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Method of preparing carbon nano tube by Ni/RE/Cu catalyst chemical gaseous phase sedimentation

A chemical vapor deposition, carbon nanotube technology, applied in chemical instruments and methods, single crystal growth, polycrystalline material growth and other directions, can solve the problem of unsuitable composite materials, and achieve uniform distribution, large output, and simple preparation.

Inactive Publication Date: 2007-01-31
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although Ni / Al 2 o 3 The development of carbon nanotubes as a catalyst is relatively mature, with high yield and high purity, but the obtained carbon tubes are not suitable for composite materials due to complicated purification steps.
However, using metal copper powder as a carrier to prepare catalysts, and then adopting CVD method to prepare carbon nanotubes, has not been reported in the literature at present.

Method used

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  • Method of preparing carbon nano tube by Ni/RE/Cu catalyst chemical gaseous phase sedimentation
  • Method of preparing carbon nano tube by Ni/RE/Cu catalyst chemical gaseous phase sedimentation

Examples

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Embodiment 1

[0017] Soak 8g of electrolytic copper powder in 30mL of absolute ethanol for 12 hours, mix with 7.926g of nickel nitrate hexahydrate and 1.723g of yttrium nitrate hexahydrate to make a 500mL aqueous solution, then make 2.721g of sodium hydroxide into a 150mL aqueous solution, and stir magnetically at room temperature Add dropwise to the above solution to obtain Ni(OH) 2 / Y(OH) 3 / Cu ternary colloid; the ternary colloid was washed with deionized water, filtered with filter paper, dehydrated and dried in a vacuum oven at 80°C, ground with an agate mortar, and calcined at 350°C for 2h under nitrogen protection to obtain Ni / Y / Cu catalyst precursor. Then take 0.5g Ni / Y / Cu catalyst precursor, raise the temperature to 500°C under the protection of nitrogen, stop the nitrogen, and pass in hydrogen for reduction. The flow rate of hydrogen is 200mL / min. Gas (nitrogen flow rate: 420mL / min, methane flow rate: 60mL / min) reacted for 1h, turned off the mixed gas, and cooled the furnace to...

Embodiment 2

[0019] Soak 17.8g of electrolytic copper powder in 30mL of absolute ethanol for several hours, and prepare 681mL of aqueous solution with 9.908g of nickel nitrate hexahydrate and 0.862g of yttrium nitrate hexahydrate, then prepare 784mL of aqueous solution with 2.906g of sodium hydroxide, and stir the Add dropwise to the above solution to obtain Ni(OH) 2 / Y(OH) 3 / Cu ternary colloid; the ternary colloid was washed and filtered, dehydrated and dried in a vacuum oven at 100°C, ground with an agate mortar, and calcined at 400°C under nitrogen protection for 2 hours to obtain a Ni / Y / Cu catalyst Precursor. Then take 0.5g of Ni / Y / Cu catalyst precursor, raise the temperature to 500°C under the protection of nitrogen, stop the nitrogen, pass in hydrogen for reduction, and the hydrogen flow rate is 100mL / min. After keeping for 2 hours, turn off the hydrogen and feed a mixed gas of nitrogen and methane (nitrogen flow rate 400mL / min, methane flow rate is 100mL / min) to react for 1h, tur...

Embodiment 3

[0021] Soak 8g of electrolytic copper powder in 30mL of absolute ethanol for several hours, and then prepare 500mL aqueous solution with 7.926g of nickel nitrate hexahydrate and 1.24g of cerium nitrate hexahydrate, and then prepare 300mL of aqueous solution with 2.523g of sodium hydroxide. Added dropwise to the above solution to obtain Ni(OH) 2 / Ce(OH) 3 / Cu ternary colloid; the ternary colloid was washed and filtered, dehydrated and dried in a vacuum oven at 150°C, ground with an agate mortar, and then the powder was first kept at 300°C for 2 hours under the protection of nitrogen and then continued to heat up to Calcined at 400°C for 2 hours to obtain a Ni / Ce / Cu catalyst precursor. Then take 0.5g of Ni / Y / Cu catalyst precursor, raise the temperature to 500°C under the protection of nitrogen, stop the nitrogen, pass in hydrogen for reduction, and the hydrogen flow rate is 100mL / min. After keeping for 2 hours, turn off the hydrogen and feed a mixed gas of nitrogen and methane...

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Abstract

The present invention discloses a method for preparing carbon nano tube by using Ni / RE / Cu catalyst and making chemical vapor deposition. Said method includes the following steps: adding nickelous nitrate hexahydrate, yttrium nitrate hexahydrate or cerous nitrate hexahydrate and soaked copper powder into deionized water according to a certain ratio to obtain nickelous nitrate solution; adding sodium hydroxide solution in the above-mentioned nickelous nitrate solution to neutralization reaction to obtain Ni(OH)2 / Y(OH)3 / Cu or Ni(OH)2 / Ce(OH)3 / Cu ternary colloid, washing, filtering, drying, grinding and calcining said ternary colloid to obtain Ni / Y / Cu or Ni / Ce / Cu catalyst precursor body, placing said precursor body into quartz reaction tube, introducing hydrogen gas to make reduction, then introducing mixed reaction gas to make catalytic fragmentation reaction to obtain mixed powder of carbon nano tube and catalyst, then using concentrated nitric acid to make treatment so as to obtain pure nano carbon tube.

Description

technical field [0001] The invention relates to a method for preparing carbon nanotubes by Ni / RE / Cu catalyst chemical vapor deposition. It belongs to the preparation technology of carbon nanotubes. Background technique [0002] Since their discovery in 1991, carbon nanotubes have attracted much attention for their unique and promising structural, electrical and mechanical properties. For example, carbon nanotubes can make their conductivity metallic, semi-metallic or semiconductive by changing the grid structure and diameter in carbon nanotubes. As a conductor, the conductivity of carbon nanotubes can be better than that of copper; the strength of carbon nanotubes It is about 100 times higher than steel, but its specific gravity is only 1 / 6 of that of steel. At the same time, carbon nanotubes are also extremely tough and soft, so they are considered to be the "super fiber" of the future. Therefore, carbon nanotubes can be widely used in high-density hydrogen storage materi...

Claims

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Application Information

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IPC IPC(8): C01B31/02C30B29/02C30B29/62
Inventor 赵乃勤康建立师春生杜希文李家俊
Owner TIANJIN UNIV