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Preparation method of high-efficiency composite catalyst film for overlength carbon nano tube growth

A technology of ultra-long carbon nanotubes and composite catalysts, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of reduced catalyst activity and low growth rate of CNTs and other problems, to achieve the effect of preventing aggregation, low preparation cost and high efficiency

Active Publication Date: 2012-01-11
SUZHOU CREATIVE CARBON NANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, during the transformation of thin-film catalysts into catalyst particles or clusters with the furnace temperature rising, the activity of the catalysts will decrease, resulting in lower CNTs growth rate and short CNTs arrays.

Method used

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  • Preparation method of high-efficiency composite catalyst film for overlength carbon nano tube growth
  • Preparation method of high-efficiency composite catalyst film for overlength carbon nano tube growth

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The silicon substrate (out-of-plane orientation (111) or (100)) was ultrasonically cleaned with acetone, ethanol and deionized water, then dried with a nitrogen gun, and immediately placed in the reaction chamber of the reactive magnetron sputtering device. Ensure that the absolute pressure of the back of the reaction chamber before deposition is lower than 5×10 -3 Pa. Metal Fe and Mg targets with a purity better than 99.99wt% are used as sputtering targets, high-purity Ar gas and O with a purity better than 99.99% 2 as the sputtering atmosphere. Ar and O 2 After the gas is fully mixed, it is introduced into the reaction chamber through the catheter, Ar gas and O 2 The flow ratio of gas is controlled at 4 (Ar gas is 10-100sccm, O 2 5-50sccm), after the substrate temperature is heated to 200°C, the sputtering gas is introduced into the reaction chamber to the deposition chamber. The vertical distance between the material and the substrate is 100mm, and the thickness...

Embodiment 2

[0020] The silicon substrate (out-of-plane orientation (111) or (100)) was ultrasonically cleaned with acetone, ethanol and deionized water, then dried with a nitrogen gun, and immediately placed in the reaction chamber of the reactive magnetron sputtering device. Ensure that the absolute pressure of the back of the reaction chamber before deposition is lower than 5×10 -3 Pa. Use metal Fe and Al targets with a purity better than 99.99wt% as sputtering targets, high-purity Ar gas and O with a purity better than 99.99% 2 as the sputtering atmosphere. Ar and O 2 After the gas is fully mixed, it is introduced into the reaction chamber through the catheter, Ar gas and O 2 The flow ratio of gas is controlled at 8 (Ar gas is 10-50sccm, O 2 2-20sccm), after the substrate temperature is heated to 700°C, the sputtering gas is introduced into the reaction chamber to the deposition chamber. The vertical distance between the material and the substrate is 50mm, and the thickness of the...

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Abstract

The invention provides a preparation method of a high-efficiency composite catalyst film for overlength carbon nano tube growth; a silicon base is cleaned firstly and is dried by blowing, and then the silicon base is placed in a reaction chamber of a reaction magnetron sputtering device, before being deposited, the absolute pressure of the back bottom of the reaction chamber is lower than 5*10-3Pa; Fe and Mg targets are used as sputtering targets, or Fe and Al targets are adopted as sputtering targets, Ar and O2 are used as sputtering gas, and the flow ratio of the Ar and O2 is controlled between 1 and 10, after the temperature of the silicon base is heated to 200-700 DEG C, the sputtering gas is led in from the reaction chamber to a settling chamber, after the whole pressure intensity reaches 1-10Pa, sputtering film formation is carried out, the sputtering power is controlled between 40 and 100W, the vertical distance of the target and the substrate is 50-100mm, the deposited film thickness is controlled to be from 1 to 5nm; after the deposition is carried out, the temperature is cooled to be room temperature along with the furnace, a gas source is cut off, a finished product is taken out, so as to obtain Mg-Fe-O or Al-Fe-O catalyst film; the method can prepare the high-efficiency catalyst film in a large-area way, the efficiency is high, the cost is low, therefore, the preparation method is suitable for batch preparation of a carbon nano tube array.

Description

technical field [0001] The invention relates to a method for preparing a high-efficiency composite catalyst film for the rapid growth of ultra-long carbon nanotubes, belonging to the technical field of carbon nanotube preparation. Background technique [0002] Since their discovery in 1991, carbon nanotubes (CNTs) have attracted widespread attention due to their excellent physical and chemical properties. The preparation methods of CNTs include arc discharge, laser ablation, chemical vapor deposition (CVD), etc. Chemical vapor deposition (CVD) is low in cost and easy to form large-scale films, so it is widely used. Different kinds of CNTs materials can be obtained by CVD method, from powder to film, from single tube to tube array, from horizontal arrangement to vertical growth, etc. One of the key technologies for the CVD preparation of CNTs materials is the controllable preparation of nanocatalysts, in which the composition, size and activity of catalysts will play a decis...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/78B01J23/745B01J35/02C01B31/02C23C14/35C23C14/18C23C14/54C23C14/02B01J35/00
Inventor 李清文陈同来杨晓杰勇振中
Owner SUZHOU CREATIVE CARBON NANOTECH