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A method for preparing phosphorus-rich copper phosphide hollow nanospheres

A hollow nano, phosphorus-rich technology, applied in the field of nano-materials and electrochemistry, can solve the problems of high energy consumption, unable to control the shape of copper phosphide, etc., to achieve uniform distribution, good safety and stability, equipment and instruments require simple effects

Active Publication Date: 2020-10-09
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, neither of these two methods can control the morphology of copper phosphide, and the energy consumption is high, and it is easy to introduce other impurity substances.

Method used

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  • A method for preparing phosphorus-rich copper phosphide hollow nanospheres
  • A method for preparing phosphorus-rich copper phosphide hollow nanospheres

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Effect test

Embodiment 1

[0026] 1) Cu(CH 3 COO) 2 ·H 2 O dissolved in ethanol solution to give Cu(CH 3 COO) 2 ·H 2 O concentration of 0.5mol / L Cu(CH 3 COO) 2 ·H 2 O ethanol solution, and then add Cu(CH 3 COO) 2 ·H 2 The pyrrole of O ethanol solution volume 0.5‰, stirs to form dark blue solution A;

[0027] 2) Place solution A in a polytetrafluoroethylene-lined stainless steel reactor at 200°C for a solvothermal reaction at a filling ratio of 70%, wash the product with absolute ethanol after the reaction, and then dry it in a freeze-drying box get the precursor;

[0028] 3) Put the precursor in a small porcelain boat of 3*6cm according to the molar ratio of precursor and red phosphorus at 1:1, put the red phosphorus in a large porcelain boat of 5*12cm, and then put the small porcelain boat into the large porcelain boat Inside the boat, cover and seal it, and then phosphating it at 400°C for 1 hour in a tube furnace with a vacuum degree of -0.1Mpa. After the reaction, the powder in the small...

Embodiment 2

[0030] 1) Cu(CH 3 COO) 2 ·H 2 O dissolved in ethanol solution to give Cu(CH 3 COO) 2 ·H 2 O concentration of 1mol / L Cu(CH 3 COO) 2 ·H 2 O ethanol solution, and then add Cu(CH 3 COO) 2 ·H 2 O ethanol solution volume 2‰ of pyrrole, stirred to form dark blue solution A;

[0031] 2) Place solution A in a polytetrafluoroethylene-lined stainless steel reactor at 190°C for solvothermal reaction at a filling ratio of 75%. After the reaction, the product is washed with absolute ethanol, and then dried in a freeze-drying box get the precursor;

[0032]3) According to the molar ratio of precursor and red phosphorus of 1:2, put the precursor in a small porcelain boat of 3*6cm, put the red phosphorus in a large porcelain boat of 5*12cm, and then put the small porcelain boat into the large porcelain boat In the boat, cover and seal it, and then phosphating reaction at 500°C for 2 hours in a tube furnace with a vacuum degree of -0.1Mpa. After the reaction, the powder in the small...

Embodiment 3

[0034] 1) Cu(CH 3 COO) 2 ·H 2 O dissolved in ethanol solution to give Cu(CH 3 COO) 2 ·H 2 O concentration of 2mol / L Cu(CH 3 COO) 2 ·H 2 O ethanol solution, and then add Cu(CH 3 COO) 2 ·H 2 O ethanol solution volume 3‰ of pyrrole, stirred to form dark blue solution A;

[0035] 2) Place solution A in a polytetrafluoroethylene-lined stainless steel reactor at 180°C for solvothermal reaction at a filling ratio of 80%, wash the product with absolute ethanol after the reaction, and then dry it in a freeze-drying box get the precursor;

[0036] 3) According to the molar ratio of precursor and red phosphorus of 1:4, put the precursor in a small porcelain boat of 3*6cm, put the red phosphorus in a large porcelain boat of 5*12cm, and then put the small porcelain boat into the large porcelain boat Inside the boat, cover and seal it, and then phosphating reaction at 800°C for 4 hours in a tube furnace with a vacuum degree of -0.1Mpa. After the reaction, the powder in the small...

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Abstract

The invention relates to a method for preparing a phosphorus-rich copper phosphide hollow nanosphere. The method comprises the following steps: dissolving Cu(CH3COO)2.H2O in an ethanol solution whilestirring, and then adding pyrrole and stirring, thereby acquiring a dark blue solution A; placing the solution A into a reaction kettle for solvothermal reaction, using absolute ethyl alcohol for washing the product after the ending of reaction, and then placing into a freeze-drying box for drying, thereby acquiring a precursor; placing the precursor into a small porcelain boat, placing red phosphorus into a big porcelain boat, sleeving the small porcelain boat into the big porcelain boat, covering and sealing, and then triggering phosphating reaction in a vacuum tube furnace; after ending thereaction, acquiring powder in the small porcelain boat, namely, the phosphorus-rich copper phosphide hollow nanosphere. The prepared phosphorus-rich copper phosphide hollow nanosphere can be used asa cathode material of lithium ion batteries or sodium-ion batteries and an electro-catalysis electrode material. In the phosphating reaction adopted by the invention, the phosphorus diffuses from outer to inner, and meanwhile, the oxide precursor also diffuses from inner to outer, and a solid sphere is converted into a hollow sphere under the coaction of the two processes.

Description

technical field [0001] The invention relates to the fields of nanomaterials and electrochemistry, in particular to a method for preparing phosphorus-rich copper phosphide hollow nanospheres. Background technique [0002] Transition metal phosphides have a wide range of applications in the fields of magnetism, optics, and energy storage. The polyphosphide anions are formed by direct P-P bonding, and transition metal phosphides exist in phases with different phosphorus contents such as metal-rich and phosphorus-rich. Among many phosphides, phosphorus-rich phase copper phosphide (CuP 2 ) is a potential material for Li / Na-ion batteries with a theoretical specific capacity as high as 1281mAh g -1 , has a very attractive application prospect. However, like other electrode materials based on the conversion reaction mechanism, there is a huge volume change in the process of lithium / sodium storage, and the hollow structure can effectively alleviate the volume change effect of the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/08
CPCC01B25/08C01P2002/72C01P2004/03C01P2004/34C01P2004/62
Inventor 曹丽云王勇黄剑锋寇领江李嘉胤
Owner SHAANXI UNIV OF SCI & TECH