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P<5+>, A1<3+> and B<3+> ion collaboratively doped K2MgSi5O12 potassium fast ion conductor and preparation method thereof

An ion conductor and ion technology, which is applied in the field of solid potassium fast ion conductor manufacturing to achieve the effect of reducing grain boundary voids and reducing migration activation energy.

Inactive Publication Date: 2019-10-25
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;, A1&lt;3+&gt; and B&lt;3+&gt; ion collaboratively doped K2MgSi5O12 potassium fast ion conductor and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Example 1 will solid K 2 CO 3 : NH 4 h 2 PO 4 : Al 2 o 3 : SiO 2 :B 2 o 3 : MgO according to K 2.08 MgB 0.05 Al 0.05 P 0.02 Si 4.88 o 12 The ratio of the stoichiometric molar ratio is uniformly mixed, adding quality is the dehydrated alcohol of mixture quality 3%, in ball mill with the rotating speed ball mill of 110 rev / mins 12 hours, after ball mill finishes, in 60 ℃ of vacuum ovens (gas pressure in the oven is at 3Pa) for 2 hours, take it out and re-grind in an agate mortar for 15 minutes, and the ground powder is heated to 550°C at a rate of 8°C / min in an air atmosphere and then cooled with the furnace after being kept 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 30 hours. After that, it was taken out of the furnace and cooled rapidly; the cooled The material was pulverized and ground for 30 minut...

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 : MgO according to K 2.25 MgB 0.15 Al 0.15 P 0.05 Si 4.65 o 12 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 450 rev / mins 43 hours, after ball mill finishes, in 110 ℃ of vacuum ovens (gas pressure in oven is at 15Pa) for 10 hours, take it out and re-grind in an agate mortar for 30 minutes, the ground powder is heated to 620°C at a rate of 30°C / min in an 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 to 1350°C in a platinum crucible in an air atmosphere at a rate of 12°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 45 minutes in the mill, soaked in 0.3...

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 : MgO according to K 2.17 MgB 0.1 Al 0.1 P 0.03 Si 4.77 o 12 The ratio of the stoichiometric molar ratio is evenly mixed, adding quality is the dehydrated alcohol of mixture quality 6%, in ball mill with the rotating speed ball mill of 350 rev / mins 25 hours, after ball mill finishes, in 90 ℃ of vacuum ovens (gas pressure in the 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 600°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 1310°C in a platinum crucible in an air atmosphere at a rate of 10°C / min and kept for 38 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 sodi...

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Abstract

The invention discloses a P<5+>, A1<3+> and B<3+> ion collaboratively doped K2MgSi5O12 potassium fast ion conductor and a preparation method thereof. The P<5+>, A1<3+> and B<3+> ion collaboratively doped K2MgSi5O12 potassium fast ion conductor is characterized in that the stoichiometric equation is K<2+x+y-z>MgB<x>Al<y>P<z>Si<5-x-y-z>O12, wherein x is within 0.05 to 0.15, y is with 0.05 to 0.15, and z is within 0.02-0.05; and the normal-temperature potassium ion conductivity exceeds 5*10<-4> S / cm. A1<3+> and B<3+> are adopted to partially replace Si<4+> ions, and interstitial potassium ions are generated in crystals to reduce migration activation energy of the potassium ions; the electronic conductivity of the fast ion conductor is further lowered through P<5+> doping; the size of a migration channel of the potassium ions is adjusted through small-ion-radius B<3+> doping so as to adapt to rapid migration of the potassium ions; and in the preparation process, the surfaces of K2MgSi5O12particles are modified, and the easy-to-sinter characteristic is formed. Through the collaborative effect, the normal-temperature potassium ion conductivity of the potassium fast ion conductor exceeds5*10<-4> S / cm and is closer to the potassium ion 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): C04B35/20H01M10/0562H01M10/054
CPCC04B35/20C04B2235/3205C04B2235/3217C04B2235/442C04B2235/447C04B2235/6562C04B2235/6567C04B2235/96H01M10/054H01M10/0562H01M2300/0068Y02E60/10
Inventor 水淼舒杰任元龙
Owner NINGBO UNIV
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