A dense sub -micron crystal β ″al 2 o 3 Products, preparation methods and applications

A dense submicron and submicron technology, which is applied in the field of its preparation and dense submicron β"-Al2O3 products, can solve problems such as residues, achieve the effects of inhibiting diffusion, reducing costs, and high mechanical strength

Active Publication Date: 2021-01-01
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The US PNNL National Laboratory reported the use of TiO in the literature: X.Lu et al.Journal of Power Sources 295(2015) 167-174 2 with MnO 2 The grain size of the sintered product is several microns, and the highest density is 98.5%, but the SEM picture of the product shows that a large number of holes still remain in the sintered sample

Method used

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  • A dense sub -micron crystal β ″al <sub>2</sub> o <sub>3</sub> Products, preparation methods and applications
  • A dense sub -micron crystal β ″al <sub>2</sub> o <sub>3</sub> Products, preparation methods and applications

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] In this example, β"-Al 2 o 3 The molecular formula of the electrolyte substrate is Na 1.67 Al1 0.67 Mg 0.67 o 17 , its preparation method is as follows:

[0048] (1) Preparation of β"-Al 2 o 3 Powder

[0049] To synthesize 10mol, 6.15kg Na 1.67 Al1 0.67 Mg 0.67 o 17 as an example.

[0050] Weigh 5.4kg of boehmite, 1.44kg of sodium metaaluminate, 395g of magnesium hydroxide, and 10kg of ethanol, mix them in a grinding barrel, use a horizontal sand mill, 2400 rpm, and grind for 5 hours to obtain a uniform slurry material;

[0051] Drying at 45-60°C to remove ethanol, and calcining at 1200°C for 2 hours to obtain a calcined product;

[0052] Grind the calcined product in water or ethanol, add an appropriate amount of binder (PVA or PVP), and spray granulate to obtain β"-Al 2 o 3 Granulated powder.

[0053] (2) Preparation of β"-Al 2 o 3 Strip

[0054] Weigh 1kgβ"-Al 2 o 3 Granulating powder, adding alcohol, PVB, DBP, PEG and tributyl citrate, ball mil...

Embodiment 2

[0058] In this embodiment, in this embodiment, the electrolyte substrate is β"-Al 2 o 3 -YSZ, its preparation method is as follows:

[0059] (1) Preparation of β"-Al 2 o 3 -YSZ powder

[0060] To synthesize 10mol, 6.15kg Na 1.67 Al1 0.67 Mg 0.67 o 17 as an example.

[0061] Weigh 5.4kg of boehmite, 1.44kg of sodium metaaluminate, 395g of magnesium hydroxide, and 10kg of ethanol, mix them in a grinding barrel, use a horizontal sand mill, 2400 rpm, and grind for 5 hours to obtain a uniform slurry Material; dry at 45-60°C to remove ethanol, and calcined at 1200°C for 2h to obtain the calcined product Na 1.67 Al1 0.67 Mg 0.67 o 17 Powder;

[0062] 6kg Na 1.67 Al1 0.67 Mg 0.67 o 17 , 4kg 8YSZ powder is ground in water or ethanol, adding an appropriate amount of binder (PVA or PVP), and spraying granulation to obtain β"-Al 2 o 3 - YSZ granulation powder.

[0063] (2) Preparation of β"-Al 2 o 3 -YSZ Strip

[0064] Weigh 1kgβ"-Al 2 o 3 -YSZ granulation powder,...

Embodiment 3

[0068] In the present embodiment, in the present embodiment, the electrolyte substrate is Mn and Ti doped β "-Al 2 o 3 -YSZ, its preparation method is as follows:

[0069] (1) Preparation of β"-Al doped with Mn and Ti 2 o 3 -YSZ powder

[0070] To synthesize 10mol, 6kg Mn and Ti-doped Na 1.67 Al1 0.67 Mg 0.67 o 17 as an example.

[0071] Weigh boehmite 5.4kg, sodium metaaluminate 1.44kg, magnesium hydroxide 395g, manganese acetate 370g, butyl titanate 68, ethanol 10kg, mix them in a grinding barrel, use a horizontal sand mill, 2400 rev / min, grind for 5h to obtain a homogeneous slurry;

[0072] Drying at 45-60°C to remove ethanol, and calcining at 1200°C for 2 hours to obtain a calcined product;

[0073] 6 kg Mn doped with Ti Na 1.67 Al1 0.67 Mg 0.67 o 17 Grind 4kg 8YSZ powder in water or ethanol, add an appropriate amount of binder (PVA or PVP), and spray granulate to obtain Mn and Ti doped β"-Al 2 o 3 - YSZ granulation powder.

[0074] (2) Preparation of Mn a...

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Abstract

The invention provides a compact submicron-grain beta''-Al2O3 product. The crystal grain size is less than or equal to 3 micrometers, and the compactness is more than or equal to 95%, the beta''-Al2O3 product can meet actual demands of a plurality of fields such as battery electrolytes, gas sensors, and sodium metal purification. The invention also provides a method for preparing the beta''-Al2O3 product by adopting a solid phase reaction for preparing beta''-Al2O3 powder, and adopting liquid-phase-assisted two-stage sintering, the method can obtain the beta''-Al2O3 product with small grain sizes and high compactness, and can control the sintering temperature to be 1450 EDG C or less during a sintering process, so that a Na element diffusion problem during the sintering process is remarkably inhibited, devices employed in the method is simplified, and the costs are reduced.

Description

technical field [0001] The present invention relates to β"-Al 2 o 3 Technical field, be specifically related to a kind of dense submicron crystal β "-Al 2 o 3 Products, their preparation methods and applications. Background technique [0002] β"-Al 2 o 3 It is a sodium ion conductor material, because it has a high sodium ion conductivity (about 0.2-0.4S / cm) at 300 ° C and is used in high-temperature sodium batteries (such as sodium-sulfur batteries, sodium-nickel chloride batteries (Zero Emission Battery Research Activities, ZEBRA)), gas sensors, sodium metal purification and many other fields have been applied. In high temperature sodium batteries, β"-Al 2 o 3 Generally used as an electrolyte material. Among them, Na 1.67 al 10.67 Mg 0.67 o 17 , Na 1.67 al 10.33 Li 0.33 o 17 is β"-Al 2 o 3 The two classical molecular formulas, when actually used as an electrolyte, in order to improve the strength, a certain amount (≤50%) of doped ZrO is usually added to i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/0562C04B35/10C04B35/622C04B35/64C04B35/626H01M10/054
CPCC04B35/10C04B35/622C04B35/62605C04B35/62695C04B35/64C04B2235/3246C04B2235/549C04B2235/656C04B2235/661C04B2235/77H01M10/054H01M10/0562Y02E60/10
Inventor 王建新官万兵刘武王成田
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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