CN103601251B

CN103601251B - Single-phase CaFe2O4 micro-nano hierarchy material with surface texture and preparation method thereof

Info

Publication number: CN103601251B
Application number: CN201310633146.5A
Authority: CN
Inventors: 王海; 王辛瑜; 王林江; 方亮
Original assignee: Guilin University of Technology
Current assignee: SUZHOU COFFMAN MACHINERY Co.,Ltd.
Priority date: 2013-12-03
Filing date: 2013-12-03
Publication date: 2014-12-24
Anticipated expiration: 2033-12-03
Also published as: CN103601251A

Abstract

The invention discloses a single-phase CaFe2O4 micro-nano hierarchy material with surface texture and a preparation method thereof. The diameter of each separate particle of the single-phase CaFe2O4 micro-nano hierarchy material with surface texture is 1 to 6 mu m, and the surface of each particle has obvious step-like texture. The preparation method comprises the following steps (1) mixing 2.0 to 0.5 mol of calcium oxalate and 4 to 1 mol of a ferric ammonium oxalate crystal, adding 30 to 40 ml of a mixed solvent of deionized water and anhydrous glycol in a volume ratio of 0.5-1 1-5 and carrying out stirring with a magnetic stirrer for 1 to 3 h; and (2) adding 1 to 3 g of oxalic acid into a solution obtained in the step (1), continuing stirring for 0.5 to 1 h, transferring an obtained mixture to a stainless steel reaction vessel with a polytetrafluoroethylene substrate, carrying out a hydrothermal reaction at a temperature of 180 to 230 DEG C for 14 to 24 h, then carrying out filtration, washing a precipitate with distilled water 2 to 3 times and drying the precipitate at normal temperature so as to obtain the single-phase CaFe2O4 micro-nano hierarchy material with surface texture. The method provided by the invention has the advantages of simple operation, low cost, low energy consumption, high product purity and capacity of large scale synthesis of the material.

Description

There is the single-phase CaFe of Surface Texture 2o 4micro-nano grading structure material and preparation method thereof

Technical field

The present invention relates to technical field of material chemistry, particularly a kind of single-phase CaFe with Surface Texture ₂o ₄micro-nano grading structure material and preparation method thereof, this material can be used as lithium ion battery electrode material.

Background technology

At present, the micro-nano material with special hierarchy is widely used in photochemical catalysis, the field such as lithium ion battery and solar cell and be subject to the common concern of domestic and international industry member and academia, but, for CaFe ₂o ₄this ternary oxide material, but gives few concern both at home and abroad.At present, the main policies that most of synthesis technique adopts is solid phase method based on ceramic post sintering theory and obtains irregular micron particle.In order to be provided a kind of novel C aFe from now on ₂o ₄tachnical storage carried out by material, and solve the unicity problem of this material of synthesis at present, the present invention aims to provide a kind of easy liquid phase method and obtains the single-phase CaFe with Surface Texture ₂o ₄micro-nano grading structure material.

Summary of the invention

The object of the present invention is to provide a kind of technique simple, the single-phase CaFe of what cost was low have Surface Texture ₂o ₄micro-nano grading structure material and preparation method thereof, the method is easy and simple to handle, cost is low, it is low to consume energy, and the product purity obtained is high, can synthesize on a large scale.

The single-phase CaFe with Surface Texture that the present invention relates to ₂o ₄the diameter of micro-nano grading structure material individual particle is 1-6 micron, and there is the texture of some obvious similar steps on the surface of each particle.

There is the single-phase CaFe of Surface Texture ₂o ₄preparation method's concrete steps of micro-nano grading structure material are:

(1) by 2.0-0.5 molar oxalic acid calcium and the mixing of 4-1 molar oxalic acid ammonium iron crystal, adding 30-40mL volume ratio is the deionized water of 0.5-1:1-5 and the mixed solvent without water glycol, with magnetic stirrer 1-3 hour.

(2) 1-3 gram of oxalic acid is added in the solution obtained in step (1), continuing to stir was proceeded in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate after 0.5-1 hour, 180-230 DEG C of hydro-thermal reaction 14-24 hour, filter, by precipitation with after distilled water wash 2-3 time, namely Air drying obtains the described single-phase CaFe with Surface Texture ₂o ₄micro-nano grading structure material.

The inventive method is easy and simple to handle, cost is low, use simple method to synthesize first has the single-phase CaFe of Surface Texture ₂o ₄micro-nano grading structure material, has enriched Material Field, and is that the fields such as electricity, magnetics, semi-conductor provide new material.

Accompanying drawing explanation

Fig. 1 is the single-phase CaFe with Surface Texture of the embodiment of the present invention 1 ₂o ₄the x-ray diffraction pattern of micro-nano grading structure material.

Fig. 2 is the single-phase CaFe with Surface Texture of the embodiment of the present invention 1 ₂o ₄the Flied emission scintigram of micro-nano grading structure material.

Embodiment

embodiment 1:

(1) by 2 molar oxalic acid calcium and the mixing of 4 molar oxalic acid ammonium iron crystal, 10 mL deionized waters and the 20mL mixed solvent without water glycol is added, by magnetic stirrer 2 hours.

(2) 1 gram of oxalic acid is added in the solution obtained in step (1), continuing stirring was proceeded in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate after 0.5 hour, 180 DEG C of hydro-thermal reactions 14 hours, filter, by precipitation with after distilled water wash 2 times, namely Air drying obtains the single-phase CaFe with Surface Texture ₂o ₄micro-nano grading structure material.

There is the single-phase CaFe of Surface Texture ₂o ₄the x-ray diffraction pattern of micro-nano grading structure material is shown in Fig. 1, has the single-phase CaFe of Surface Texture ₂o ₄the Flied emission scintigram of micro-nano grading structure material is shown in Fig. 2.

embodiment:

(1) by 0.5 molar oxalic acid calcium and the mixing of 1 molar oxalic acid ammonium iron crystal, 8 mL deionized waters and the 32mL mixed solvent without water glycol is added, by magnetic stirrer 3 hours.

(2) 3 grams of oxalic acid are added in the solution obtained in step (1), continuing stirring was proceeded in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate after 1 hour, 230 DEG C of hydro-thermal reactions 24 hours, filter, by precipitation with after distilled water wash 3 times, namely Air drying obtains the described single-phase CaFe with Surface Texture ₂o ₄micro-nano grading structure material.

Claims

1. one kind has the single-phase CaFe of Surface Texture ₂o ₄micro-nano grading structure material, is characterized in that the single-phase CaFe with Surface Texture ₂o ₄the diameter of micro-nano grading structure material individual particle is 1-6 micron, and there is the texture of some obvious similar steps on the surface of each particle.

2. the single-phase CaFe with Surface Texture according to claim 1 ₂o ₄the preparation method of micro-nano grading structure material, is characterized in that concrete steps are:

(1) by 2.0-0.5 molar oxalic acid calcium and the mixing of 4-1 molar oxalic acid ammonium iron crystal, adding 30-40mL volume ratio is the deionized water of 0.5-1:1-5 and the mixed solvent without water glycol, with magnetic stirrer 1-3 hour;