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Fe<3+> and Ti<4+> co-doped epsilon-LiVOPO4 lithium fast ion conductor and preparation method thereof

A lithium fast ion and lithium ion technology, which is applied in the field of solid lithium fast ion conductor manufacturing, can solve the problems of high energy consumption and high temperature, and achieve the effects of uniform reaction raw materials, high material purity, and reduction of conduction activation energy.

Pending Publication Date: 2021-01-29
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in occasions where the current requirement is high, the conductivity often reaches 5.0×10 -4 Only about S / cm can meet the needs of the normal operation of the battery. In addition, the synthesis temperature of the fast ion conductor is about 1350°C, which is high in temperature and consumes a lot of energy.

Method used

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  • Fe&lt;3+&gt; and Ti&lt;4+&gt; co-doped epsilon-LiVOPO4 lithium fast ion conductor and preparation method thereof
  • Fe&lt;3+&gt; and Ti&lt;4+&gt; co-doped epsilon-LiVOPO4 lithium fast ion conductor and preparation method thereof
  • Fe&lt;3+&gt; and Ti&lt;4+&gt; co-doped epsilon-LiVOPO4 lithium fast ion conductor and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: Li 2 CO 3 : NH 4 h 2 PO 4 : Fe 2 o 3 :TiO 2 : VO 2 According to Li 1.05 Fe 0.05 Ti 0.05 V 0.9 OPO 4 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 200 rev / mins 10 hours, after ball mill finishes, in 60 ℃ of vacuum ovens (gas pressure in oven is at 5 Pa) for 3 hours, take it out and re-grind in an agate mortar for 10 minutes, the ground powder is heated to 500°C at a rate of 5°C / min in an air atmosphere and then cooled with the furnace for 11 hours; The powder was ground again in an agate mortar for 12 minutes, and the ground powder was heated to 600 °C at a rate of 5 °C / min in the air atmosphere for 10 hours, then quickly taken out and cooled in argon at room temperature; Afterwards in a press in a 1×10 7 Pressed into thin slices under the pressure of Pa, put the prepared thin slices into a tube furnace, raise the te...

Embodiment 2

[0016] Embodiment 2: Li 2 CO 3 : NH 4 h 2 PO 4 : Fe 2 o 3 :TiO 2 : VO 2 According to Li 1.1 Fe 0.1 Ti 0.1 V 0.8 OPO 4 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 45 hours, after ball mill finishes, in 120 ℃ of vacuum ovens (gas pressure in the oven is at 90Pa) for 10 hours, and after taking it out, re-grind in an agate mortar for 30 minutes, and the ground powder is heated to 520°C at a rate of 30°C / min in an air atmosphere and then cooled with the furnace after being kept for 20 hours; The powder was ground again in an agate mortar for 30 minutes, and the ground powder was heated to 650 °C at a rate of 14 °C / min in the air atmosphere for 20 hours, then quickly taken out and cooled in argon at room temperature; Afterwards in the press at 8×10 7 Pressed into a thin sheet under the pressure of Pa, put the prepared thin shee...

Embodiment 3

[0017] Embodiment 3: with Li 2 CO 3 : NH 4 h 2 PO 4 : Fe 2 o 3 :TiO 2 : VO 2 According to Li 1.06 Fe 0.06 Ti 0.06 V 0.88 OPO 4 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 400 rev / mins 30 hours, after ball mill finishes, in 75 ℃ of vacuum ovens (gas pressure in the oven is at 100Pa) for 6 hours, take it out and re-grind in an agate mortar for 20 minutes, the ground powder is heated to 500°C at a rate of 20°C / min in an air atmosphere and then cooled with the furnace for 15 hours; The powder was ground again in an agate mortar for 20 minutes, and the ground powder was heated to 600 °C at a rate of 10 °C / min in the air atmosphere for 15 hours, then quickly taken out and cooled in argon at room temperature; Afterwards in the press at 5×10 7 Pressed into thin slices under the pressure of Pa, put the prepared thin slices into a tube furnace,...

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Abstract

The invention relates to a Fe<3+> and Ti<4+> co-doped epsilon-LiVOPO4 lithium fast ion conductor and a preparation method thereof. The Fe<3+> and Ti<4+> co-doped epsilon-LiVOPO4 lithium fast ion conductor is characterized in that the stoichiometric formula is Li1+xFexTiyV-1-x-yOPO4, wherein x is 0.05-0.10, and y is 0.05-0.10. Through the synergistic doping of Fe<3+> and Ti<4+>, the conduction activation energy of lithium ions is greatly reduced, and the activity ability and conductivity of the lithium ions are improved; through two calcining processes, the reaction raw materials are more uniform, and the purity of the obtained material is higher; and the concentration of oxygen vacancies and defects in the material is increased through rapid room-temperature cooling, and conduction of lithium ions is facilitated. Due to the measures, the normal-temperature lithium ion conductivity of the lithium fast ion conductor exceeds 5 * 10<-4> S / cm, and the application of the lithium fast ion conductor is facilitated.

Description

technical field [0001] The invention relates to the field of manufacturing solid lithium fast ion conductors. Background technique [0002] Fast ionic conductors, also known as superionic conductors, refer to a class of ionic conductivity that can be compared with liquid electrolytes in a certain temperature range (10 -6 S / cm) and low ion conductance activation energy (generally less than 0.4eV). Fast ionic conductors have important applications in the fields of energy storage battery electrode materials, gas detectors, solid electrolyte diaphragms, supercapacitors, timers, coulomb counters, and electrochromic displays. [0003] The migration rate of carriers in fast ion conductors is often much lower than the charge transfer on the electrode surface and the ion diffusion rate in the electrode material, which becomes the rate-controlling step in the entire electrode reaction kinetics. Lithium fast-ion conductors are at the heart of developing high-performance applications....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M10/0525C04B35/447C04B35/622
CPCH01M4/5825H01M10/0525C04B35/447C04B35/622C04B2235/3203C04B2235/447C04B2235/3232C04B2235/3239C04B2235/3272C04B2235/96Y02E60/10
Inventor 水淼舒杰任元龙
Owner NINGBO UNIV
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