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Transition metal sulfied nano-pipe and preparation process and its application

A technology of transition metals and nanotubes, applied in chemical instruments and methods, molybdenum sulfide, niobium compounds, etc., to achieve high-rate discharge, excellent high-temperature performance, long cycle life, and small volume expansion

Inactive Publication Date: 2004-06-30
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, except for this topic about MoS 2 [Chen J, Kuriyama N, Yuan H T, et al. Electrochemical hydrogen storage in MoS 2 nanotubes.J Am Chem Soc, 2001, 123:11813-11814.], but high-purity MS X The use of open, multi-wall or single-wall nanotubes as reversible hydrogen storage, lithium storage and battery electrode materials has not been reported at home and abroad.

Method used

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  • Transition metal sulfied nano-pipe and preparation process and its application
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  • Transition metal sulfied nano-pipe and preparation process and its application

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1: high-purity MS 2 Low-temperature catalytic preparation of nanotubes.

[0021] High-purity TiS 2 , ZrS 2 , NbS 2 Low-temperature catalytic preparation of nanotubes. In an Ar gas glove box, 5 g of TiS with a purity of 99% 3 , ZrS 3 or NbS 3 The crystal powder and 25g stainless steel balls (Φ6mm) were put into a stainless steel tank, and sealed with a cover. The sealed stainless steel tank was placed on a planetary ball mill (Nanjing University Instrument Factory, QM-1SPR-CL) for high-energy ball milling (rotation speed: 600 rpm) for 1 hour. Put the ball-milled powder on the Al 2 o 3 On the sheet, put it into the high-temperature reaction furnace. In the experiment, H was introduced at a volume ratio of 18:1:1 2 / CH 4 / C 4 h 4 S (total flow 100mL / min), heat reaction at 360°C for 1h. The reaction tail gas is introduced into 1M ZnSO 4 solution to remove the generated gas H 2 S. The thermal decomposition reactions involved in its growth are:

[...

Embodiment 2

[0027] TiS prepared according to embodiment 1 2 and MoS 2 Nanotubes outperform ordinary TiS in terms of gas / solid hydrogen storage capacity 2 and MoS 2 Polycrystalline materials have been greatly improved. TiS was measured using a pressure / composition / temperature (PCT) device 2 and MoS 2 Hydrogen storage comparison between nanotubes and polycrystalline materials image 3 shown. After reaching the hydrogen absorption platform, TiS 2 The hydrogen uptake of nanotubes is 1.8wt%, MoS 2 The hydrogen absorption capacity of the nanotubes is 1.2wt%, while the TiS 2 and MoS 2 The hydrogen uptake of polycrystalline materials is only 0.2wt% and 0.25wt%, respectively. Therefore, using TiS 2 and MoS 2 The capacity of nanotubes for gas / solid hydrogen storage is significantly higher than that of their polycrystalline counterparts.

Embodiment 3

[0028] Example 3: TiS prepared in Example 1 by using an electrochemical three-electrode measurement system 2 and MoS 2 The nanotubes were analyzed for electrochemical hydrogen storage. The electrochemical hydrogen storage capacity data are shown in Table 1. The results showed that: TiS 2 and MoS 2 The discharge capacity of nanotubes is significantly higher than their polycrystalline counterparts, and the high-rate discharge performance of nanotubes is also good. After 100 0.5C charge / discharge cycles, the TiS 2 and MoS 2 The electrode capacity of nanotubes decays only about 2% ( Figure 4 ). Therefore, such nanotubes can be applied to the development of new nickel / hydrogen batteries.

[0029] Electrode material

[0030] Note: The high rate discharge performance refers to the ratio of the capacity of the electrode discharged at 200mA / g and 50mA / g.

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Abstract

A nanotube of transition metal sulfide (MSx, where M is Ti, Sr, Nb, Mo, W, etc and X=1 or 2) is prepared by low-temp gas-solid catalytic reaction. The said nanotube has unique laminated tubular structure and large specific surface area, and can be used as the hydrogen bearing or lithium bearing electrode of battery as it has high change-discharge speed and excellent cycle life.

Description

Technical field [0001] The present invention relates to the preparation of sulfide nanotubes, it is about transition metal MS X Preparation methods of nanotubes and their applications in hydrogen storage, lithium storage and electrode materials. MS X In the formula, M is a transition metal of Group IV-VIB, such as Ti, Zr, Nb, Mo, W, etc.; X is 1 or 2. This series of nanotubes has a very ordered layered tubular structure, the length of which can reach 3-5 μm, the inner diameter is 10-25 nm, the outer diameter is 25-60 nm, and the layer spacing is 0.57-0.63 nm. Background technique [0002] Nanotechnology will speed up human life as a bridge linking ICT and life sciences and as a future enabling technology. The ultimate goal of nanotechnology is to manufacture products with special functions starting from atoms and molecules. In order to achieve this goal, it is necessary to carry out applied research on nanomaterials and nanodevices. In the big family of nanomaterials, n...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G1/12C01G23/00C01G25/00C01G33/00C01G39/06C01G41/00
Inventor 陈军李锁龙陶占良蔡锋石徐丽娜
Owner NANKAI UNIV
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