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Method for preparation of copper nanocubes utilizing tributylphosphine as a ligand

A tributylphosphine, copper nanotechnology, applied in nanotechnology, chemical instruments and methods, metal processing equipment and other directions, can solve problems such as unclear formation mechanism

Active Publication Date: 2021-02-02
HONDA MOTOR CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, their formation mechanism is unclear and the reproducibility of copper nanocube formation needs to be improved

Method used

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  • Method for preparation of copper nanocubes utilizing tributylphosphine as a ligand
  • Method for preparation of copper nanocubes utilizing tributylphosphine as a ligand
  • Method for preparation of copper nanocubes utilizing tributylphosphine as a ligand

Examples

Experimental program
Comparison scheme
Effect test

Embodiment I

[0056] Embodiment 1: the preparation of Cu-TDA precursor complex solution

[0057] Copper chloride (99.0%), tributylphosphine (TBP, 99%), trioctylphosphine (TOP, 97%), oleylamine (OLA, 70%), toluene (99.9%), acetone (99%) and chloroform (99.9%) and 1-octadecene (ODE, 98%) were purchased from Sigma-Aldrich. Tetradecylamine (TDA, >96%) was purchased from Tokyo Chemical Industry Co., Ltd. (TCI). Hexane (99%), methanol (99%) and ethanol (200 proof) were purchased from Fisher Chemicals. All chemicals were used as received unless otherwise stated.

[0058] in Ar or N 2 100 mg of copper(I) chloride (1.0 mmol), 240 mg of TDA and 2 mL of ODE were added to the flask under flow. in Ar or N 2 After purging for 20 minutes, the mixed solution was heated to 200° C. and kept at this temperature for 10 minutes. The amount of copper(I) chloride was varied from 50 mg to 600 mg, while the amounts of TDA and TBP were increased from 120 mg to 1.44 g and from 0.5 mL to 6.0 mL, respectively. ...

Embodiment II

[0059] Example II: Synthesis of Cu nanocubes

[0060] 6.0 mL of oleylamine (OLA, 70%) was loaded into a 25 mL three-necked flask, where oxygen was removed by Ar purging for 20 min. 1.0 mL of tributylphosphine (TBP, 4.0 mmol) was injected into the flask under Ar flow. After 20 minutes of Ar flow, the flask was placed in a heating mantle with a temperature controller and rapidly heated to 300°C at a heating rate of 15-25°C / min. Next, 2 mL of Cu-TDA complex solution was quickly injected into the heated flask and the reaction solution turned red. The reaction was held at 300°C for 30 minutes. The reaction solution was then naturally cooled to room temperature, and injected with 5 mL of hexane (or another hydrophobic solvent such as toluene and chloroform). The product was isolated by centrifugation at 8000 rpm for 5 minutes. Discard the supernatant. Then 10 mL of hexane was added to the precipitate, and the mixture was centrifuged at 8000 rpm for 5 minutes. This washing pr...

Embodiment III

[0061] Example III: Synthesis of Cu nanosheets

[0062] 6.0 mL of OLA (70%) was loaded into a 25 mL three-neck flask, where oxygen was removed by Ar purging for 20 minutes. Then 1.0 mL of TOP (97%) was injected into the flask under Ar flow. After 20 minutes of Ar flow, the flask was rapidly heated to 300°C. Next, 2 mL of Cu-TDA complex solution was quickly injected into the heated flask and the reaction solution turned red. The reaction was held at 300°C for 3 minutes (at least less than 5 minutes). The reaction solution was then cooled to room temperature and injected with 5 mL of hexane (or another hydrophobic solvent such as toluene and chloroform). The product was isolated by centrifugation at 10000 rpm for 5 minutes. Discard the supernatant. Then 5 mL of hexane was added to the precipitate, and the mixture was centrifuged at 10000 rpm for 5 minutes. Repeat the washing procedure twice to remove unreacted precursors and surfactants. Two-dimensional Cu nanosheets wi...

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Abstract

The title of the invention is method for preparation of copper nanocubes utilizing tributylphosphine as a ligand. A method for preparing copper nanocubes with specific facets and uniform size, the method comprising combining a copper complex solution in a reaction mixture with a ligand. Using a ligand of pure, unoxidized tributylphosphine, uniform copper nanocubes with six facets are prepared.

Description

technical field [0001] The present disclosure relates to methods for preparing copper nanocubes. Background technique [0002] The reduction of carbon dioxide using various catalysts has received great attention due to the potential to produce fuels and chemicals in a sustainable manner. Considering global warming, carbon dioxide has attracted attention as a renewable resource. Metallic nanostructures with various features have shown excellent catalytic performance for the carbon dioxide reduction reaction. Using copper nanostructures, the reduction of carbon dioxide can be used to produce a variety of chemical products, and the nanostructured surface can affect various aspects of the catalytic process. The structure of the various copper nanocubes can vary depending on the methods and conditions used for production. Therefore, specific methods for producing copper nanocubes have attracted attention due to the potential ability to tailor subsequent catalytic reactions usi...

Claims

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Application Information

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IPC IPC(8): B22F9/24B22F1/00B01J35/00B01J23/72B82Y40/00B22F1/054
CPCB22F9/24B01J23/72B82Y40/00B22F1/07B22F1/054B22F1/0547B22F1/0553B01J35/33B22F2304/054B22F2301/10
Inventor 陈顾刚陈书堂
Owner HONDA MOTOR CO LTD
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