Preparation method for synthesizing carbon nanotubes in quantity and with low cost

A technology for synthesizing carbon and nanotubes, applied in nanotechnology and other directions, can solve the problems of complex process, limited engineering application, high energy consumption, etc., and achieve the effect of simple preparation process, easy implementation of conditions, and time saving.

Inactive Publication Date: 2012-11-28
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of preparing carbon nanotubes, the catalyst plays a very important role. In the past research, people have developed many catalyst preparation processes, among which the sol-gel method is the most typical, but the sol-gel method is complicated and requires Heat treatment, long preparation cycle, high energy consumption
On the other hand, the traditional CVD preparation method still has problems such as long synthesis time and low yield.
[0003] Due to the above reasons, carbon nanotubes, which have amazing properties and may be widely used, are limited in engineering applications due to high preparation costs.

Method used

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  • Preparation method for synthesizing carbon nanotubes in quantity and with low cost
  • Preparation method for synthesizing carbon nanotubes in quantity and with low cost
  • Preparation method for synthesizing carbon nanotubes in quantity and with low cost

Examples

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preparation example Construction

[0014] The steps of the preparation method for low-cost mass synthesis of carbon nanotubes are as follows:

[0015] 1) At room temperature, put nickel foam in an electronic universal testing machine, compact it with a pressure of 3.6MPa, cut it into several pieces of 20mm×40mm or 20mm×60mm in size, put it into an ultrasonic cleaner and clean it with ethanol , then wash it several times with deionized water and dry it; heat the plating solution containing the metal catalyst to 80-90°C, put the cleaned foamed nickel into the plating solution, and plate for 20-30 minutes. Enter into baking oven and dry, obtain the nickel foam sample that contains metal catalyst;

[0016] 2) Place the sample of 20mm×40mm or 20mm×60mm containing metal catalyst nickel foam horizontally or vertically in the quartz boat, push the quartz boat into the quartz tube of the horizontal resistance furnace, and inject nitrogen gas with a flow rate of 200ml / min, When the temperature reaches 650°C, lower the f...

Embodiment 1

[0024] Take a 20×40mm nickel foam and weigh it as 235mg, put it into the plating solution heated to 80°C, put it into the oven for 30 minutes after plating, and dry it in an oven, and weigh it as 265mg.

[0025] Place the nickel foam sample crossing the iron horizontally in a quartz boat, heat it with an ordinary horizontal resistance furnace, and feed in N at a flow rate of 200ml / min. 2 Degas the quartz tube. When the temperature reaches 650°C, turn down the N 2 The flow rate reaches 50ml / min, and 50ml / min of H 2 Restore for 10 minutes. When the temperature reaches 690°C, feed 50ml / min of C 2 h 2 , adjust H 2 The flow is closed after 30 minutes of reaction at 50 ml / min C 2 h 2 and H 2 Valve. Increase N 2 The flow rate is up to 200ml / min. Turn off N when the temperature drops to 300°C 2 valve, after the furnace is cooled to room temperature, the quartz boat is taken out, and the total weight of the product to be obtained is 980mg. The SEM photograph of the product ...

Embodiment 2

[0027] Take a piece of 20×40mm nickel foam and weigh it as 235mg, put it into the plating solution heated to 90°C, put it into the oven for 20 minutes after plating, and dry it in an oven, and weigh it as 250mg.

[0028] Place the nickel foam sample crossing the iron horizontally in a quartz boat, heat it with an ordinary horizontal resistance furnace, and feed in N at a flow rate of 200ml / min. 2 Degas the quartz tube. When the temperature reaches 650°C, turn down the N 2 The flow rate reaches 50ml / min, and 50ml / min of H 2 Reduce for 10 minutes, when the temperature reaches 700°C, feed 100ml / min of C 2 h 2 , turn off C after 30 minutes of reaction 2 h 2 Valve, increase N 2 The flow rate is up to 200ml / min. Turn off N when the temperature drops to 300°C 2 Valve, after the furnace is cooled to room temperature, the quartz boat is taken out, and the total weight of the product that can be obtained is 1690mg. The product is a carbon nanotube, and its SEM picture is as fol...

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Abstract

The invention discloses a preparation method for synthesizing carbon nanotubes in quantity and with low cost. The method comprises the following steps of: plating and coating nano-grade metal catalysts such as iron, cobalt, molybdenum and the like on foamed nickel by a chemical plating process; placing the foamed nickel plated with the catalysts into a quartz boat; heating the foamed nickel plated with the catalysts by using the common horizontal resistance furnace; introducing nitrogen with flow of 200 ml / min to remove air from a quartz tube; when the temperature reaches 650 DEG C, introducing hydrogen with flow of 50 ml / min to reduce the metal catalysts for 10 minutes; when the temperature reaches 690 to 720 DEG C, introducing acetylene gas with flow of 50 to 100 ml / min, wherein the hydrogen flow can be set to be 25 to 100 ml / min; closing an acetylene valve and a hydrogen valve after the reaction is performed for 30 minutes; introducing nitrogen with the flow of 20 ml / min; when the temperature is reduced to 300 DEG C, closing a nitrogen valve; and after the hearth is cooled to room temperature, taking out the quartz boat, wherein black products are found to be generated on the foamed nickel and are the carbon nanotubes according to electron microscope and Raman spectrum detection. By the method, the preparation process is simple; energy consumption is small; cost is low; time is saved; and preparation conditions are easy to implement.

Description

technical field [0001] The invention relates to a preparation method for synthesizing carbon nanotubes in large quantities at low cost. Background technique [0002] Due to its unique structure and excellent electrical, optical, mechanical, and thermal properties, carbon nanotubes have broad application prospects in various fields such as materials, machinery, electronics, and energy. At present, the methods for preparing carbon nanotubes mainly include arc discharge method and chemical vapor deposition method. Among them, chemical vapor deposition (chemical vapor deposition, CVD) is currently the most popular and widely used preparation method, using transition metals Fe, Co, Ni, etc. as catalysts, with low growth temperature, strong controllability and easy realization. Large-scale production and other characteristics, this method is mainly used in the preparation of multi-walled carbon nanotubes. In the process of preparing carbon nanotubes, the catalyst plays a very im...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/02B82Y40/00
Inventor 王淼张国俊李振华韩立静刘丽芳宋萌顾智企王宏涛
Owner ZHEJIANG UNIV
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