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Method for direct growth of porous carbon nanotubes on nano-porous copper

A technology of nanoporous copper and porous carbon, applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of multiple by-products, complicated operation, low yield, etc., and achieve simple preparation process and equipment requirements, high purity High, high yield effect

Inactive Publication Date: 2016-06-08
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although various technological methods have made great progress, there are still shortcomings of complex operation and low yield, and more by-products are easily mixed in the product, so it is still a challenge to uniformly prepare a large amount of high-purity carbon nanotubes. Important and Urgent Issues
[0004] After searching, it is not found that there are only nanoporous copper as a template and a catalyst, and a large number of porous carbon nanotubes are synthesized in one step by chemical vapor deposition (CVD) Report papers or patent reports

Method used

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  • Method for direct growth of porous carbon nanotubes on nano-porous copper
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  • Method for direct growth of porous carbon nanotubes on nano-porous copper

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Cu with a length of 20 mm, a width of 5 mm, and a thickness of 30 μm 30 mn 70 After the alloy strip is cleaned and dried with deionized water, it is placed in a dilute hydrochloric acid solution with a concentration of 0.02mol / L for dealloying corrosion, and the sample is taken out when there are basically no bubbles overflowing;

[0018] Wash with deionized water until neutral, and the number of cleanings is 3 times, then put the sample into a vacuum drying oven and dry at room temperature for 3 hours to obtain a nanoporous copper (NPC) precursor with a microstructure such as figure 2 shown in;

[0019] Put the obtained nanoporous copper catalyst precursor into a quartz boat, place it in the constant temperature zone of the tube furnace, and raise the temperature to 630°C at 10°C / min under an argon atmosphere with a flow rate of 100sccm;

[0020] Then pass hydrogen reduction annealing at a flow rate of 100 sccm for 0.5 h;

[0021] Then stop feeding hydrogen, and th...

Embodiment 2

[0026] Cu with a length of 20 mm, a width of 5 mm, and a thickness of 30 μm 30 mn 70 After the alloy strip is cleaned and dried with deionized water, it is placed in a dilute hydrochloric acid solution with a concentration of 0.02mol / L for dealloying corrosion, and the sample is taken out when there are basically no bubbles overflowing;

[0027] Wash with deionized water to neutrality, and the number of cleanings is 5 times, then put the sample into a vacuum drying oven and dry at room temperature for 3 hours to obtain a nanoporous copper catalyst precursor (NPC);

[0028] Put the obtained nanoporous copper catalyst precursor into a quartz boat, place it in the constant temperature zone of the tube furnace, and raise the temperature to 630°C at 10°C / min under an argon atmosphere with a flow rate of 100sccm;

[0029] Then pass hydrogen reduction annealing at a flow rate of 100 sccm for 0.5 h;

[0030] Afterwards, stop feeding hydrogen, and feed a mixture of acetylene and 200 ...

Embodiment 3

[0034] Cu with a length of 20 mm, a width of 5 mm, and a thickness of 30 μm 30 mn 70 After the alloy strip is cleaned and dried with deionized water, it is placed in a dilute hydrochloric acid solution with a concentration of 0.02mol / L for dealloying corrosion, and the sample is taken out when there are basically no bubbles overflowing;

[0035] Wash with deionized water to neutrality, and the number of cleanings is 4 times, and then put the sample into a vacuum drying oven to dry at room temperature for 3 hours to obtain a nanoporous copper catalyst precursor (NPC);

[0036] Put the obtained nanoporous copper catalyst precursor into a quartz boat, place it in the constant temperature zone of the tube furnace, and raise the temperature to 650°C at 10°C / min under an argon atmosphere with a flow rate of 100sccm;

[0037] Then pass hydrogen reduction annealing at a flow rate of 100 sccm for 0.5 h;

[0038] Afterwards, stop feeding the hydrogen, and feed the mixed gas of acetyle...

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Abstract

The present invention relates to a method for direct growth of porous carbon nanotubes on the nano-porous copper. The method comprises the steps of: (1) preparation of a nano-porous copper catalyst precursor: rinsing a Cu30Mn70 alloy strip with thickness of 20-50 mum with deionized water, drying, placing the alloy strip in dilute hydrochloric acid solution with concentration of 0.001-0.02 mol / L for dealloying etching and taking out the sample until no bubble overflow; rinsing with deionized water; then placing the alloy strip in a vacuum oven and drying at room temperature; (2) preparation of a porous carbon nanotube: placing the nano-porous copper catalyst precursor into a quartz ark, placing the quartz ark in a constant-temperature area of a tube furnace, and heating to 600-800 DEG C in argon atmosphere with flow of 50-100 sccm under a heating rate of 2-10 DEG C / min; introducing hydrogen with flow of 50-100 sccm, reducing and annealing for 0.5-2 h; closing the hydrogen, introducing a mixed gas of acetylene and argon in the volume ratio of 1:(10-30) for growing for 0.2-1 h; cooling to 200-300 DEG C in an argon atmosphere with flow of 50-100 sccm at a cooling rate of 2-10 DEG C / min; and cooling to room temperature with the furnace and taking out the finished product.

Description

technical field [0001] The invention belongs to the technical field of carbon nanometer materials, in particular to a method for directly growing porous carbon nanotubes on nanoporous copper. Background technique [0002] Since the beginning, carbon nanotubes have always had great potential application prospects in electronic energy storage devices, hydrogen storage materials, etc. due to their unique structure, excellent thermodynamic and electrical characteristics, especially their unique crystalline structure is very suitable for use As a catalyst support material, it has received more and more attention from the scientific community. Carbon nanotubes can be divided into single-walled and multi-walled according to the number of flake graphite layers. Single-walled carbon nanotubes can be regarded as a single-layer flake graphite curled structure with good symmetry and unity. Multi-walled carbon nanotubes can be understood as a set of single-walled carbon nanotubes of dif...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82Y30/00B01J23/72B01J35/10
CPCB82Y30/00B01J23/72C01P2004/03C01P2004/62C01P2006/12C01P2006/80B01J35/60
Inventor 康建立邹程雄于镇洋张志佳乔志军
Owner TIANJIN POLYTECHNIC UNIV