CN105957681A - Preparation method of soft magnetic material - Google Patents

Preparation method of soft magnetic material Download PDF

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Publication number
CN105957681A
CN105957681A CN201610242698.7A CN201610242698A CN105957681A CN 105957681 A CN105957681 A CN 105957681A CN 201610242698 A CN201610242698 A CN 201610242698A CN 105957681 A CN105957681 A CN 105957681A
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soft magnetic
powder
crucible
dried object
preparation
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CN201610242698.7A
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CN105957681B (en
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潘艳丽
薛培龙
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Shandong spring magnetoelectric Technology Co., Ltd.
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CHANGZHOU DA AO NEW MSTAR TECHNOLOGY Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/33Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials mixtures of metallic and non-metallic particles; metallic particles having oxide skin

Abstract

Belonging to the technical field of magnetic material preparation, the invention relates to a preparation method of a soft magnetic material. The method consists of: firstly conducting ball milling on quartz sand, blast furnace slag and other substances into powder, then soaking the powder in a sodium hydroxide solution, conducting filtration and drying, and mixing the dried material with ferric oxide and aluminum powder, inserting a magnesium ribbon, igniting the magnesium ribbon to carry out reaction, then carrying out annealing, cold press molding and other processes so as to obtain the soft magnetic material that is coated with a layer of silicon dioxide and other insulating substances and contains iron and other magnetic substances. The soft magnetic material prepared by the method provided by the invention has saturation magnetic induction of greater than 1.3 and can resist high temperature up to 700-800DEG C.

Description

A kind of preparation method of soft magnetic materials
Technical field
The present invention relates to the preparation method of a kind of soft magnetic materials, belong to magnetic material preparing technical field.
Background technology
Soft magnetic materials refers to a class soft magnetic materials that is the most independent between magnetic powder and that coupled together by insulating layer material.The outstanding advantages of this soft magnetic materials is to have low iron loss and Three-Dimensional Isotropic character under AC magnetic field.Therefore the parts that a lot of conventional soft magnetic materials is difficult to be can prepare, switching magnetic-resistance, resonant inductance, anti-lock brake sensor, electromagnetic actuator device, brshless DC motor, rotating machinery, the field such as low-frequency filter had been supplied in.The preparation technology of compound soft magnetic material is typically metal or alloy Magnaglo Surface coating inorganic matter and organic electric insulation layer, or use Magnaglo matrix high resistivity continuous fiber complex method to form composite soft-magnetic powder body, then use powder metallurgy compaction process to be prepared as closely knit block soft magnetic materials.
In soft magnetic materials preparation process, need to be applied more than the pressure of 800MPa, to reach the compacted density needed, but meet good saturation induction density and pcrmeability again simultaneously, being accomplished by anneals to the compound soft magnetic material containing Coated with Organic Matter layer removes the residual stress of material, owing to pure Organic substance is higher as the compound soft magnetic material eddy-current loss of electric insulation layer, it is generally therefore all outside phosphate coating, be coated with organic insulator again.But generally phosphate coating non-refractory, so it is difficult to effectively remove its residual stress.For the compound soft magnetic material of existing inorganic matter clad, the insulating properties of clad does not reaches requirement, and the existing clad environmental pollution containing P or S is serious, then occurs in that and uses SiO2, MgO, SiO2Powder, Al2O3Powder, ZrO2Inorganic insulation layer prepared by the mixture of powder and mica powder is as inorganic matter clad, and inorganic insulation layer generally has high-temperature stable, the shortcoming which overcoming the usual non-refractory of Coated with Organic Matter layer.But existing inorganic insulation layer also has shortcoming, relatively big and inorganic insulation layer the thermal coefficient of expansion of of the thermal coefficient of expansion difference of inorganic insulation layer and magnetic powder itself can not change, thermal stress can be produced in magnetic powder at the bigger environment of the temperature difference or during long-time use, cause the compound soft magnetic material of inorganic matter clad cannot have excellent magnetic property.These problems all govern development and the application of compound soft magnetic material.There is the problem that magnetic property difference cannot prepare, with prior art, the compound soft magnetic material having excellent magnetic characteristics in the most existing compound soft magnetic material.
Summary of the invention
The technical problem to be solved: for the soft magnetic materials non-refractory containing Organic substance or inorganic matter clad, it is difficult to effectively remove residual stress or the problem cannot with excellent magnetic property, provide a kind of by quartz sand, the material ball grinds such as blast furnace slag, it is placed in sodium hydroxide solution immersion again, filter, it is dried, and by dried object and iron sesquioxide, aluminium powder mixes, and insert magnesium ribbon, light magnesium ribbon, after making it react, it is annealed, the processes such as cold moudling, prepare the megohmite insulants such as outer cladding layer of silicon dioxide, the soft magnetic materials of interior iron content equimagnetic material.The saturated magnetic strength of soft magnetic materials prepared by the present invention > 1.3, high temperature resistant up to 700~800 DEG C.
For solving above-mentioned technical problem, the present invention uses the technical scheme as described below to be:
(1) count by weight, weigh 40~50 parts of quartz sands, 30~35 parts of blast furnace slags, 20~25 parts of calcites respectively, after being mixed uniformly, after it being washed with clear water, dry, be placed in ball milling in ball mill and cross 200 mesh sieves, obtain mixed-powder;
(2) it is to soak after 1~2h in 2.0mol/L sodium hydroxide solution that the mixed-powder of above-mentioned preparation is placed in mass concentration, filter, and it is washed with deionized filtrate, until the deionized water after Xi Di is neutral, it is to be dried 1~2h in 70~80 DEG C of baking ovens that washings is placed in temperature again, obtains dried object;
(3) dried object of above-mentioned preparation is placed in crucible, and in crucible, add dried object quality 60~75% iron sesquioxide and dried object quality 50~55% aluminium powder, after being uniformly mixed, magnesium ribbon by 7~8cm inserts in mixture, lighting magnesium ribbon, and be slowly introducing nitrogen simultaneously in crucible, control nitrogen being passed through speed is 17~25mL/s, after being passed through 40~55min so that it is continue reaction 1~2h;
(4), after question response terminates, mixture in crucible is cooled to 100~120 DEG C with the speed of 2 DEG C/min, insulation reaction 1~2h, then be placed in firm compression mould and carry out cold moudling, controlling pressure is 30~50MPa, and the time is 3~5min;
(5) after cold moudling, then being placed in calcining furnace, and calcine under nitrogen protection, controlling calcining heat is 700~800 DEG C, after calcining 30~40min, cools to room temperature with the furnace, can be prepared into soft magnetic materials.
The saturated magnetic strength of copper zinc ferrite soft magnetic materials that the present invention prepares > 1.3, Curie temperature is 700~800 DEG C, and resistivity is 1.30~1.42 μ Ω m, and saturation field intensity is 33000~32500A/m, and pcrmeability is 115~130mH/m.
The present invention is compared with additive method, and Advantageous Effects is:
(1) the saturated magnetic strength of soft magnetic materials that prepared by the present invention > 1.3, high temperature resistant up to 700~800 DEG C;
(2) preparation process is simple, required low cost.
Detailed description of the invention
Count the most by weight, weigh 40~50 parts of quartz sands, 30~35 parts of blast furnace slags, 20~25 parts of calcites respectively, after being mixed uniformly, after it being washed with clear water, dry, be placed in ball milling in ball mill and cross 200 mesh sieves, obtain mixed-powder;It is to soak after 1~2h in 2.0mol/L sodium hydroxide solution that the mixed-powder of above-mentioned preparation is placed in mass concentration again, filter, and be washed with deionized filtrate, until the deionized water after Xi Di is neutral, it is to be dried 1~2h in 70~80 DEG C of baking ovens that washings is placed in temperature again, obtains dried object;Then the dried object of above-mentioned preparation is placed in crucible, and in crucible, add dried object quality 60~75% iron sesquioxide and dried object quality 50~55% aluminium powder, after being uniformly mixed, magnesium ribbon by 7~8cm inserts in mixture, lighting magnesium ribbon, and be slowly introducing nitrogen simultaneously in crucible, control nitrogen being passed through speed is 17~25mL/s, after being passed through 40~55min so that it is continue reaction 1~2h;After question response terminates, mixture in crucible is cooled to 100~120 DEG C with the speed of 2 DEG C/min, insulation reaction 1~2h, then be placed in firm compression mould and carry out cold moudling, controlling pressure is 30~50MPa, and the time is 3~5min;After cold moudling, then being placed in calcining furnace, and calcine under nitrogen protection, controlling calcining heat is 700~800 DEG C, after calcining 30~40min, cools to room temperature with the furnace, can be prepared into soft magnetic materials.
Example 1
Count the most by weight, weigh 50 parts of quartz sands, 30 parts of blast furnace slags, 20 parts of calcites respectively, after being mixed uniformly, after it being washed with clear water, dry, be placed in ball milling in ball mill and cross 200 mesh sieves, obtain mixed-powder;It is to soak after 2h in 2.0mol/L sodium hydroxide solution that the mixed-powder of above-mentioned preparation is placed in mass concentration again, filter, and be washed with deionized filtrate, until the deionized water after Xi Di is neutral, it is to be dried 2h in 80 DEG C of baking ovens that washings is placed in temperature again, obtains dried object;Then the dried object of above-mentioned preparation is placed in crucible, and in crucible, add dried object quality 75% iron sesquioxide and dried object quality 55% aluminium powder, after being uniformly mixed, the magnesium ribbon of 8cm is inserted in mixture, lighting magnesium ribbon, and be slowly introducing nitrogen simultaneously in crucible, control nitrogen being passed through speed is 25mL/s, after being passed through 55min so that it is continue reaction 2h;After question response terminates, mixture in crucible is cooled to 120 DEG C with the speed of 2 DEG C/min, insulation reaction 2h, then be placed in firm compression mould and carry out cold moudling, control pressure is 50MPa, and the time is 5min;After cold moudling, then being placed in calcining furnace, and calcine under nitrogen protection, controlling calcining heat is 800 DEG C, after calcining 40min, cools to room temperature with the furnace, can be prepared into soft magnetic materials.After testing, the saturated magnetic strength of soft magnetic materials prepared by the present invention is 1.4, high temperature resistant up to 700 DEG C;Preparation process is simple, required low cost.
Example 2
Count the most by weight, weigh 40 parts of quartz sands, 35 parts of blast furnace slags, 25 parts of calcites respectively, after being mixed uniformly, after it being washed with clear water, dry, be placed in ball milling in ball mill and cross 200 mesh sieves, obtain mixed-powder;It is to soak after 1h in 2.0mol/L sodium hydroxide solution that the mixed-powder of above-mentioned preparation is placed in mass concentration again, filter, and be washed with deionized filtrate, until the deionized water after Xi Di is neutral, it is to be dried 1h in 70 DEG C of baking ovens that washings is placed in temperature again, obtains dried object;Then the dried object of above-mentioned preparation is placed in crucible, and in crucible, add dried object quality 60% iron sesquioxide and dried object quality 50% aluminium powder, after being uniformly mixed, the magnesium ribbon of 7cm is inserted in mixture, lighting magnesium ribbon, and be slowly introducing nitrogen simultaneously in crucible, control nitrogen being passed through speed is 17mL/s, after being passed through 40min so that it is continue reaction 1h;After question response terminates, mixture in crucible is cooled to 100 DEG C with the speed of 2 DEG C/min, insulation reaction 1h, then be placed in firm compression mould and carry out cold moudling, control pressure is 30MPa, and the time is 3min;After cold moudling, then being placed in calcining furnace, and calcine under nitrogen protection, controlling calcining heat is 700 DEG C, after calcining 30min, cools to room temperature with the furnace, can be prepared into soft magnetic materials.The saturated magnetic strength of soft magnetic materials prepared by the present invention is 1.5, high temperature resistant up to 750 DEG C;Preparation process is simple, required low cost.
Example 3
Count the most by weight, weigh 45 parts of quartz sands, 30 parts of blast furnace slags, 25 parts of calcites respectively, after being mixed uniformly, after it being washed with clear water, dry, be placed in ball milling in ball mill and cross 200 mesh sieves, obtain mixed-powder;It is to soak after 2h in 2.0mol/L sodium hydroxide solution that the mixed-powder of above-mentioned preparation is placed in mass concentration again, filter, and be washed with deionized filtrate, until the deionized water after Xi Di is neutral, it is to be dried 2h in 75 DEG C of baking ovens that washings is placed in temperature again, obtains dried object;Then the dried object of above-mentioned preparation is placed in crucible, and in crucible, add dried object quality 70% iron sesquioxide and dried object quality 52% aluminium powder, after being uniformly mixed, the magnesium ribbon of 7cm is inserted in mixture, lighting magnesium ribbon, and be slowly introducing nitrogen simultaneously in crucible, control nitrogen being passed through speed is 20mL/s, after being passed through 50min so that it is continue reaction 2h;After question response terminates, mixture in crucible is cooled to 110 DEG C with the speed of 2 DEG C/min, insulation reaction 2h, then be placed in firm compression mould and carry out cold moudling, control pressure is 40MPa, and the time is 4min;After cold moudling, then being placed in calcining furnace, and calcine under nitrogen protection, controlling calcining heat is 750 DEG C, after calcining 35min, cools to room temperature with the furnace, can be prepared into soft magnetic materials.The saturated magnetic strength of soft magnetic materials prepared by the present invention is 1.3, high temperature resistant up to 800 DEG C;Preparation process is simple, required low cost.

Claims (1)

1. the preparation method of a soft magnetic materials, it is characterised in that concrete preparation process is:
(1) count by weight, weigh 40~50 parts of quartz sands, 30~35 parts of blast furnace slags, 20~25 parts of calcites respectively, after being mixed uniformly, after it being washed with clear water, dry, be placed in ball milling in ball mill and cross 200 mesh sieves, obtain mixed-powder;
(2) it is to soak after 1~2h in 2.0mol/L sodium hydroxide solution that the mixed-powder of above-mentioned preparation is placed in mass concentration, filter, and it is washed with deionized filtrate, until the deionized water after Xi Di is neutral, it is to be dried 1~2h in 70~80 DEG C of baking ovens that washings is placed in temperature again, obtains dried object;
(3) dried object of above-mentioned preparation is placed in crucible, and in crucible, add dried object quality 60~75% iron sesquioxide and dried object quality 50~55% aluminium powder, after being uniformly mixed, magnesium ribbon by 7~8cm inserts in mixture, lighting magnesium ribbon, and be slowly introducing nitrogen simultaneously in crucible, control nitrogen being passed through speed is 17~25mL/s, after being passed through 40~55min so that it is continue reaction 1~2h;
(4), after question response terminates, mixture in crucible is cooled to 100~120 DEG C with the speed of 2 DEG C/min, insulation reaction 1~2h, then be placed in firm compression mould and carry out cold moudling, controlling pressure is 30~50MPa, and the time is 3~5min;
(5) after cold moudling, then being placed in calcining furnace, and calcine under nitrogen protection, controlling calcining heat is 700~800 DEG C, after calcining 30~40min, cools to room temperature with the furnace, can be prepared into soft magnetic materials.
CN201610242698.7A 2016-04-19 2016-04-19 A kind of preparation method of soft magnetic materials Active CN105957681B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106495664A (en) * 2016-10-21 2017-03-15 常州亚环环保科技有限公司 A kind of preparation method of high breaking strength Imitation Rock Porcelain Tiles

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006128521A (en) * 2004-10-29 2006-05-18 Jfe Steel Kk Dust core and soft magnetic metal powder therefor
CN101226804A (en) * 2007-11-29 2008-07-23 祁峰 Method of preparing iron silicon aluminum magnetic powder core with magnetic-conductivity [Mu] of 125
CN102136331A (en) * 2010-12-30 2011-07-27 长春工业大学 High-efficiency soft magnetic composite material and preparation method thereof
JP2012136770A (en) * 2010-12-10 2012-07-19 Nec Tokin Corp Fe-BASED NANO-CRYSTALLINE ALLOY POWDER AND METHOD FOR PRODUCING THE SAME, AND DUST CORE AND METHOD FOR MANUFACTURING THE SAME

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006128521A (en) * 2004-10-29 2006-05-18 Jfe Steel Kk Dust core and soft magnetic metal powder therefor
CN101226804A (en) * 2007-11-29 2008-07-23 祁峰 Method of preparing iron silicon aluminum magnetic powder core with magnetic-conductivity [Mu] of 125
JP2012136770A (en) * 2010-12-10 2012-07-19 Nec Tokin Corp Fe-BASED NANO-CRYSTALLINE ALLOY POWDER AND METHOD FOR PRODUCING THE SAME, AND DUST CORE AND METHOD FOR MANUFACTURING THE SAME
CN102136331A (en) * 2010-12-30 2011-07-27 长春工业大学 High-efficiency soft magnetic composite material and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106495664A (en) * 2016-10-21 2017-03-15 常州亚环环保科技有限公司 A kind of preparation method of high breaking strength Imitation Rock Porcelain Tiles

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