Preparation method of six-membered spinel type iron-cobalt-chromium-manganese-magnesium-copper high-entropy oxide and powder thereof

An iron-cobalt-chromium-manganese-magnesium-copper-based, spinel-type technology is applied in the field of high-entropy oxide powder materials, which can solve the problems of high raw material cost, complex process, long holding time, etc., and achieves uniform distribution, simple operation, simple method effect

Inactive Publication Date: 2020-06-05
NANCHANG HANGKONG UNIVERSITY
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  • Description
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Problems solved by technology

[0010] The preparation method of the spinel type high-entropy oxide that domestic and foreign document reports or Chinese invention patent announces mainly contains two kinds of solid phase reaction method and wet chemical method at present, wherein the heat preservation time that solid phase reaction method adopts is very long (10~ 20 hours, 20 hours, 20-30 hours), and it needs to be placed on an aluminum plate for air quenching, which has the characteristics of relatively complicated process and long cycle; in addition, the spinel type is prepared by wet chemical methods (including solution combustion synthesis method) High-entropy oxides have the characteristics of high raw material cost, many preparation steps, complex and uncontrollable process, etc.
At present, there is no related report on high-entropy oxides with six-element spinel structure. The present invention provides a six-element spinel-type iron-cobalt-chromium-manganese-magnesium-copper-based high-entropy oxide and its powder preparation method

Method used

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  • Preparation method of six-membered spinel type iron-cobalt-chromium-manganese-magnesium-copper high-entropy oxide and powder thereof
  • Preparation method of six-membered spinel type iron-cobalt-chromium-manganese-magnesium-copper high-entropy oxide and powder thereof
  • Preparation method of six-membered spinel type iron-cobalt-chromium-manganese-magnesium-copper high-entropy oxide and powder thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A method for preparing a six-element spinel-type iron-cobalt-chromium-manganese-magnesium-copper-based high-entropy oxide and its powder, comprising the following steps:

[0028] Step 1, mix:

[0029] (1) Weigh Fe respectively according to molar ratio 1:1:1:2:1:1 2 o 3 (52.3g), Co 2 o 3 (54.3g), Cr 2 o 3 (49.8g), MnO 2 (61.9g), MgO (13.1g) and CuO (26.0g) powder, the powder after mixing is packed in the ball mill jar;

[0030] (2) According to the mass ratio of ball: material: water is 3:1:1, add ZrO respectively 2 Grinding balls and distilled water;

[0031] (3) Place the polyurethane ball milling pot milling on the pot milling machine station, and continuously ball milling at 220r / min for 12 hours to obtain mixed powder;

[0032] (4) The ball-milled powder is dried and sieved.

[0033] Step 2, calcining:

[0034] The sieved mixed powder is calcined in a muffle furnace and heated to 1000 ° C for 1 hour, and the furnace is cooled to room temperature after cal...

Embodiment 2

[0040] A method for preparing a six-element spinel-type iron-cobalt-chromium-manganese-magnesium-copper-based high-entropy oxide and its powder, comprising the following steps:

[0041] Step 1, mix:

[0042] (1) Weigh Fe respectively according to molar ratio 1:1:1:2:1:1 2 o 3 (52.3g), Co 2 o 3 (54.3g), Cr 2 o 3 (49.8g), MnO 2 (61.9g), MgO (13.1g) and CuO (26.0g) powder, the powder after mixing is packed in the ball mill jar;

[0043] (2) According to the mass ratio of ball: material: water is 3:1:1, add ZrO respectively 2 Grinding balls and distilled water;

[0044] (3) Place the polyurethane ball milling pot milling on the pot milling machine station, and continuously ball milling at 220r / min for 12 hours to obtain mixed powder;

[0045] (4) The ball-milled powder is dried and sieved.

[0046] Step 2, calcining:

[0047] The sieved mixed powder is calcined in a muffle furnace and heated to 900 ° C for 2 hours, and the furnace is cooled to room temperature after cal...

Embodiment 3

[0049] A method for preparing a six-element spinel-type iron-cobalt-chromium-manganese-magnesium-copper-based high-entropy oxide and its powder, comprising the following steps:

[0050] Step 1, mix:

[0051] (1) Weigh Fe respectively according to molar ratio 1:1:1:2:1:1 2 o 3 (52.3g), Co 2 o 3 (54.3g), Cr 2 o 3 (49.8g), MnO 2 (61.9g), MgO (13.1g) and CuO (26.0g) powder, the powder after mixing is packed in the ball mill jar;

[0052] (2) According to the mass ratio of ball: material: water is 3:1:1, add ZrO respectively 2 Grinding balls and distilled water;

[0053] (3) Place the polyurethane ball milling pot milling on the pot milling machine station, and continuously ball milling at 220r / min for 12 hours to obtain mixed powder;

[0054] (4) The ball-milled powder is dried and sieved.

[0055] Step 2, calcining:

[0056] The sieved mixed powder is calcined in a muffle furnace and heated to 800 ° C for 3 hours, and the furnace is cooled to room temperature after cal...

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Abstract

The invention discloses a preparation method of a six-membered spinel type iron-cobalt-chromium-manganese-magnesium-copper high-entropy oxide and powder thereof, and belongs to the field of high-entropy oxide powder materials. The chemical formula of the high-entropy oxide is (FeCoCrMnMgCu)3O4, the crystal structure of the high-entropy oxide is a face-centered cubic structure, and the space pointgroup of the high-entropy oxide is Fd-3m. The preparation method comprises following steps: firstly, ball-milling and uniformly mixing Fe2O3 powder, Cr2O3 powder, Co2O3 powder, MnO2 powder, MgO powderand CuO powder according to a molar ratio of 1: 1: 1: 2: 1: 1; drying, sieving, sintering for 1-3 hours at 800-1000 DEG C in a muffle furnace, calcining, and cooling in the furnace to the room temperature to obtain the single-phase spinel structure (FeCoCrMnMgCu)3O4 high-entropy oxide powder material. The preparation method has the advantages of low cost, short production period, industrial production, simple operation process, low energy consumption and the like, and the prepared powder is high in purity, small in particle size and uniform in distribution, and can be widely applied to the fields of super capacitor electrodes, lithium ion battery electrodes, water electrolysis hydrogen production and other novel energy materials.

Description

technical field [0001] The invention belongs to the field of high-entropy oxide powder materials, and in particular relates to a six-element iron-cobalt-chromium-manganese-magnesium-copper-based spinel-type high-entropy oxide and a method for preparing the powder. Background technique [0002] High-entropy alloys break through the traditional design concept of one or two metal elements as the main elements, but are a new type of alloy formed by solid solution of five or more metal elements in a certain proportion. It has a high mixing entropy, so the alloy generally has the characteristics of high strength, high hardness and excellent corrosion resistance. High-entropy oxide material is a new type of ceramic material developed on the basis of high-entropy alloys. In 2015, Rost et al. first proposed the concept of high-entropy oxides on the basis of high-entropy alloys, and successfully prepared High-entropy oxide (MgNiCoCuZn)O with rock-salt structure. In recent years, res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/26C04B35/626
CPCC04B35/2625C04B35/265C04B35/62605C04B2235/3206C04B2235/3241C04B2235/3267C04B2235/3274C04B2235/3275C04B2235/3281
Inventor 梁炳亮杨书伟陈卫华张建军何文欧阳晟刘长虹王义良程培栋艾云龙
Owner NANCHANG HANGKONG UNIVERSITY
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