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Iron selenium alloy and preparation method thereof

A technology of iron-selenium alloy and selenium powder, which is applied in the field of iron-selenium alloy and its preparation, can solve the problems such as the complexity of the method reported in the newspaper, and achieve the effects of high production efficiency, high utilization rate of raw materials and equipment, and low environmental pollution

Active Publication Date: 2019-07-02
广东先导稀贵金属材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the common synthesis methods of FeSe alloys include hydrothermal method and vacuum high-temperature synthesis, etc., but the methods reported in the newspapers are relatively complicated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0016] The preparation method of the iron-selenium alloy according to the first aspect of the present invention comprises the steps of: mixing the iron powder and the selenium powder, placing them in a quartz boat or a graphite boat; placing the quartz boat or a graphite boat in a quartz tube, and passing into the quartz tube Protective gas; place the quartz tube in the synthesis furnace, raise the temperature to 650°C-850°C at a rate of 20°C / min-70°C / min, cool down after heat preservation, and take it out of the furnace to complete the preparation of the iron-selenide alloy.

[0017] In the preparation method of the iron-selenium alloy according to the first aspect of the present invention, the heating rate is lower than 20°C / min, the reaction rate is slower and easily causes selenium volatilization, and the uniformity of the obtained iron-selenium alloy is poor; If the rate is higher than 70°C / min, the selenium vapor pressure is too large to react in time, resulting in the lo...

Embodiment 1

[0032] Filter with 100 mesh molecular sieves to obtain 2N iron powder 500.0g and 2N selenium powder 520.0g. Pour the iron powder and selenium powder into the homogenizer in sequence, and mix for 60 minutes to obtain a mixed powder.

[0033] Use a graphite boat to hold the mixed powder, then put the graphite boat into the quartz tube of the tubular atmosphere furnace, open the nitrogen valve, control the flow rate to 3-5L / min, connect the tail gas pipeline, and use sodium hydroxide solution to absorb the tail gas. After being evacuated with nitrogen for 15 minutes, the temperature was raised to 800° C. at a rate of 30° C. / min, and then kept for 2 hours for reaction.

[0034] After the reaction was finished, the temperature was lowered, and when the hearth of the tubular atmosphere furnace dropped below 100°C, the graphite boat was taken out, cooled to room temperature, and then sampled to obtain 1003g of iron-selenide alloy. Wherein, in the iron-selenium alloy obtained, the ma...

Embodiment 2

[0036] Filter with 200 mesh molecular sieves to obtain 2N iron powder 500.0g and 3N selenium powder 421.4g. Pour the iron powder and selenium powder into the homogenizer in sequence, and mix for 90 minutes to obtain a mixed powder.

[0037] Use a graphite boat to hold the mixed powder, then put the graphite boat into the quartz tube of the tubular atmosphere furnace, open the nitrogen valve, control the flow rate to 3-5L / min, connect the tail gas pipeline, and use sodium hydroxide solution to absorb the tail gas. After being evacuated with nitrogen for 20 min, the temperature was raised to 750 °C at a rate of 40 °C / min, and then kept for 3 h for reaction.

[0038] After the reaction was completed, the temperature was lowered, and when the hearth of the tubular atmosphere furnace dropped below 100°C, the graphite boat was taken out, cooled to room temperature, and then sampled to obtain 907g of iron-selenide alloy. Wherein, in the iron-selenium alloy obtained, the mass percent...

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Abstract

The present invention provides an iron-selenium alloy and a preparation method thereof. The preparation method comprises: uniformly mixing iron powder and selenium powder, and placing the mixture in aquartz boat or a graphite boat; placing the quartz boat or the graphite boat in a quartz pipe, and introducing a protection gas into the quartz pipe; and placing the quartz pipe into a synthesis furnace, heating to a temperature of 650-850 DEG C at a heating rate of 20-70 DEG C / min, carrying out thermal insulation, cooling, and discharging out of the furnace so as to complete the preparation of the iron-selenium alloy. According to the present invention, the preparation method has advantages of simple process, short production period, high production efficiency, high raw material utilizationrate and high equipment utilization rate.

Description

technical field [0001] The invention relates to the field of chemistry and chemical engineering, in particular to an iron-selenium alloy and a preparation method thereof. Background technique [0002] Selenium has the symbol Se and atomic number 34. The division of selenium in the earth's crust is 5×10 -6 , is one of the rare metals. Selenium has a wide range of uses and can be used in many fields such as electronics, metallurgy, glass, ceramics, chemical industry, agriculture, food, hygiene and environmental protection. With the continuous understanding of the properties of selenium and the improvement of product purity, the downstream demand for selenium is still increasing. is growing. [0003] The chemical element symbol of iron is Fe, and its atomic number is 56. It is one of the most widely used metal materials in industry. Iron-based superconducting materials are new members discovered in recent years. The 11-system is the iron-based superconducting material with ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22C33/04C22C38/60C22C28/00C22C1/02
Inventor 王波朱刘
Owner 广东先导稀贵金属材料有限公司
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