates
  • Preparation method of high-purity and high-crystallinity titanium disulfide nanometer plates
  • Preparation method of high-purity and high-crystallinity titanium disulfide nanometer plates

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Experimental program
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Embodiment 1

[0030] A two-step liquid-phase colloid synthesis method is adopted. In the first step, a titanium source and a surfactant are added to a container, heated to a certain temperature, stirred and mixed. In the second step, the sulfur source is injected, and the temperature is raised to the reaction temperature for a period of time to prepare TiS with uniform size and shape and high purity. 2 Nanosheets, the specific steps are as follows:

[0031] Step 1. Add 0.11ml TiCl to a 100ml four-neck flask 4 , 3.7ml oleylamine, 15ml octadecene, mixed and stirred.

[0032]Step 2. Raise the temperature to 100°C, pump air with a mechanical pump for 40 seconds, and then introduce Ar gas, and repeat this 10 times to remove impurities.

[0033] Step 3. Continue to raise the temperature to 180° C. and stir for 30 minutes to make the reactants evenly mixed.

[0034] Step 4. Inject CS into the container 2 , raised to 300°C, and kept warm for 3h.

[0035] Step 5, after the reaction ...

Embodiment 2

[0039] A two-step liquid-phase colloid synthesis method is adopted. In the first step, a titanium source and a surfactant are added to a container, heated to a certain temperature, stirred and mixed. In the second step, the sulfur source is injected, the temperature is raised to the reaction temperature and kept for a period of time, and high-purity TiS is prepared. 2 Nanosheets, the specific steps are as follows:

[0040] Step 1. Add 0.11ml TiCl to a 100ml four-neck flask 4 , 3.7ml oleylamine, 10ml octadecene, mixed and stirred.

[0041] Step 2. Raise the temperature to 120°C, pump air with a mechanical pump for 40 seconds, and then introduce Ar gas, repeating this 15 times to remove impurities.

[0042] Step 3. Continue to raise the temperature to 260°C, and stir for 20 minutes to make the reactants evenly mixed.

[0043] Step 4. Inject CS into the container 2 , raised to 270°C, and kept warm for 1h.

[0044] Step 5, after the reaction is over, remove the he...

Embodiment 3

[0048] A two-step liquid-phase colloid synthesis method is adopted. In the first step, a titanium source and a surfactant are added to a container, heated to a certain temperature, stirred and mixed. In the second step, the sulfur source is injected, the temperature is raised to the reaction temperature and kept for a period of time, and high-purity TiS is prepared. 2 Nanosheets, the specific steps are as follows:

[0049] Step 1. Add 0.11ml TiCl to a 100ml four-neck flask 4 , 3.7ml oleylamine, 20ml octadecene, mixed and stirred.

[0050] Step 2. Raise the temperature to 140°C, pump air with a mechanical pump for 40 seconds, and then introduce Ar gas, and repeat this 12 times to remove impurities.

[0051] Step 3. Continue to raise the temperature to 300° C. and stir for 20 minutes to make the reactants evenly mixed.

[0052] Step 4. Inject CS into the container 2 , raised to 310°C, and kept warm for 3h.

[0053] Step 5, after the reaction is over, remove the ...

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Abstract

The invention discloses a preparation method of high-purity and high-crystallinity titanium disulfide nanometer plates. A layer-like TiS2 nanometer plate has good electronic mobility and good intercalation performance and is applicable to a cathode material of a lithium ion battery, a super capacitor and the like. By adopting a two-step liquid-phase colloid synthesis technology, the preparation method can be used for synthesizing hexagonal crystal system type high-purity high-crystallinity TiS2 nanometer plates through reaction of a titanium source, a sulfur source and a surfactant. The preparation method comprises the following steps: firstly uniformly mixing the titanium source with the surfactant, then filling the sulfur source, heating to a specified temperature and preserving heat for a certain time so as to generate the high-purity high-crystallinity TiS2 nanometer plates different in thickness. The preparation method disclosed by the invention is moderate in reaction condition, simple in preparation process, easy to control and good in repeatability. The TiS2 nanometer plates obtained through the preparation method disclosed by the invention are uniform in size and shape, controllable in size, good in crystallinity and high in purity.

Description

technical field [0001] The invention relates to nanomaterial technology, in particular to a hexagonal titanium disulfide (TiS 2 ) Preparation method of nanosheets. Background technique [0002] Titanium disulfide (TiS 2 ) is a typical transition metal dichalcogenide, and its stable structure is a 1T-type octahedral coordination structure, which is a hexagonal close-packed CdI 2 structure, the hexagonal basal plane is highly anisotropic perpendicular to the basal plane; the adjacent six S atoms in the layer form an octahedron, and Ti is located in the center of the octahedron, forming a TiS 6 Octahedrons, which are covalently bonded; form a "sandwich" layered structure of S-Ti-S in the c-axis direction, and the layers are connected by weak van der Waals force. [0003] Layered TiS 2 Due to the van der Waals layer with a large gap, other molecular atoms can be easily intercalated into it, due to the Li + It is easier to enter and exit TiS 2 The van der Waals layer, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00B82Y30/00B82Y40/00
Inventor 朱正峰邹友生曾海波宋秀峰
Owner NANJING UNIV OF SCI & TECH
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