Method for high-efficiency purification of single-wall carbon nanotubes prepared by chemical vapor deposition

A single-wall carbon nanotube, chemical vapor deposition technology, applied in nanotechnology, nanotechnology, nanostructure manufacturing and other directions, can solve the problem of purification yield and purity can not be guaranteed at the same time, to ensure purity and yield, easy to expand Effect

Active Publication Date: 2012-04-04
唯碳纳米科技(沈阳)有限公司
View PDF1 Cites 11 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a universal and efficient method for purifying single-walled carbon nanotubes prepared by chemical vapor deposition, which does not destroy the intrinsic structure of single-walled carbon nanotubes, and solves the current problem of different conditions and different batches. In the purification method of single-walled carbon nanotubes prepared by chemical vapor deposition, the purification yield and purity cannot be guaranteed at the same time.
[0005] In addition, the present invention also solves the bottleneck problem that currently restricts the industrial application of single-walled carbon nanotubes

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for high-efficiency purification of single-wall carbon nanotubes prepared by chemical vapor deposition
  • Method for high-efficiency purification of single-wall carbon nanotubes prepared by chemical vapor deposition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 3 mg of single-walled carbon nanotube samples prepared by floating catalyst vapor deposition method (reaction temperature 1000° C., using ferrocene as catalyst, 200 ml / min hydrogen as carrier gas, and 4 ml / min methane as carbon source). , the specifications of single-walled carbon nanotubes are as follows: diameter distribution: 0.8-3.0nm, purity: 30wt%, anti-oxidation temperature: 460°C.

[0026] The thermogravimetric / differential thermal analysis experiment is carried out under the air atmosphere, and the obtained thermogravimetric / differential thermal curve is as follows figure 1 (a) shown. According to the thermogravimetric curve, the concentrated oxidation temperature of amorphous carbon is 350-370°C, and the weight percentages of amorphous carbon, catalyst particles and single-walled carbon nanotubes are 5%, 65% and 30% respectively. 20 mg of the above-mentioned single-walled carbon nanotube sample was evenly placed in a horizontal heating furnace tube with ...

Embodiment 2

[0028] Get the single-walled carbon nanotube sample 1g that utilizes the floating catalyst vapor deposition method of embodiment 1 (reaction temperature 1100 ℃, take ferrocene as catalyst, 200ml / min hydrogen as carrier gas, 4ml / min methane as carbon source), Evenly place it in a horizontal heating furnace tube with an inner diameter of 45mm and a constant temperature zone length of 10cm, pass in 1000ml / min of air, and oxidize at 370°C for 20h. After the sample was cooled to room temperature, it was taken out and soaked in hydrochloric acid solution (concentration: 20wt%) and washed at 80°C for several times until the hydrochloric acid solution no longer changed color. Wash the sample with deionized water until the pH is 7, dry the sample in vacuum at 120° C. for 5 hours, take it out after cooling, and weigh it. The weight of the sample is 0.28 g. Take 3 mg of the purified single-walled carbon nanotube sample, and carry out the thermogravimetric / differential thermal analysis ex...

Embodiment 3

[0030] 3 mg of purchased single-walled carbon nanotubes prepared by the Hipco method. In this embodiment, the specifications of the single-walled carbon nanotubes are as follows: the diameter distribution is 0.6-1.3nm, the purity is 95wt%, and the oxidation resistance temperature is 500°C.

[0031] Carry out thermogravimetric / differential thermal analysis experiment under air atmosphere, according to this thermogravimetric curve qualitatively draw the temperature that the concentrated oxidation of amorphous carbon is 350 ℃, wherein the weight percent of amorphous carbon and single-walled carbon nanotube is 2%, respectively. 95%, and the rest are catalyst particles accounting for 3%. Put 50 mg of the above-mentioned single-walled carbon nanotube sample evenly in a horizontal heating furnace tube with an inner diameter of 22 mm and a constant temperature zone length of 4 cm, pass air at 100 ml / min, and oxidize at 325 ° C for 10 h. After the sample was cooled to room temperature,...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
diameteraaaaaaaaaa
diameteraaaaaaaaaa
anti-oxidation temperatureaaaaaaaaaa
Login to view more

Abstract

The invention relates to the field of single-wall carbon nanotubes, and specifically, relates to a method for high-efficiency purification of single-wall carbon nanotubes prepared by chemical vapor deposition. The method has high efficiency, is simple and is suitable for industrialization. The method comprises the following steps of uniformly placing single-wall carbon nanotubes prepared by chemical vapor deposition in a horizontal heating furnace, carrying out oxidation in an air atmosphere at an amorphous carbon rapid oxidation temperature for 5 to 20 hours, immersing the oxidized single-wall carbon nanotubes in a hydrochloric acid solution to remove catalyst particles, cleaning the single-wall carbon nanotubes treated by the previous step by deionized water multiple times, and drying to obtain a purified single-wall carbon nanotube sample. The method is simple, is suitable for large-scale industrialized production and purification of single-wall carbon nanotubes or multi-wall carbon nanotubes prepared by chemical vapor deposition, and has important industrial application prospects. The method can determine a sample oxidation temperature through a thermogravimetric / differential thermal analysis experiment and thus solving the problem that because carbon nanotubes prepared by the existing chemical vapor deposition under different conditions and carbon nanotubes which have different production batch numbers and are prepared under the same conditions are different in inoxidizability, purification purity and a yield cannot be controlled accurately.

Description

technical field [0001] The invention relates to the field of single-wall carbon nanotubes, in particular to an efficient, simple and industrializable purification method for single-wall carbon nanotubes prepared by chemical vapor deposition. Background technique [0002] Since their discovery in 1993, single-walled carbon nanotubes have unique physical and chemical properties and excellent electrical and mechanical properties due to their unique structure. They have broad application prospects in the fields of nanoelectronic components, field emission, and composite materials. All these attractive application prospects are based on the premise of obtaining high-purity, large-scale, and cheap single-walled carbon nanotubes. Among the three traditional methods for preparing single-walled carbon nanotubes (chemical vapor deposition, arc method, and laser evaporation method), chemical vapor deposition is favored by people because of its simplicity, large amount, low cost and sca...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82B3/00
Inventor 侯鹏翔于冰刘畅成会明
Owner 唯碳纳米科技(沈阳)有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap