Preparation method of nano-micron pyrrhotite soft magnetic material

A technology of pyrrhotite and soft magnetic materials, applied to the magnetic properties of inorganic materials, iron sulfide, etc., can solve the problems of nano-micron pyrrhotite soft magnetic materials that have not been studied or practiced before, and achieve low coercive force , avoid the process, the effect of high purity

Active Publication Date: 2014-12-10
NORTHEASTERN UNIV
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Problems solved by technology

In previous reports, there is no research or practice precedent for the preparation of nano-micro pyrrhotite soft magnetic materials by iron sulfide method

Method used

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  • Preparation method of nano-micron pyrrhotite soft magnetic material
  • Preparation method of nano-micron pyrrhotite soft magnetic material
  • Preparation method of nano-micron pyrrhotite soft magnetic material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Weigh the analytically pure reduced iron powder (Fe) and sublimated sulfur (S) respectively, so that the ratio of Fe to S is 1:1, put them in a mortar and grind them until they are evenly mixed; put the mixed powder in a crucible , sealed and put into a vacuum heating device. Vacuumize the vacuum heating device to 6*10 -2 Pa. According to the heating rate of 5 °C / min, the temperature was raised to 300 °C for 22 hours, and then cooled to room temperature according to the cooling rate of 5 °C / min, and the product in the crucible was taken out to obtain gray-black powder particles.

[0035] Observation by scanning electron microscope (see figure 1 ), the powder crystallizes well, the particle morphology is mainly hexagonal flake and plate shape, and the particle size is between 400nm and 10um. The product obtained by measuring XRD is a pure phase pyrrhotite (see Figure 4 ). The hysteresis loop of the prepared sample was measured with a vibrating sample magnetometer ...

Embodiment 2

[0037] Weigh the analytically pure reduced iron powder (Fe) and sublimated sulfur (S) respectively, so that the ratio of Fe to S is 1:1, put them in a mortar and grind them until they are evenly mixed; put the mixed powder in a crucible , sealed and put into a vacuum heating device. Vacuumize the vacuum heating device to 4.5*10 -2 Pa. According to the heating rate of 5 °C / min, the temperature was raised to 350 °C and kept for 22 hours, and then cooled to room temperature according to the cooling rate of 5 °C / min, and the product in the crucible was taken out to obtain gray-black powder particles.

[0038] Observation by scanning electron microscope shows that the crystal morphology of the powder is mainly hexagonal plate shape, and the particle size is between 350nm and 18um. The product obtained by measuring XRD is a pure phase pyrrhotite (see Figure 5 ). The hysteresis loop of the prepared sample was measured with a vibrating sample magnetometer (VSM), such as Figure ...

Embodiment 3

[0040] Weigh the analytically pure reduced iron powder (Fe) and sublimated sulfur (S) respectively, so that the ratio of Fe to S is 1:1, put them in a mortar and grind them until they are evenly mixed; put the mixed powder in a crucible , sealed and put into a vacuum heating device. Vacuumize the vacuum heating device to 3.2*10 -2 Pa. According to the heating rate of 5 °C / min, the temperature was raised to 400 °C for 22 hours, and then cooled to room temperature according to the cooling rate of 5 °C / min, and the product in the crucible was taken out to obtain gray-black powder particles.

[0041] Observation by a scanning electron microscope shows that the powder crystallizes in a hexagonal plate shape with a particle size between 800nm ​​and 30um. The product obtained by measuring XRD is a pure phase pyrrhotite (see Figure 5 ). The hysteresis loop of the prepared sample was measured with a vibrating sample magnetometer (VSM), such as Figure 9 shown. The magnetic perfo...

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Abstract

The invention provides a preparation method of a nano-micron pyrrhotite soft magnetic material. The preparation method comprises the following steps: by using reduced iron powder (Fe) and sublimed sulfur as main raw materials, and grinding the two raw materials in a certain proportion until the two raw materials are uniformly mixed; heating for a certain time under a certain temperature condition; performing heat preservation and cooling, thereby finally obtaining the ash black pyrrhotite soft magnetic powered material with crystals developing well. The material has the characteristics of low residual magnetism and low coercivity. The basic expression of the components is Fe1-xS (x is greater than or equal to 0 but less than or equal to 0.223). By using materials which are low in price and simple and easily available, the pyrrhotite soft magnetic material which is high in purity, uniform in granular distribution and low in coercivity and residual magnetism is manually prepared by virtue of an iron-sulfur compound method and can be used for satisfying the actual demand of the magnetic material. The soft magnetic material is the magnetic material with low residual magnetism and low coercivity, has the characteristics of easiness for magnetization and easiness for demagnetization, can be widely applied to electrical equipment and electronic equipment and has actual application value.

Description

technical field [0001] The invention relates to a method for preparing a nano-micro pyrrhotite soft magnetic material, in particular to a method for preparing a multifunctional nano-micro composite material by a medium-low temperature iron vulcanization method. Background technique [0002] Soft magnetic material is a kind of magnetic material with low coercive force and low remanence. It has the characteristics of easy magnetization and easy demagnetization, and is widely used in electrical equipment and electronic equipment. With the rapid development of science and technology, radar, television broadcasting, and the creation of integrated circuits have put forward higher requirements for soft magnetic materials. Multi-variety, easy-to-produce, and low-cost soft magnetic materials are an inevitable trend in market demand. [0003] As an important member of magnetic materials, iron sulfide has unique physical properties. However, natural pyrrhotite, which exists widely in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/12H01F1/34
Inventor 黄菲杨多高文元
Owner NORTHEASTERN UNIV
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