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Electric field induced crystallization K6Si2O7 potassium fast ionic conductor synergistically doped with P5+, Al3+ and B3+ ions and preparation method thereof

A technology of electric field induction and ion conductor, which is applied in the direction of circuits, electrical components, secondary batteries, etc., to reduce the activation energy of migration, accelerate the speed of crystallization, and improve the integrity of crystallization

Inactive Publication Date: 2019-09-20
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the potassium ion conductors that are essential for the construction of potassium ion all-solid-state batteries are still basically blank.

Method used

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  • Electric field induced crystallization K6Si2O7 potassium fast ionic conductor synergistically doped with P5+, Al3+ and B3+ ions and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Embodiment 1: the solid K 2 CO 3 : NH 4 h 2 PO 4 :Al 2 o 3 : SiO 2 :B 2 o 3 According to K 6.18 B 0.1 Al 0.i P 0.02 Si 1.78 o 7 The ratio of the stoichiometric molar ratio is evenly mixed, adding quality is the dehydrated alcohol of mixture quality 4.5%, in ball mill with the rotating speed ball mill of 120 rev / mins 16 hours, after ball mill finishes, in 60 ℃ of vacuum ovens (gas pressure in the oven is at 5 Pa) for 2 hours, take it out and re-grind in an agate mortar for 12 minutes, the ground powder is heated to 470°C at a rate of 6°C / min in an air atmosphere and then cooled with the furnace for 3 hours; The powder was ground again in an agate mortar for 10 minutes, and the ground powder was heated up to 750°C at a rate of 5°C / min in an air atmosphere for 10 hours and then cooled with the furnace; after grinding, it was oxidized in 0.1M hydrogen After soaking in sodium solution for 6 minutes, filter, dry and press at 1×10 7 Press it into thin slices un...

Embodiment 2

[0012] Embodiment 2: the solid K 2 CO 3 : NH 4 h 2 PO 4 :Al 2 o 3 : SiO 2 :B 2 o 3 According to K 6.25 B 0.15 Al 0.15 P 0.05 Si 1.65 o 7 The ratio of the stoichiometric molar ratio is evenly mixed, adding quality is the dehydrated alcohol of mixture quality 9%, in ball mill with the rotating speed ball mill of 480 rev / mins 45 hours, in 110 ℃ of vacuum ovens after ball mill finishes (gas pressure in oven is at 20Pa) for 9 hours, take it out and re-grind it in an agate mortar for 30 minutes, heat up the ground powder to 530°C in an air atmosphere at a rate of 30°C / min and keep it warm for 10 hours, then cool it with the furnace; The powder was ground again in an agate mortar for 30 minutes, and the ground powder was heated to 850°C at a rate of 15°C / min in the air atmosphere and kept for 19 hours, then cooled with the furnace; after grinding, it was oxidized in 0.3M hydrogen After soaking in sodium solution for 12 minutes, filter, dry and press in a 7×10 7 Press ...

Embodiment 3

[0013] Embodiment 3: the solid K 2 CO 3 : NH 4 h 2 PO 4 :Al 2 o 3 : SiO 2 :B 2 o 3 According to K 6.22 B 0.12 Al 0.13 P 0.03 Si 1.72 o 7 The ratio of the stoichiometric molar ratio is evenly mixed, adding quality is the dehydrated alcohol of mixture quality 5%, in ball mill with the rotating speed ball mill of 300 rev / mins 30 hours, after ball mill finishes, in 80 ℃ of vacuum ovens (gas pressure in oven is at 15Pa) for 7 hours, take it out and re-grind in an agate mortar for 20 minutes, and the ground powder is heated to 510°C at a rate of 20°C / min in an air atmosphere and then cooled with the furnace for 7 hours; The powder was ground again in an agate mortar for 20 minutes, and the ground powder was heated to 810°C at a rate of 10°C / min in the air atmosphere and kept for 15 hours, then cooled with the furnace; after grinding, it was oxidized in 0.2M hydrogen After soaking in sodium solution for 10 minutes, filter, dry and place in a press at 5×10 7 Press it i...

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Abstract

An electric field induced crystallization K6Si2O7 potassium fast ionic conductor synergistically doped with P5+, Al3+ and B3+ ions and a preparation method thereof are characterized in that the stoichiometric formula is K<6+x+y-z>B<x>Al<y>P<z>Si<2-x-y-z>O7, wherein x is 0.1-0.15, y is 0.1-0.15, and z is 0.02-0.05; Al3+ and B3+ partially replace Si4+ ions to produce high-concentration interstitial potassium ions in a crystal, which is helpful to reduce the activation energy of potassium ion migration; the electronic conductivity of the fast ionic conductor is further reduced through doping of P5+; the size of the potassium ion migration channel is adjusted through doping of B3+ with small ion radius in order to adapt to the rapid migration of potassium ions; and the surface of K6Si2O7 particles is modified in the preparation process to make the conductor easy to sinter. At the same time, a strong DC electric field is introduced to induce crystallization, so as to accelerate the crystallization rate, reduce the crystallization temperature and improve the crystallization integrity. The synergistic effect makes the conductivity of potassium ions of the potassium fast ionic conductor exceed 5*10<-4>S / cm at room temperature, which is closer to the conductivity of potassium ions of liquid electrolyte.

Description

technical field [0001] The invention relates to the field of manufacturing a solid potassium fast ion conductor. Background technique [0002] Lithium-ion batteries have absolute advantages such as high volume, high weight-to-energy ratio, high voltage, low self-discharge rate, no memory effect, long cycle life, and high power density. They have an annual share of more than 30 billion US dollars in the global mobile power market and far exceed other The market share of batteries is the most promising chemical power source [Wu Yuping, Wan Chunrong, Jiang Changyin, Lithium-ion Secondary Batteries, Beijing: Chemical Industry Press, 2002.]. At present, most of the lithium-ion secondary batteries at home and abroad use liquid electrolytes. Liquid lithium-ion batteries have some disadvantages, such as: liquid organic electrolytes may leak, and may explode at too high a temperature, causing safety accidents, and cannot be used in some applications. Occasions with high safety requi...

Claims

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Application Information

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IPC IPC(8): H01M10/054H01M10/0562
CPCH01M10/054H01M10/0562H01M2300/0068Y02E60/10
Inventor 水淼舒杰任元龙
Owner NINGBO UNIV
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