P<5+>, Al<3+>, Be<2+> and Zn<2+> synergistically doped K2MgSi5O12 potassium fast ion conductor and preparation method thereof

A technology of ionic conductors and ions, which is applied in the field of manufacturing solid potassium fast ionic conductors, to achieve the effect of reducing grain boundary voids

Inactive Publication Date: 2019-10-22
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;, Al&lt;3+&gt;, Be&lt;2+&gt; and Zn&lt;2+&gt; synergistically doped K2MgSi5O12 potassium fast ion conductor and preparation method thereof

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Experimental program
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Embodiment 1

[0011] Embodiment 1: the solid K 2 CO 3 : NH 4 h 2 PO 4 : Al 2 o 3 : SiO 2 : BeO: ZnO: MgO according to K 2.09 MgB 0.05 Al 0.0 5 P 0.02 Zn 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 560°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...

Embodiment 2

[0012] Embodiment 2: the solid K 2 CO 3 : NH 4 h 2 PO 4 :Al 2 o 3 : SiO 2 : BeO: ZnO: MgO according to K 2.36 MgB 0.15 Al 0.1 5 P 0.03 Zn 0.03 Si 4.67 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 500 rev / mins 43 hours, after ball mill finishes, in 110 ℃ of vacuum ovens (gas pressure in the oven is at 15Pa) for 10 hours, take it out and re-grind in an agate mortar for 30 minutes, heat up the ground powder to 650°C at a rate of 30°C / min in an air atmosphere, and then cool it 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,...

Embodiment 3

[0013] Embodiment 3: the solid K 2 CO 3 : NH 4 h 2 PO 4 :Al 2 o 3 : SiO 2 : BeO: ZnO: MgO according to K 2.24 MgB 0.1 Al 0. 1 P 0.02 Zn 0.02 Si 4.78 o 12 The ratio of the stoichiometric molar ratio is evenly mixed, adding quality is the dehydrated alcohol of mixture quality 7%, in ball mill with the rotating speed ball mill of 370 rev / mins 25 hours, after ball mill finishes, in 90 ℃ of vacuum ovens (gas pressure in oven is at 15Pa) for 8 hours, take it out and re-grind in an agate mortar for 20 minutes, the ground powder is heated 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 to 1300°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 sod...

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Abstract

The invention relates to a P<5+>, Al<3+>, Be<2+> and Zn<2+> synergistically doped K2MgSi5O12 potassium fast ion conductor and a preparation method thereof, wherein the stoichiometric formula is K[2+2x+y-z-2m]MgBe[x]Al[y]P[z]Zn[m]Si[5-x-y-z]O12, x is 0.05-0.15, y is 0.05-0.15, z is 0.01-0.03, m is 0.01-0.03, and the conductivity of the potassium ion at a room temperature exceeds 5*10<-4> S / cm. According to the present invention, by partially replacing Si<4+> ions with Al<3+> and Be<2+>, the gap potassium ions are generated in the crystal so as to reduce the potassium ion migration activation energy; through the P<5+> doping, the electron conductivity of the fast ion conductor is further reduced; by doping with the small ionic radius Be<2+>, the size of the potassium ion migration channel isadjusted so as to adapt to the rapid potassium ion migration; by partially replacing the potassium ions with Zn<2+>, the cation vacancy is added so as to increase the potassium ion migration channels; during the preparation, the surface of the K2MgSi5O12 particles is modified so as to form the easy-sintering property; and under the synergistic effects, the room temperature potassium ion conductivity of the potassium fast ion conductor exceeds 5*10<-4> S / cm so as to be close to the potassium ion conductivity of the liquid-state 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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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/16C04B35/622C04B35/626H01M10/054H01M10/0562
CPCC04B35/16C04B35/622C04B35/62605C04B2235/3205C04B2235/3206C04B2235/3217C04B2235/3284C04B2235/34C04B2235/602C04B2235/6562C04B2235/6567C04B2235/6583H01M10/054H01M10/0562H01M2300/0071Y02E60/10
Inventor 水淼舒杰任元龙
Owner NINGBO UNIV
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