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A positive electrode material for mg0.5+y(ni0.5yv0.5yti1-y)2(po4)3 magnesium battery and its preparation method

A cathode material, PO43- technology, used in battery electrodes, secondary batteries, circuits, etc., can solve the problems of high charge density, rapid decomposition, slow kinetic rate, etc.

Inactive Publication Date: 2016-06-15
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(ni0.5yv0.5yti1-y)2(po4)3 magnesium battery and its preparation method
  • A positive electrode material for mg0.5+y(ni0.5yv0.5yti1-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 positive electrode material of the magnesium battery obtained: Mg: Ni: V: Ti: PO 4 3- The molar ratio of MgCO 3 , (NH 4 ) 2 HPO 4 , as well as nickel oxalate and NH 4 VO 3 , the MgCO 3 and (NH 4 ) 2 HPO 4 Dissolved in deionized water, nickel oxalate dissolved in ammonia, NH 4 VO 3 dissolve in hot water;

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

[0030] 2) The solutions obtained in step 1) were mixed, stirred vigorously at 70°C for 8 hours, dehydrated to form a yellow sol, and dried at 100°C to obtain a light yellow xerogel;

[0031] 3) The light yellow xerogel was ground and placed in an atmosphere tube furnace and fed with N 2 -H 2 Mixed gas, pre-calcined at 500°C for 5 hours, and finally calcined at 700°C for 26 hours to obtain black powder that is Mg 0.6 (Ni 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 positive electrode material of the magnesium battery obtained: Mg: Ni: V: Ti: PO 4 3- The molar ratio of MgCO 3 , (NH 4 ) 2 HPO 4 , as well as nickel oxalate and NH 4 VO 3 , the MgCO 3 and (NH 4 ) 2 HPO 4 Dissolved in deionized water, nickel oxalate dissolved in ammonia, NH 4 VO 3 dissolve in hot water;

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

[0035] 2) The solutions obtained in step 1) were mixed, vigorously stirred at 80°C for 4 hours, dehydrated to form a yellow sol, and dried at 80°C to obtain a light yellow xerogel;

[0036] 3) The light yellow xerogel was ground and placed in an atmosphere tube furnace and fed with N 2 -H 2 Mixed gas, pre-calcined at 300°C for 5 hours, and finally calcined at 700°C for 20 hours to obtain black powder that is Mg 0.7 (Ni 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 positive electrode material of the magnesium battery obtained: Mg: Ni: V: Ti: PO 4 3- The molar ratio of MgCO 3 , (NH 4 ) 2 HPO 4 , as well as nickel oxalate and NH 4 VO 3 , the MgCO 3 and (NH 4 ) 2 HPO 4 Dissolved in deionized water, nickel oxalate dissolved in ammonia, NH 4 VO 3 dissolve in hot water;

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

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

[0041] 3) The light yellow xerogel was ground and placed in an atmosphere tube furnace and fed with N 2 -H 2 Mixed gas, pre-calcined at 400°C for 4 hours, and finally calcined at 700°C for 24 hours, to obtain black powder that is Mg 0.8 (Ni 0.15 V 0.15 Ti 0.7 ) 2 (PO 4 ) 3 Magnesium battery cathode material.

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Abstract

The invention discloses an Mg0.5+y(Ni0.5yV0.5yTi1-y)2(PO4)3 magnesium battery cathode material. The cathode material is prepared by a method comprising the following steps: 1) weighing MgCO3, (NH4)2HPO4, nickel oxalate and NH4VO3 according to the mole ratio of Mg to Ni to V to Ti to PO4<3-> in a molecular formula of the obtained magnesium battery cathode material, dissolving MgCO3 and (NH4)2HPO4 in deionized water, dissolving nickel oxalate in ammonia water, dissolving NH4VO3 in hot water, weighing Ti(C4H9O)4 and dissolving Ti(C4H9O)4 with absolute ethyl alcohol according to a proportion of 1 to 4; 2) mixing various solutions obtained in the step 1), stirring the solutions fiercely at 70-80 DEG C for 4-8 hours to dehydrate the solutions to generate yellow sol and drying the yellow sol at 80-100 DEG C to obtain light yellow xerogel; 3) grinding the light yellow xerogel and then putting the ground light yellow xerogel in an atmosphere tube furnace, introducing an N2-H2 gas mixture, presintering the ground light yellow xerogel at 300-500 DEG C for 3-5 hours and finally calcining the product at 700 DEG C for 20-26 hours, thus obtaining black powder, namely the Mg0.5+y(Ni0.5yV0.5yTi1-y)2(PO4)3 magnesium battery cathode material, wherein y is equal to 0.1-0.5. The cathode material prepared by the method has better discharge capacity and capacity retention ratio.

Description

technical field [0001] The invention relates to the field of preparation of secondary batteries, in particular, the invention relates to a Mg 0.5+y (Ni 0.5y V 0.5y Ti 1-y ) 2 (PO 4 ) 3 A cathode material for a magnesium battery and a preparation method thereof. Background technique [0002] In recent years, with the development of electronic consumer goods, electric tools and electric vehicles, the market demand for batteries continues to grow. Among the existing battery systems, zinc-manganese dry batteries have serious 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. The battery development mainly represented by lithium-ion batteries has made great progress and has been widely used in various fields. However, because Li is particularly active, it is easy t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/136H01M4/1397
CPCH01M4/136H01M4/1397H01M4/5825H01M10/054Y02E60/10
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