Preparation methods of iron-sulfur compound and preparation method of iron-sulfur compound composite material

A technology of iron-sulfur compounds and composite materials, applied in the direction of iron sulfide, nanotechnology for materials and surface science, electrochemical generators, etc., can solve the problem of harmful L-cysteine ​​inhalation into the respiratory tract, poor vulcanization effect, etc. problems, to achieve the effect of excellent electrochemical performance, uniform morphology, and short reaction cycle

Active Publication Date: 2017-05-31
TAIYUAN UNIV OF TECH
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Problems solved by technology

The disadvantage of this method is that the inhalation of L-cysteine ​​is...

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  • Preparation methods of iron-sulfur compound and preparation method of iron-sulfur compound composite material
  • Preparation methods of iron-sulfur compound and preparation method of iron-sulfur compound composite material

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[0019] A preparation method for an iron-sulfur compound, comprising the steps of:

[0020] 1) Preparation of precursor A; the precursor A is iron oxide α-FeOOH or F-MIL, F=Fe; MIL=Materials from the Lavoisier Institute;

[0021] 2) Weigh the precursor A and sulfur powder respectively and place them in a porcelain boat, wherein the mass ratio of precursor A to sulfur powder is between 1:20-1:30 (1:20, 1:22, 1:24 can be selected , 1:26, 1:28, 1:30); put the porcelain boat in the annealing furnace, annealing reaction in the protective gas, the heating rate is between 1°C / min-3°C / min, precursor A and sulfur The way to put the powder in the porcelain boat is to mix it evenly or place it separately on both sides of the porcelain boat. ), the constant temperature time is between 1h-2h (1.0h, 1.2h, 1.4h, 1.6h, 1.8h, 2.0h), and the obtained product is iron-sulfur compound.

[0022] A preparation method of an iron-sulfur compound composite material, comprising the steps of:

[00...

Embodiment 1

[0029] 1) Preparation of α-FeOOH;

[0030] 2) α-FeOOH@C is obtained by wrapping α-FeOOH with carbon;

[0031] 3) Weigh 0.0500gα-FeOOH@C and 1g sulfur powder respectively, mix them evenly and place them on both sides of the porcelain boat respectively, place the porcelain boat in the annealing furnace, and raise the temperature at 2°C / min to 500°C, keep warm for 2h, cool down at 10°C / min, and collect the product, which is FeS 2 Nano stave. TEM transmission electron microscope photos are attached figure 1As shown, the shape of the nanorod is uniform, the diameter is about 15-20nm, and the size is about 400nm.

Embodiment 2

[0033] 1) Preparation of α-FeOOH;

[0034] 2) α-FeOOH@C is obtained by wrapping α-FeOOH with carbon;

[0035] 3) Weigh 0.0500g of α-FeOOH@C and 1g of sulfur powder respectively, mix them evenly and place them in a porcelain boat, place the porcelain boat in an annealing furnace, and heat up to 500°C at 2°C / min in an argon atmosphere. Keep warm for 12h, cool down at 10°C / min, and collect the product, which is FeS 2 @C nanorods.

[0036] The XRD diffraction pattern of the ferrous disulfide in the present embodiment is as attached figure 2 shown. The ferrous disulfide nanorod in the present embodiment is carried out the electrochemical test of sodium ion battery:

[0037] 1) Mix and grind the prepared ferrous sulfide nanorods with acetylene black and carboxymethyl cellulose (CMC) in a mass ratio of 7:2:1 with deionized water as a solvent;

[0038] 2) Evenly coat the slurry obtained by grinding on the copper foil, after vacuum drying, punch holes into electrode sheets of...

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Abstract

The invention belongs to the field of electrode materials of electrochemistry, and in particular to a preparation method of an iron-sulfur compound and a preparation method of an iron-sulfur compound composite material. The invention solves the problems of high cost and poor vulcanization effect in an iron-sulfur compound production process at present. The preparation method of the iron-sulfur compound comprises the following steps: 1) preparing a precursor A, wherein the precursor A is oxide alpha-FeOOH of iron or F-MIL (Materials from the Lavoisier Institute); 2) respectively weighing the precursor A and powdered sulfur, placing same into a porcelain boat, wherein the mass ratio of the precursor A to the powdered sulfur is between (1 to 20) to (1 to 30); placing the porcelain boat into an annealing furnace, performing annealing reaction in protective gas so as to obtain the final product iron-sulfur compound, wherein the precursor A and powdered sulfur are uniformly mixed and placed in the porcelain boat or the precursor A and powdered sulfur are arranged on two sides of the porcelain boat separately, the constant temperature ranges from 400 DEG C to 500 DEG C, the time for constant temperature is 1-2 hours. Sulfide nanorods prepared according to the invention is uniform in morphology and excellent in electrochemical performance; the operation is simple, the reaction period is short, the cost is low, and the preparations are suitable for batch production.

Description

technical field [0001] The invention belongs to the field of electrochemical electrode materials, and in particular relates to a preparation method of an iron-sulfur compound and a composite material thereof. Background technique [0002] In recent years, one-dimensional nanomaterials have become a research hotspot in the field of materials. Because of its ability to realize direct electron transport and strong charge transport ability, it has good application prospects in the fields of optics, electronics, environment and medicine. One-dimensional nanomaterials refer to nanoscale materials in the two-dimensional direction and macroscale in length, including nanowires, nanorods, nanotubes, and nanoribbons [Chang Yingxing, Zhang Wen. Electricity of one-dimensional nanomaterials Chemical Preparation and Application Research [J]. Materials Herald, 2012,26(2):44-49]. [0003] Metal sulfide nanomaterials have special nonlinear properties, fluorescence properties, quantum size e...

Claims

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Application Information

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IPC IPC(8): C01G49/12H01M4/58H01M10/054B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01G49/12C01P2002/72C01P2004/04C01P2004/16C01P2004/64H01M4/5815H01M10/054Y02E60/10
Inventor 柏中朝卢贞晓王孝广唐宾
Owner TAIYUAN UNIV OF TECH
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