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P<5+> and Be<2+> co-doped K2MgSi5O12 potassium fast ion conductor crystallized under induction of electric field and preparation method of potassium fast ion conductor

A technology of electric field induction and ion conductor, which is applied in the direction of circuits, electrical components, secondary batteries, etc., to achieve the effects of reducing grain boundary gaps, accelerating crystallization speed, and reducing migration activation energy

Inactive Publication Date: 2019-10-08
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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  • P&lt;5+&gt; and Be&lt;2+&gt; co-doped K2MgSi5O12 potassium fast ion conductor crystallized under induction of electric field and preparation method of potassium fast ion conductor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Embodiment 1: the solid K 2 CO 3 : NH 4 h 2 PO 4 :MgO:SiO 2 : BeO according to K 2.18 MgB 0.1 P 0.02 Si 4.88 o 12 The ratio of the stoichiometric molar ratio is evenly mixed, adding quality is the dehydrated alcohol of mixture quality 3%, in ball mill with the rotating speed ball mill of 120 rev / mins 10 hours, after ball mill finishes, in 60 ℃ of vacuum ovens (gas pressure in oven is at 5Pa) for 3 hours, take it out and re-grind in an agate mortar for 12 minutes, and the ground powder is heated to 560°C at a rate of 7°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 1260 °C at a rate of 5 °C / min in a platinum crucible in an air atmosphere and kept for 25 hours, then taken out of the furnace and cooled rapidly; the cooled The material was pulverized and ground for 30 minutes in the mill, soaked in 0.1M sodium hydroxide solution for 5 min...

Embodiment 2

[0012] Embodiment 2: the solid K 2 CO 3 : NH 4 h 2 PO 4 :MgO:SiO 2 : BeO according to K 2.35 MgB 0.2 P 0.05 Si 4.75 o 12 The ratio of the stoichiometric molar ratio is uniformly mixed, adding quality is the dehydrated alcohol of mixture quality 9%, in ball mill with the rotating speed ball mill of 500 rev / mins 50 hours, after ball mill finishes, in 110 ℃ of vacuum ovens (gas pressure in the oven is at 20Pa) for 10 hours, take it out and re-grind in an agate mortar for 30 minutes, the ground powder is heated to 650°C at a rate of 30°C / min in the air atmosphere and then cooled with the furnace for 10 hours; The powder was ground again in an agate mortar for 30 minutes, and the ground powder was heated up to 1350°C in a platinum crucible in an air atmosphere at a rate of 13°C / min and kept at 1350°C for 45 hours, then taken out of the furnace and cooled rapidly; the cooled The material was pulverized and ground for 50 minutes in the mill, soaked in 0.3M sodium hydroxide ...

Embodiment 3

[0013] Embodiment 3: the solid K 2 CO 3 : NH 4 h 2 PO 4 :MgO:SiO 2 : BeO according to K 2.27 MgB 0.15 P 0.03 Si 4.82 o 12 The ratio of the stoichiometric molar ratio is uniformly mixed, adding quality is the dehydrated alcohol of 6% of mixture quality, ball milled with the rotating speed of 350 rev / mins in ball mill for 30 hours, after ball mill finishes, in 90 ℃ of vacuum ovens (gas pressure in the oven is at 15Pa) and dry for 6 hours, take it out and re-grind in an agate mortar for 20 minutes, the ground powder is heated up to 610°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 up to 1300°C in a platinum crucible in an air atmosphere at a rate of 10°C / min and kept at 1300°C for 35 hours, then taken out of the furnace and cooled rapidly; the cooled The material was pulverized and ground for 40 minutes in the mill, soaked in 0.2M ...

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Abstract

The invention relates to a P<5+> and Be<2+> co-doped K2MgSi5O12 potassium fast ion conductor crystallized under induction of an electric field and a preparation method of the potassium fast ion conductor. The potassium fast ion conductor is characterized in that the stoichiometric formula is K<2+2x-z>MgBe<x>P<z>Si<5-x-z>O<12>, wherein x is in a range of 0.1-0.2, and z is in a range of 0.02-0.05; and the normal-temperature potassium ion electrical conductivity exceeds 5*10<-4> S / cm. Be<2+> is used to partially substitute Si<4+> ions, and gap potassium ions are generated in the crystal, so thatmigration activation energy of potassium ions is reduced; electron conductivity of the fast ion conductor is further reduced through doping of P<5+>; the size of migration channels of the potassium ions is adjusted through doping of the Be<2+> with a small ion radius so as to adapt to rapid migration of the potassium ions; and the surfaces of the K2MgSi5O12 particles are modified in the preparation process so as to form an easy-to-sinter characteristic. Meanwhile, a strong direct current field is introduced to induce crystallization for increasing the crystallization speed, reducing the crystallization temperature and improving crystallization integrity. The synergistic effect enables normal-temperature potassium ion electrical conductivity of the potassium fast ion conductor to exceed 5*10<-4> S / cm, which is closer to potassium ion electrical conductivity of a 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): C04B35/20C04B35/622C04B35/626H01M10/0562
CPCC04B35/20C04B35/622C04B35/62605C04B2235/3201C04B2235/3205C04B2235/447C04B2235/602C04B2235/6562C04B2235/6567H01M10/0562Y02E60/10
Inventor 水淼舒杰任元龙
Owner NINGBO UNIV
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