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A positive electrode material for mg0.5+y(co0.5yv0.5yti1-y)2(po4)3 magnesium battery and its preparation method

A cathode material, PO43- technology, applied in battery electrodes, chemical instruments and methods, circuits, etc., can solve the problems of high charge density, rapid decomposition, slow kinetic rate, etc.

Active Publication Date: 2016-01-06
QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] relative to Li + Say, Mg 2+ The charge density is high and the solvation is more serious, so most of the positive electrode materials that can be used for lithium secondary batteries cannot be directly applied to magnesium secondary batteries
Lithium is generally used as the positive electrode material of the secondary battery as follows: transition metal sulfide and organic sulfide, transition metal oxide, organic matter or phosphate Mg with NASICION structure 0.5 Ti 2 (PO 4 ) 3 (MTP), but the above-mentioned cathode materials have certain disadvantages. For example, the main disadvantages of transition metal sulfides as cathode materials are: it is difficult to prepare and requires high-temperature synthesis under vacuum or argon atmosphere; it is easy to be corroded compared with oxides, and its Oxidation stability is not ideal
Insufficient oxides as cathode materials for magnesium secondary batteries: Mg 2+ The kinetic rate of intercalation is very slow; for most materials, the Mg 2+ The degree of embedding is low; most embedding materials have poor cycle performance and will decompose quickly in the cycle
For phosphate Mg with NASICION structure 0.5 Ti 2 (PO 4 ) 3 (MTP), Mg 2+ available in Mg 0.5 Ti 2 (PO 4 ) 3 reversible intercalation / deintercalation in , but their reversibility is limited by Mg 2+ Kinetic Limits of Diffusion

Method used

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  • A positive electrode material for mg0.5+y(co0.5yv0.5yti1-y)2(po4)3 magnesium battery and its preparation method
  • A positive electrode material for mg0.5+y(co0.5yv0.5yti1-y)2(po4)3 magnesium battery and its preparation method

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Experimental program
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Effect test

Embodiment 1

[0028] 1) According to the molecular formula of the obtained magnesium battery cathode material, Mg:Co:V:Ti:PO 4 3- The molar ratio of MgCO was weighed 3 , (NH 4 ) 2 HPO 4 , as well as cobalt nitrate and NH 4 VO 3 , the MgCO 3 and (NH 4 ) 2 HPO 4 Soluble in deionized water, cobalt nitrate in citric acid, NH 4 VO 3 dissolve in hot water;

[0029] Weigh Ti (C 4 H 9 O)4 , and the Ti (C 4 H 9 O) 4 dissolve;

[0030] 2) Mix the solutions obtained in step 1), stir vigorously at 70° C. for 8 hours to dehydrate to form a yellow sol, and dry at 100° C. to obtain a pale yellow xerogel;

[0031] 3) Grind the light yellow xerogel and place it in an atmosphere tube furnace and pass N 2 -H 2 The mixed gas was pre-fired at 500 °C for 5 hours, and finally calcined at 700 °C for 26 hours to obtain black powder, which is Mg 0.6 (Co 0.05 V 0.05 Ti 0.9 ) 2 (PO 4 ) 3 Magnesium battery cathode material.

Embodiment 2

[0033] 1) According to the molecular formula of the obtained magnesium battery cathode material, Mg:Co:V:Ti:PO 4 3- The molar ratio of MgCO was weighed 3 , (NH 4 ) 2 HPO 4 , as well as cobalt nitrate and NH 4 VO 3 , the MgCO 3 and (NH 4 ) 2 HPO 4 Soluble in deionized water, cobalt nitrate in citric acid, NH 4 VO 3 dissolve in hot water;

[0034] Weigh Ti (C 4 H 9 O) 4 , and the Ti (C 4 H 9 O) 4 dissolve;

[0035] 2) Mix the solutions obtained in step 1), stir vigorously at 80°C for 4h, dehydrate it to form a yellow sol, and dry at 80°C to obtain a pale yellow xerogel;

[0036] 3) Grind the light yellow xerogel and place it in an atmosphere tube furnace and pass N 2 -H 2 The mixed gas is pre-fired at 300°C for 5h, and finally calcined at 700°C for 20h to obtain a black powder which is Mg 0.7 (Co 0.1 V 0.1 Ti 0.8 ) 2 (PO 4 ) 3 Magnesium battery cathode material.

Embodiment 3

[0038] 1) According to the molecular formula of the obtained magnesium battery cathode material, Mg:Co:V:Ti:PO 4 3- The molar ratio of MgCO was weighed 3 , (NH 4 ) 2 HPO 4 , as well as cobalt nitrate and NH 4 VO 3 , the MgCO 3 and (NH 4 ) 2 HPO 4 Soluble in deionized water, cobalt nitrate in citric acid, NH 4 VO 3 dissolve in hot water;

[0039] Weigh Ti (C 4 H 9 O) 4 , and the Ti (C 4 H 9 O) 4 dissolve;

[0040] 2) Mix the solutions obtained in step 1), stir vigorously at 75°C for 6h, dehydrate it to form a yellow sol, and dry at 90°C to obtain a pale yellow xerogel;

[0041] 3) Grind the light yellow xerogel and place it in an atmosphere tube furnace and pass N 2 -H 2 The mixed gas is pre-fired at 400°C for 4h, and finally calcined at 700°C for 24h to obtain a black powder which is Mg 0.8 (Co 0.15 V 0.15 Ti 0.7 ) 2 (PO 4 ) 3 Magnesium battery cathode material.

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Abstract

The invention discloses a positive electrode material of a Mg<0.5+y>(Co<0.5y>V<0.5y>Ti<1-y>)2(PO4)3 magnesium cell. The positive electrode material is prepared by the following steps: (1) weighing MgCO3, (NH4)2HPO4, cobalt nitrate, and NH4VO3 according to the mole ratio of Mg:Co:V:Ti:PO4<3-> in the molecular formula Mg<0.5+y>(Co<0.5y>V<0.5y>Ti<1-y>)2(PO4)3, dissolving MgCO3 and (NH4)2HPO4 into deionized water, dissolving cobalt nitrate into critic acid, dissolving NH4VO3 into hot water, weighing Ti(C4H9O)4, dissolving Ti(CH4H9O)4 into absolute ethanol according to a ratio of 1:4 of absolute ethanol to Ti(C4H9O)4; (2) mixing all solutions prepared in the step (1), fiercely stirring for 4 to 8 hours at a temperature of 70 to 80 DEG C to dehydrate so as to obtain yellow gel, drying the yellow gel at a temperature of 80 to 100 DEG C so as to obtain light-yellow xerogel; (3) grinding the light-yellow xerogel, placing the powder into an atmosphere tube furnace, introducing N2-H2 mixed gas into the atmosphere tube furnace, pre-burning for 3 to 5 hours at a temperature of 300 to 500 DEG C, and finally burning for 20 to 26 hours at a temperature of 700 DEG C so as to obtain the black powder, namely the positive electrode material of a Mg<0.5+y>(Co<0.5y>V<0.5y>Ti<1-y>)2(PO4)3 magnesium cell, wherein the y is in a range of 0.1 to 0.5. The prepared positive material has a large discharge capacity and capacity retention ratio.

Description

technical field [0001] The present invention relates to the field of preparation of secondary batteries, in particular, the present invention relates to a kind of Mg 0.5+y (Co 0.5y V 0.5y Ti 1-y ) 2 (PO 4 ) 3 Magnesium battery cathode material and preparation method thereof. Background technique [0002] In recent years, with the development of consumer electronics, power tools and electric vehicles, the market demand for batteries has continued to grow. Among the existing battery systems, zinc-manganese dry batteries have prominent mercury pollution, low capacity, and are not suitable for long-term high-current discharge, and the price of zinc is relatively high. Lead-acid and nickel-cadmium batteries contain harmful elements Pb and Cd, which are potentially dangerous to the environment. Significant progress has been made in the development of batteries, mainly represented by lithium-ion batteries, and they are widely used in various fields. However, because Li is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/45H01M4/58
CPCY02E60/10
Inventor 李法强王敏贾国凤彭正军祝增虎诸葛芹时历杰赵有璟李锦丽龚龑王青磊
Owner QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI