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Method for preparing titanium disulfide crystal and product

A technology of titanium disulfide and crystals, which is applied in the field of efficient preparation of titanium disulfide crystals, can solve problems such as unclear safety, high reaction temperature, and many reaction steps, and achieve the effects of good repeatability, high purity, and short reaction time

Inactive Publication Date: 2020-12-22
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, the safety of using hydrogen and hydrogen sulfide gas is not clear; the reaction time is long; the reaction temperature is too high, the reaction steps are many, the process is cumbersome; the production efficiency is low, etc.

Method used

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  • Method for preparing titanium disulfide crystal and product
  • Method for preparing titanium disulfide crystal and product
  • Method for preparing titanium disulfide crystal and product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1 Optimal temperature prepares the whole process of titanium disulfide crystal

[0022] It uses titanium powder and sulfur powder as raw materials. First weigh 0.0032 mol of titanium powder, then weigh 0.0071 mol of sulfur powder; then weigh the weighed titanium powder and sulfur powder respectively, pack them in sealed bags, and finish loading the samples in the glove box Use SX-8307 1300 single-component ultra-high temperature structural adhesive to seal the quartz tube, and then place the sealed quartz tube under a baking lamp at 120°C for 4-6 hours. After the sealant is completely solidified, put it into the tube furnace at 600 ℃ for 48 hours. After the reaction is finished, wait for it to cool to room temperature, and a black powder sample can be obtained.

[0023] figure 1 The TiS prepared under the above conditions is given 2 The Raman spectrum of the crystal, where the Raman vibration mode: including E g Mode and A 1g mode, respectively located ...

Embodiment 2

[0024] Embodiment 2 prepares the whole process of titanium disulfide crystal at slightly lower temperature (counterexample)

[0025] It uses titanium powder and sulfur powder as raw materials. First weigh 0.0032mol of titanium powder, then weigh 0.0071mol of sulfur powder; then put the weighed titanium powder and sulfur powder into sealed bags, and use SX-8307 1300 single Component ultra-high temperature structural glue to seal the quartz tube, then place the sealed quartz tube under a 120°C oven lamp for 4-6 hours, and put it in a tube furnace for 48 hours at 550°C after the sealant is completely solidified . After the reaction is finished, wait for it to cool to room temperature, and a black powder sample can be obtained.

[0026] Figure 6 The XRD spectrum of the sample prepared under the above conditions is given, which proves that the crystallinity of the sample synthesized at 550°C is poor, the purity is low, and there is residual titanium after the reaction, which sh...

Embodiment 3

[0027] Example 3 The whole process of preparing titanium disulfide crystals with different reactant ratios

[0028] It uses titanium powder and sulfur powder as raw materials. First, according to the molar ratio of titanium to sulfur 2:3 (Ti:0.0042mol, S:0.0062mol); 1:2 (Ti: 0.0032mol, S:0.0071mol); 1:3 (Ti:0.0022mol, S:0.0069mol) ) Weigh the corresponding starting reactants; pack the weighed titanium powder and sulfur powder with weighing paper respectively and put them into sealed bags, complete the sample loading and sealing in the glove box and mark Ⅰ, Ⅱ, and In group III experiment, place the sealed quartz tube under a baking lamp at 120°C for 4-6 hours. After the sealant is completely solidified, put it into a tube furnace and keep it at the optimum temperature of 600°C for 48 hours. After the reaction is finished, wait for it to cool to room temperature, and a black powder sample can be obtained.

[0029] By drawing the XRD spectrum ( Figure 7 ), proving that the sa...

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Abstract

The invention discloses a method for preparing a titanium disulfide crystal and a product, and belongs to the technical field of preparation of IVB-VIA group transition metal chalcogenide. The preparation method comprises the following steps: sequentially filling a quartz tube with titanium powder and sulfur powder in a glove box, conducting standing for 1-2 hours, sealing the quartz tube, placingthe quartz tube under a baking lamp at 120 DEG C for 4-6 hours, placing the quartz tube into a tube furnace, conducting vacuumizing for three times, introducing argon, carrying out sealed reaction inthe tube furnace for 4-8 hours, and conducting cooling to room temperature to obtain titanium disulfide crystals. The titanium disulfide crystal is a 1T-TiS2 hexagonal crystal, and the space group ofthe titanium disulfide crystal is P-3m1. The crystal is of a layered structure. The length of a wafer is 10-11 [mu]m, the width of the wafer is 11-13 [mu]m, and the thickness of the wafer is 1-2 [mu]m. The method is simple and easy to operate, good in repeatability and low in cost, and the prepared TiS2 crystal has the advantages of being high in purity, complete in wafer development, uniform indistribution and the like.

Description

technical field [0001] The invention belongs to the technical field of preparing IVB-VIA group transition metal chalcogenides, and in particular relates to a simple, novel and efficient method for preparing titanium disulfide crystals and products prepared by the method. Background technique [0002] Transition metal dichalcogenides are an important class of materials, which have attracted people's attention due to their rich physical and chemical properties. Especially MoS 2 、WS 2 and WSe 2 As typical transition metal dichalcogenides, the abundant phenomena exhibited in the fields of optoelectronics, valley electrons, and spintronics have aroused extensive research enthusiasm. Recent studies have shown that the application of titanium disulfide in transition metal dichalcogenides in nanoelectronics, photonics, sensors, electrodes for energy storage systems, etc. has attracted widespread attention. Layered titanium disulfide has good electron mobility and intercalation, ...

Claims

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Application Information

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IPC IPC(8): C30B29/46C30B25/00C30B28/14C01G23/00
CPCC01G23/007C01P2002/60C01P2002/72C01P2002/76C01P2002/82C01P2004/03C01P2004/20C01P2004/61C30B25/00C30B28/14C30B29/46
Inventor 李芳菲冯登满李亮周强黄丽彤朱健
Owner JILIN UNIV
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