Preparation method of FeSe nano powder

A nano-powder and solution technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of high cost and difficult to promote, achieve low environmental pollution, wide promotion potential, technology short process effect

Active Publication Date: 2014-03-26
NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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Problems solved by technology

However, this method is expensive and difficult to promote

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  • Preparation method of FeSe nano powder
  • Preparation method of FeSe nano powder
  • Preparation method of FeSe nano powder

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Embodiment 1

[0039] The preparation method of the present embodiment FeSe nanopowder comprises the following steps:

[0040] Step 1. Dissolve 80g NaOH in deionized water to prepare a NaOH solution with a pH value of 8, and then prepare according to Se:OH - =1:2 molar ratio, add 79g of Se powder into the NaOH solution, stir until the Se powder is completely dissolved, and obtain a clear and uniform solution A;

[0041] Step 2. According to NaBH 4 : Se=2:1 molar ratio, 76g NaBH 4 Powder slowly added to solution A in step 1, NaBH 4 The feeding rate of powder is 1.0g / min, stirring until NaBH 4 The powder was completely dissolved to obtain a clear and uniform solution B;

[0042] Step 3, feed inert gas into solution B to remove dissolved oxygen in the solution, then in a glove box full of inert gas, according to Fe 2+ : Se=1:1 molar ratio, 127g FeCl 2 Slowly add in the solution B described in step 2, FeCl 2 The feeding rate is 5g / min, stirring for 30min makes precipitation reaction occur...

Embodiment 2

[0046] The preparation method of the present embodiment FeSe nanopowder comprises the following steps:

[0047] Step 1. Dissolve 280g KOH in deionized water to prepare a KOH solution with a pH value of 12, and then follow the Se:OH - =1:5 molar ratio, add 79g of Se powder into the KOH solution, stir until the Se powder is completely dissolved, and obtain a clear and uniform solution A;

[0048] Step 2. According to NaBH 4 : Se=3:1 molar ratio, 114g NaBH 4 Powder slowly added to solution A in step 1, NaBH 4 The feeding rate of powder is 1.2g / min, stirring until NaBH 4 The powder was completely dissolved to obtain a clear and uniform solution B;

[0049] Step 3, feed helium into solution B to remove dissolved oxygen in the solution, then in a glove box full of helium, according to Fe 2+ : Se=1.1:1 molar ratio, 167.2g FeSO 4 Slowly add in the solution B described in step 2, FeSO 4 The feeding rate is 6g / min, stirring for 60min makes precipitation reaction occur, and obtain...

Embodiment 3

[0053] The preparation method of the present embodiment FeSe nanopowder comprises the following steps:

[0054] Step 1. Dilute 375g of industrial ammonia water (28wt%) with deionized water to prepare an ammonia solution with a pH value of 9, and then use Se:OH - =1:3 molar ratio, add 79g of Se powder into the ammonia solution, stir until the Se powder is completely dissolved, and obtain a clear and uniform solution A;

[0055] Step 2. According to NaBH 4 : Se=5:1 molar ratio, 190g NaBH 4 Powder slowly added to solution A in step 1, NaBH 4 The feeding rate of powder is 0.8g / min, stirring until NaBH 4 The powder was completely dissolved to obtain a clear and uniform solution B;

[0056] Step 3, feed argon into solution B to remove dissolved oxygen in the solution, then in a glove box full of argon, according to Fe 2+ : Se=1.2:1 molar ratio, 108g Fe(OH) 2 Slowly add in the solution B described in step 2, Fe(OH) 2 The feeding rate is 3g / min, stirring for 45min makes precipi...

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Abstract

The invention provides a preparation method of FeSe nano powder. The method comprises the following steps: 1, adding Se powder to an alkali liquor according to a certain molar ratio and agitating for dissolving, so as to obtain a solution A; 2, adding NaBH4 powder to the solution A according to a certain molar ratio and agitating for dissolving, so as to obtain a solution B; 3, adding a ferrous salt to the solution B according to a certain molar ratio in a glove box full of inert gases and agitating, so as to obtain a solution C; 4, adjusting the pH value of the solution C, and then orderly settling, filtering, washing and drying, so as to obtain the FeSe nano powder. The preparation method of the FeSe nano powder is simple and easy-to-control in preparation technology, short in technological process, strong in repeatability and applicable to industrial large-scale production. The FeSe prepared by the preparation method is tetragonal nanoscale powder, the chemical components and particle size distribution are even, and the requirements of subsequent application can be met.

Description

technical field [0001] The invention belongs to the technical field of FeSe superconducting materials, and in particular relates to a preparation method of FeSe nano powder. Background technique [0002] In 2008, LaO with a critical temperature of 26K was first reported by the Japanese Hosono research group. 1-x f x FeAs, followed by Fe-based superconducting materials (FHS) developed rapidly. At present, four main systems have been developed, namely "1111" system (such as LaFeAsOF), "122" system (such as BaFe 2 As 2 ), "111" system (such as LiFeAs) and "11" system (such as FeSe). Similar to the high-temperature copper oxide superconductor (HTS), the crystal structure of FHS is a layered structure, with -FeAs-layer (or -FeSe-layer) as the superconducting layer. [0003] There are three main reasons for the rapid development of FHS: First, it is generally believed that the magnetism of Fe can destroy the electron pairing in conventional superconductors, so in FHS, the coe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04B82Y30/00
Inventor 张胜楠王亚林卢天倪冯建情李成山
Owner NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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