Method for preparing MxR1-xFe2O4 nanometer powder quickly

A mxr1-xfe2o4, nano-powder technology, applied in the field of soft magnetic ferrite nano-materials, can solve the problems of increased energy consumption, poor reproducibility, and inability to industrialize production, etc., to reduce grinding time and increase single-time processing capacity , the effect of avoiding experimental error

Inactive Publication Date: 2013-01-23
SHANDONG UNIV OF TECH
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Problems solved by technology

This is also the reason why the traditional low-temperature solid-state reaction preparation technology uses manual grinding to control the wall sticking phenomenon instead of mechanical grinding.
However, due to manual grinding, there will be more errors in the experimental process, and the single processing volume is small, and there are certain differences in the experimental conclusions obtained by different operators. The reproducibility is not good, resulting in unstable product performance and cannot be industrialized. Production
Moreover, the subsequent heat treatment process will cause the agglomeration and growth of particles, resulting in uneven particle size and increasing energy consumption.
The traditional high-energy ball milling to prepare soft magnetic ferrite nanopowder is to use Fe 2 o 3 And other oxide powders as raw materials usually require a longer high-energy ball milling time, generally more than 10 hours, to cause the reactants to pulverize the mechanochemical effect, generate the target product, increase energy consumption, and the product purity is not high

Method used

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  • Method for preparing MxR1-xFe2O4 nanometer powder quickly
  • Method for preparing MxR1-xFe2O4 nanometer powder quickly

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: The grinding medium of the planetary mill adopts alumina balls. The diameters of the large, medium and small balls are 12mm, 10mm and 5mm respectively, and the numbers are 68, 40 and 160 respectively. The specific steps are:

[0018] (1) FeSO 4 ·7H 2 O and NiSO 4 ·6H 2 O Moore than Ni 2+ : Fe 2+ = 1:2 weighed and placed in a planetary mill, mixed and ground for 5 minutes;

[0019] (2) by Fe 2+ :OH - Add NaOH solid at a molar ratio of 1:3, and the ball-to-material ratio is 3:1. The planetary mill dry grinding process is used in two stages. The first stage is ground for 8 minutes. The grinding medium and materials in the grinding tank are taken out at the same time and dried naturally. 10 hours, then carry out the second stage of grinding for 10 minutes;

[0020] (3) Add deionized water, the mass ratio concentration of the prepared slurry is 40%, and use the planetary mill wet grinding process to grind for 5min; the slurry is centrifuged and washed w...

Embodiment 2

[0022] Embodiment 2: The grinding medium of the planetary mill adopts alumina balls, the diameters of the large balls, the middle balls and the small balls are respectively 12mm, 10mm and 5mm, and the numbers are respectively 90, 30 and 100. The specific steps are:

[0023] (1) FeSO 4 ·7H 2 O, NiSO 4 ·6H 2 O and ZnSO 4 ·7H 2 O Moore than Ni 2+ : Zn 2+ : Fe 2+ =0.5:0.5:2 Weigh and place in a planetary mill, mix and grind for 5 minutes;

[0024] (2) by Fe 2+ :OH -Add NaOH solid at a molar ratio of 1:3, and the ball-to-material ratio is 4:1. The planetary mill dry grinding process is used in two stages. The first stage is ground for 10 minutes. The grinding medium and materials in the grinding tank are taken out at the same time and dried naturally. After 10 hours, carry out the second stage of grinding for 5 minutes;

[0025] (3) Add deionized water, the mass ratio concentration of the prepared slurry is 45%, and use the planetary mill wet grinding process to grind fo...

Embodiment 3

[0027] Embodiment 3: The grinding medium of the planetary mill adopts alumina balls. The diameters of the large, medium and small balls are 12mm, 10mm and 5mm respectively, and the numbers are 70, 60 and 120 respectively. The specific steps are:

[0028] (1) FeSO 4 ·7H 2 O, NiSO 4 ·6H 2 O and MnSO 4 ·H 2 O Moore than Ni 2+ :Mn 2+ : Fe 3+ =0.95:0.05:2 Weigh and place in a planetary mill for mixing and grinding for 3 minutes;

[0029] (2) by Fe 2+ :OH - Add NaOH solid at a molar ratio of 1:3, and the ball-to-material ratio is 3:1. The planetary mill dry grinding process is used in two stages. The first stage is ground for 8 minutes. The grinding medium and materials in the grinding tank are taken out at the same time and dried naturally. 10 hours, then carry out the second stage of grinding for 10 minutes;

[0030] (3) Add deionized water, the mass ratio concentration of the prepared slurry is 45%, and use the planetary mill wet grinding process to grind for 8min; the...

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Abstract

The invention provides a method for preparing MxR1-xFe2O4 nanometer powder quickly, which is characterized by comprising the following steps of: (1) mixing ferrous sulfate heptahydrate and one or more of crystal water-containing metal sulfates according to a molar ratio of M<2+> to R<2+> to Fe<3+> of x:(1-x):2 in a chemical structural formula MxR1-xFe2O4, and putting the mixture in a planet mill,and mixing and grinding for 3 to 5 minutes, wherein x is equal to 0.5 to 1; (2) adding a NaOH solid according to a molar ratio of Fe<2+> to OH<-> of 1:3, performing dry grinding by using the planet mill at two stages, wherein the dry grinding is performed for 8 to 10 minutes at the first stage, and is performed for 5 to 10 minutes at the second stage; and (3) adding deionized water, so that the mass ratio concentration of slurry is between 40 and 50 percent, performing wet grinding by using the planet mill for 5 to 10 minutes, and performing centrifugal separation, washing and drying sequentially to obtain the MxR1-xFe2O4 nanometer powder. In the method, the MxR1-xFe2O4 nanometer powder with an excellent crystal structure and high purity can be synthesized directly without calcining, so the method is high in operability and repeatability, the phenomenon of unstable hand lapping process of mortars in the conventional low-temperature solid-phase reaction method is prevented, energy consumption is reduced, and the method is suitable for industrial production.

Description

technical field [0001] The present invention relates to a M x R 1-x Fe 2 o 4 The invention relates to a rapid preparation method of nanometer powder, which belongs to the technical field of soft magnetic ferrite nanomaterials. Background technique [0002] At present, soft magnetic ferrite nanopowders are prepared by low-temperature solid-state reaction, which adopts the method of artificial grinding, so that the reactant completes part of the solid-state reaction in an agate mortar to form a precursor. Moreover, in the process of grinding and preparation, there will be a phenomenon of strong adhesion to the wall of the grinder, which will cause the reaction to fail or be incomplete. Therefore, the subsequent low-temperature heat treatment process is usually used to heat the precursor to promote the solid phase reaction. Completely, the desired product is prepared. This is also the reason why the traditional low-temperature solid-state reaction preparation technology us...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/02B82Y40/00C04B35/26C04B35/28C04B35/30
Inventor 焦万丽张磊
Owner SHANDONG UNIV OF TECH
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