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Preparation method of transition metal fluoride

A transition metal and transition metal salt technology, applied in metal material coating process, nickel halide, iron halide and other directions, can solve the problem of uncontrollable purity of synthetic materials, and achieve the effects of low cost, simple raw materials and good crystallinity

Active Publication Date: 2018-12-25
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the commonly used synthesis methods of transition metal fluorides are: (1) CoF synthesis by electrochemical plating 2 materials, and used in supercapacitors [Chem.Commun., 2014, 50, 7067-7070.], however, the purity of materials synthesized in this way cannot be controlled, and in addition, a large amount of fluorine-containing waste liquid will be generated; (2 ) Hydrothermal synthesis of cobalt-nickel fluoride / carbon nanotube composite materials, there are many steps for synthesizing materials, and a large amount of waste liquid is formed at the same time [CN201510404046.4]; (3) Hydrosynthesis metallurgy produces nickel fluoride, the material has purity and composition There are many problems such as waste liquid and waste slag formed by this [CN201410551409.2]; (4) NiF is prepared by direct current arc plasma evaporation 2 [J.Power Sources,2017,366,131-142.] Co-precipitation with ionic liquids to prepare CoF 2 [J.Power Sources 2016,303,49-56.], high temperature pyrolysis Fe(CF 3 COO) 2 (CF 3 COOH) 2 Preparation of FeF 2 [J.Mater.Chem.A,2017,5,7383–7393], Pyrolysis of CoSiF 6 Preparation of CoF 2 [Small 2015,11,No.38,5164–5173], Preparation of CoF by Pyrolysis of Cobalt Hexafluoroacetylacetonate Hydrate 2 Preparation of FeF with Iron Thienoyltrifluoroacetonate 2 Used in the field of lithium-ion power supplies, but the cost of such raw materials is high and cannot be mass-produced

Method used

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  • Preparation method of transition metal fluoride
  • Preparation method of transition metal fluoride
  • Preparation method of transition metal fluoride

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Preparation of cobalt fluoride supported on nickel foam: deposit 100mg of cobalt hydroxide precursor on nickel foam, and place 2g of ammonium fluoride upstream and downstream, place it in an inert atmosphere tube furnace, and conduct pyrolysis treatment at 350°C for 120 Minutes later, the mixture was washed with deionized water, filtered and dried to obtain cobalt fluoride supported on nickel foam.

[0024] figure 1 This is the XRD pattern of the nickel foam material loaded with cobalt fluoride. It can be seen from the figure that only the characteristic peaks of cobalt fluoride and nickel foam exist, and there are no other impurity phases, which proves that the cobalt fluoride material has been successfully synthesized.

Embodiment 2

[0026] Preparation of cobalt fluoride / nickel fluoride: place 100mg of transition metal precursor (cobalt nitrate and nickel nitrate molar ratio is 1:1) and 2g of ammonium fluoride upstream and downstream, and place them in an inert atmosphere tube furnace at 350°C After pyrolysis treatment for 120 minutes, the mixture was washed with deionized water, filtered and dried to obtain a cobalt fluoride / nickel fluoride mixture.

[0027] figure 2 is the XRD pattern of the cobalt fluoride / nickel fluoride mixture material obtained, it can be seen from the figure that only the characteristic peaks of the cobalt fluoride / nickel fluoride mixture exist, and the cobalt fluoride / nickel fluoride mixture material is synthesized in one step.

Embodiment 3

[0029] Preparation of cobalt fluoride: mix 100mg of cobalt oxide precursor and 500mg of ammonium fluoride, place in an inert atmosphere tube furnace, and after pyrolysis treatment at 350°C for 120 minutes, wash the mixture with deionized water, filter and dry Cobalt fluoride can be obtained.

[0030] image 3 It is the XRD figure of the prepared cobalt fluoride, it can be seen from the figure that only the characteristic peaks of cobalt fluoride exist.

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Abstract

The invention discloses a preparation method of a transition metal fluoride, comprising: mixing a transition metal precursor and ammonium fluoride in a mass ratio of 1:(5-20) or placing them with oneupstream and the other downstream, pyrolyzing at 250 DEG C and above, washing with water, filtering, and drying to obtain the transition metal fluoride. The preparation method is simple to perform; afluorine source and transition metal material herein are simple; the cost is low; the transition metal fluoride has good crystallizing performance and is suitable for batch production.

Description

technical field [0001] The invention belongs to the technical field of transition metal compound preparation, and relates to a preparation method of transition metal fluoride. Background technique [0002] Metal fluorides have a wide range of applications in catalytic synthesis, coating protection, power storage and conversion. For example, use cobalt fluoride to prepare sulfur hexafluoride, etc. [CN201210589193.X]; metal fluorides are applied on the surface of magnetic bodies, and the magnetic properties of materials are improved by coating transition metal fluorides [CN200810008924.0]; in hydrogen storage composite materials , transition metal fluorides can also effectively store and release hydrogen at lower temperatures, such as [CN201711123813.X] and [CN201310717737.0]; in lithium-ion battery cathode materials, use iron trifluoride and lithium hexafluoroferrate The composite material effectively enhances the stability of the cathode material [CN201710426552.2]. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/08C01G53/08C01G49/10C23C18/12
CPCC23C18/1204C01G49/10C01G51/08C01G53/08C01P2002/72C01P2004/82
Inventor 冯立纲刘宗方波王复龙郁旭
Owner YANGZHOU UNIV
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