Method for synthesizing black phosphate on carbon paper by one-step method and application of method

A technology of carbon paper and black phosphorus, applied in chemical instruments and methods, electrical components, electrochemical generators, etc., can solve the problems of high catalyst, low output, environmental pollution, etc., and achieve good electrochemical performance, small particles, good reversible effect

Inactive Publication Date: 2017-11-17
QINGDAO UNIV
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AI-Extracted Technical Summary

Problems solved by technology

At present, the commonly used preparation method of black phosphorus is still the preparation method of high temperature and high pressure. Although black phosphorus can be successfully prepared, the output is relatively low, and the requi...
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Abstract

The invention relates to a method for synthesizing black phosphate on carbon paper by a one-step method and application of the method. The method mainly comprises the following steps of weighing a phosphate source, annealing and drying the phosphate source, taking a certain amount of a phosphate source precursor, uniformly placing the phosphate source precursor in a magnetic boat, arranging empty carbon paper on the magnetic boat, introducing a protection gas, rising a temperature at an uniform speed, performing heating, reducing the temperature to a room temperature at the uniform speed, and obtaining the black phosphate on the carbon paper. The black phosphate on the carbon paper is synthesized by a vapor deposition method, and the detects of high energy consumption caused by high temperature, high requirement on equipment, a special catalyst needed, relatively long synthesis time and the like in a traditional industrial high-temperature solid-phase synthesis method are overcome; moreover, the preparation method has the characteristics of simplicity, low cost and the like, is convenient to operate and is beneficial for industrial production; and through electrochemical performance and oxygen precipitation test, it is found out that the black phosphate on the carbon paper, synthesized by the method, has the advantages of high initial specific capacity, good cycle property and high-efficiency oxygen precipitation, and thus, the method is friendly to an application environment and is wide in market prospect.

Application Domain

Technology Topic

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  • Method for synthesizing black phosphate on carbon paper by one-step method and application of method
  • Method for synthesizing black phosphate on carbon paper by one-step method and application of method
  • Method for synthesizing black phosphate on carbon paper by one-step method and application of method

Examples

  • Experimental program(3)

Example Embodiment

[0022] Example 1:
[0023] A one-step method for synthesizing black phosphorus on carbon paper and its application specifically include the following steps:
[0024] S1. Weigh 5.0g of red phosphorus and evenly put it into the quartz boat, then put the quartz boat into the tube furnace, and then pass the argon protective gas into the tube furnace; heat the tube furnace to 180℃ at a constant speed, and heat 4h, perform annealing treatment;
[0025] S2, after annealing, prepare annealed samples, and cool them to room temperature for later use;
[0026] S3. Transfer the sample of S2 to a mortar and grind it for 40 minutes to obtain the required precursor red phosphorus for later use;
[0027] S4. Weigh 0.5g of the precursor red phosphorus prepared in S3, and evenly put it into the quartz boat, then put the blank carbon paper on the quartz boat, and then transfer it to the middle of the tube furnace;
[0028] S5. Pass the protective gas argon into the tube furnace, strictly control the flow rate of argon to 4sccm, heat the tube furnace to 500℃ at a constant rate, keep it for 3h, then lower the temperature to 350℃, and keep it for 3h. Black phosphorous material on carbon paper.
[0029] The black phosphorus on carbon paper prepared in this embodiment can be applied to the field of lithium ion battery cathode materials and oxygen evolution (OER). figure 1 The first discharge curve obtained from the test of the black phosphorus assembled battery on the carbon paper prepared in the example, from figure 1 It can be seen that there is an obvious discharge platform at 0.78V, which indicates that the black phosphorous material on carbon paper has good reversibility at 0.78V platform; figure 1 It can also be seen that the first discharge specific capacity of the black phosphorous cathode material on the carbon paper synthesized in this example is 2234.5mAh·g -1 , Which proves that the material prepared in this example has good electrochemical performance; figure 2 The cycle performance curve of the battery assembled with black phosphorus on the carbon paper prepared in this example, from figure 2 It can be seen that the first specific capacity of the black phosphorous cathode material on the carbon paper prepared in this example is 2234.1mAh·g -1 After 200 cycles of charge and discharge, the specific capacity can still reach 1677.3mAh·g -1 , The capacity retention rate after 200 cycles is 75.14%, indicating that the cycle performance of the black phosphorous cathode material on the prepared carbon paper is relatively stable; image 3 The linear curve of the precipitation of black phosphorous oxygen on the carbon paper prepared in this example, it can be seen from the figure that the overpotential of the black phosphorous material on the carbon paper is 1.47V, and at 1.6V, the current density can reach 100mA·cm -2 (RHE).

Example Embodiment

[0030] Example 2:
[0031] A one-step method for synthesizing black phosphorus on carbon paper and its application specifically include the following steps:
[0032] S1. Weigh 4.0g of red phosphorus and evenly put it into the quartz boat, then put the quartz boat into the tube furnace, and then pass the argon protective gas into the tube furnace; heat the tube furnace to 180℃ at a constant speed, and heat 2h, perform annealing treatment;
[0033] S2, after annealing, prepare annealed samples, and cool them to room temperature for later use;
[0034] S3. Transfer the sample of S2 to a mortar and grind it for 20 minutes to obtain the required precursor red phosphorus for later use;
[0035] S4. Weigh 0.4g of the precursor red phosphorus prepared in S3 and evenly put it into the quartz boat, then put the blank carbon paper on the quartz boat, and then transfer it to the middle of the tube furnace;
[0036] S5. Pass the protective gas argon into the tube furnace, strictly control the flow rate of argon to 5sccm, heat the tube furnace to 550℃ at a constant speed, keep it for 2h, then lower the temperature to 350℃, and keep it for 2h. Black phosphorous material on carbon paper.

Example Embodiment

[0037] Example 3:
[0038] A one-step method for synthesizing black phosphorus on carbon paper and its application specifically include the following steps:
[0039] S1. Weigh 6.0g of red phosphorus and evenly put it into the quartz boat, then put the quartz boat into the tube furnace, and then pass the argon protective gas into the tube furnace; heat the tube furnace to 250℃ at a constant speed, and heat 4h, perform annealing treatment;
[0040] S2, after annealing, prepare annealed samples, and cool them to room temperature for later use;
[0041] S3. Transfer the sample of S2 to a mortar and grind it for 60 minutes to obtain the required precursor red phosphorus for later use;
[0042] S4. Weigh 0.4g of the precursor red phosphorus prepared in S3 and evenly put it into the quartz boat, then put the blank carbon paper on the quartz boat, and then transfer it to the middle of the tube furnace;
[0043] S5. Pass the protective gas argon into the tube furnace, strictly control the flow rate of argon to 6sccm, heat the tube furnace to 600℃ at a constant speed, keep it for 2h, then lower the temperature to 350℃, and keep it for 1h. Black phosphorous material on carbon paper.
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PUM

PropertyMeasurementUnit
First discharge specific capacity2234.5mAh/g
Specific capacity1677.3mAh/g
tensileMPa
Particle sizePa
strength10

Description & Claims & Application Information

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