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A kind of preparation method of nano copper phosphide

A phosphide, nano-copper technology, applied in phosphide, nanotechnology, nanotechnology and other directions, can solve the problems of complex raw materials, cumbersome process, difficult to obtain nanometer size, etc., to achieve good particle uniformity, easy to obtain raw materials, good circulation The effect of stability

Active Publication Date: 2016-09-28
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the above defects or improvement needs of the prior art, the present invention provides a method for preparing nano-copper phosphide, the purpose of which is to use a preparation method with simple process and controllable cost to react phosphorus and copper at a certain temperature to directly obtain nano Copper phosphide of the largest size, thereby solving the technical problems of the existing preparation method of copper phosphide, which are cumbersome, complicated raw materials and difficult to obtain nanometer size

Method used

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  • A kind of preparation method of nano copper phosphide
  • A kind of preparation method of nano copper phosphide
  • A kind of preparation method of nano copper phosphide

Examples

Experimental program
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Effect test

Embodiment 1

[0032] S1: red phosphorus powder obtained by ball milling red phosphorus with a purity of 98% for 6 hours, wherein the red phosphorus was purchased from Sinopharm. The copper mesh is also purchased from Sinopharm Group, the copper mesh is surface treated with hydrochloric acid, pickled to remove oxides on the surface of the copper mesh and make it clean, and the copper mesh and red phosphorus powder are sealed in a stainless steel tank filled with inert gas . Wherein, the red phosphorus mass is 0.1 to the copper mesh mass, and the volume of the stainless steel tank is 50ml.

[0033] S2: Sinter the stainless steel tank sealed with red phosphorus and copper mesh in step S1 in a muffle furnace, the sintering temperature is 450°C, the sintering time is 1h, and Cu with a particle size of about 120nm is obtained. 3 p.

[0034] figure 1 It is the XRD curve figure of the copper phosphide of the present embodiment, as can be seen from this figure, the main component of the synthetic...

Embodiment 2

[0036] S1: red phosphorus powder obtained by ball milling red phosphorus with a purity of 99% for 12 hours, wherein the red phosphorus was purchased from Sinopharm. The copper mesh is purchased from Sinopharm Group. The surface of the copper mesh is treated with hydrochloric acid, and the oxide on the surface of the copper mesh is removed and cleaned by pickling. The copper mesh and red phosphorus powder are sealed in a stainless steel tank filled with inert gas. Wherein, the red phosphorus mass is 0.3 to the copper mesh mass, and the volume of the stainless steel tank is 50ml.

[0037] S2: The stainless steel tank sealed with red phosphorus and copper mesh in step S1 is sintered in a muffle furnace, the sintering temperature is 350° C., and the sintering time is 6 hours.

[0038] figure 2 (a), (b) are the present embodiment copper phosphide Cu 3 SEM image of P, figure 2 (a) The magnification is 290 times, figure 2 (b) The magnification is 2323 times. It can be seen fr...

Embodiment 3

[0040] S1: red phosphorus powder obtained by ball milling red phosphorus with a purity of 98.5% for 24 hours, wherein the red phosphorus was purchased from Sinopharm. The copper mesh is purchased from Sinopharm Group. The surface of the copper mesh is treated with hydrochloric acid, and the oxide on the surface of the copper mesh is removed and cleaned by pickling. The copper mesh and red phosphorus powder are sealed in a stainless steel tank filled with inert gas. Wherein, the red phosphorus mass is 0.5 to the copper mesh mass, and the volume of the stainless steel tank is 50ml.

[0041] S2: The stainless steel tank sealed with red phosphorus and copper mesh in step S1 is sintered in a muffle furnace, the sintering temperature is 250° C., and the sintering time is 10 h.

[0042] image 3 It is the scanning electron micrograph of the copper phosphide of this embodiment, and the magnification of this figure is 1500 times. It can be seen from the figure that the synthesized Cu ...

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Abstract

The invention discloses a preparation method of nano cuprous phosphide / copper phosphide. The preparation method comprises the following steps: step one, sealing red phosphorus with a purity of 98% or more and a copper screen with a processed surface into a container full of inert gas; step two, sintering the container mentioned in the step one for 1 to 10 hours at a sintering temperature of 250 to 450 DEG C so as to obtain the cuprous phosphide with a nano-level size. When the weight ratio of red phosphorus to copper screen is 0.1 to 0.5, cuprous phosphide (Cu3P) can be obtained. When the weight ratio of red phosphorus to copper screen is 0.51 to 1.5, copper phosphide (Cu3P2) will be obtained. The preparation method has the advantages of simple process, easily-available and cheap raw materials, and low requirements on equipment. The obtained nano-sized cuprous phosphide / copper phosphide has a good particle uniformity and excellent electrochemical performance in the field of sodium ion battery.

Description

technical field [0001] The invention belongs to the field of transition metal phosphides, and in particular relates to a preparation method of nanometer copper phosphides. Background technique [0002] Transition metal phosphides are a general term for binary or multi-component compounds formed by metals and phosphorus. The chemical bonds in the formed phosphides are different for different metal elements, which can be ionic, metallic and covalent. Metal phosphides have a special bonding structure and have both metal and semiconductor properties, and have many important applications in the fields of catalysis and electrochemistry. Amorphous Ni 2 P. Co. 2 P exhibits unique activity in the hydrodesulfurization and hydrodenitrogenation refining processes of gasoline and diesel oil; studies have shown that Sn 3 P 4 It shows good performance in sodium-ion secondary batteries, with a capacity of 465mA h / g after 100mA / g discharge for 100 cycles; the study also found that NiP ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/08H01M4/58B82Y40/00B82Y30/00
CPCY02E60/10
Inventor 张五星段建黄云辉
Owner HUAZHONG UNIV OF SCI & TECH
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