CN102049515B - Iron-silicon-aluminum soft magnetic powder and manufacturing method thereof - Google Patents
Iron-silicon-aluminum soft magnetic powder and manufacturing method thereof Download PDFInfo
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Abstract
The invention relates to iron-silicon-aluminum soft magnetic powder and a manufacturing method thereof, belonging to the field of metal magnetic materials. The iron-silicon-aluminum soft magnetic powder comprises the following components in percentage by weight: 9-10% of silicon, 5-6% of aluminum, 0.5-1% of chromium and the balance of iron. The iron-silicon-aluminum soft magnetic powder provided by the invention has the advantage of good magnetic property. The method provided by the invention not only can be used for producing the high-quality iron-silicon-aluminum soft magnetic powder, but also has the advantage of effectively reducing the production cost.
Description
Technical field
The present invention relates to a kind of iron-silicon-aluminum soft magnet powder and manufacturing approach thereof, belong to the metallicl magnetic material field.
Background technology
Soft magnetic materials is historical to existing 100 years of development such as permalloys from pure iron, silicon steel; Novel magnetically soft alloy materials such as nearly two amorphous alloys that successively grow up during the last ten years and nanometer crystal alloy; The institutional framework of soft magnetic materials is jumped to amorphous state from crystalline state; Develop into crystalline state nanometer from amorphous state again, thereby pushed the research and development of magnetically soft alloy new material and application to a new climax.The investigation of materials worker once was devoted for years in research has high saturated magnetic induction, high magnetic permeability, low-loss soft magnetic materials simultaneously, calls " ideal " soft magnetic materials of it " two high is low ", but fails all the time to realize.Metal soft magnetic alloy not only microstructure novel, be different from crystalline state and amorphous state, and have comprehensive excellent soft magnetic characteristic, promptly have than high saturated magnetic induction, high magnetic permeability, low-loss etc.; Meanwhile, this alloy also has characteristics such as production technology is simple, cost is low, pollution-free.Thereby can say that the appearance of metal soft magnetic alloy is a breakthrough of soft magnetic materials, it has solved people's long-term endeavour research and a unsolved difficult problem; Its contribution just is: 1. found one to make the Fe based alloy grain refine to 1～20 nanometer and approach that saturation magnetostriction coefficient and magnetocrystalline anisotropy constant go to zero simultaneously; 2. changed in the past that the magnetic conductivity of all kinds of soft magnetic materials, loss conflict with saturation induction density mutually, the afoul situation of magnetic property and cost.But specific to producing soft magnetic materials, domestic level and developed country's level exist gap.Modern electronic technology has proposed more and more high-level requirement to high frequency, efficient, high-power, small-sized, energy saving direction development to soft magnetic materials.
Summary of the invention
The objective of the invention is for solving the problems of the technologies described above, a kind of iron-silicon-aluminum soft magnet powder is provided.
Above-mentioned technical purpose of the present invention is achieved through following technical scheme:
The iron-silicon-aluminum soft magnet powder contains the silicon of 9～10wt% in its constituent, the aluminium of 5～6wt%, and the chromium of 0.5～1wt%, surplus is an iron.
Usually the metallic element that is added into the iron-silicon-aluminum soft magnet powder as trace element has Mn, La, Ni, Ta.Through experiment repeatedly, the inventor has added Cr, the plasticity that this has improved material, and the flattening that helps material is handled.As adopt ball-milling treatment technology to the processing of retrofiting of sendust material; Can obtain flat sheet shape contour structures; Also make its grain refinement and obtain the nanocrystalline structure of crystallite dimension less than exchange interaction length; The microwave complex permeability real part and the imaginary part of material all are significantly increased, and dielectric constant effectively reduces.
Another object of the present invention provides above-mentioned iron-silicon-aluminum soft magnet manufacturing method of power.
The iron-silicon-aluminum soft magnet manufacturing method of power may further comprise the steps:
1. ferroaluminium, iron powder, silica flour and chromium powder are smelted into the alloy of siliceous 9～10wt%, aluminium 5～6wt%, chromium 0.5～1wt%;
2. the alloy that 1. step is made is broken into alloy block, and this alloy block is poured into ball mill and in ball mill, added the dispersant that accounts for alloy block quality 3～6% at this, through ball mill alloy block is ground to form the alloy powder below 100 orders then; Said dispersant is the mixture of DBSA, polyethylene glycol, silane coupler and n-hexane;
3. the alloy powder that 2. makes through step is heat-treated; Heat treatment comprises heating, insulation and cooling three phases; Said three phases all carries out under the condition that with nitrogen is protective gas; The temperature of holding stage is controlled to be 900～950 ℃, and cooling stage is cooled to room temperature with the cooling velocity of >=10 ℃/min.
In the technique scheme of the present invention, as raw material, its reason is without fine aluminium; Because the fusing point of aluminium is low, about 660 ℃, and the temperature of molten iron is about in the of 1500 ℃; Make aluminium in the process of dissolving, volatilize easily, so aluminium content control difficulty is big, in addition because the density of aluminium is low; The content of the first half aluminium of alloy solution is high, causes the lack of homogeneity of alloying component easily.And the present invention adopts ferroaluminium as one of raw material, and the ferroaluminium fusing point is higher about 300 ℃ than the fusing point of aluminium, and density is big, sinks easily during dissolving, so solved an above-mentioned difficult problem effectively.
In the technique scheme of the present invention, be added with chromium in the raw material, and addition control makes that within the specific limits the chromium constituent content is controlled at 0.5～1wt% in the alloy that 1. makes through step.Being added with of chromium is beneficial to the plasticity of improving material, and the flattening that helps material is handled.As adopt ball-milling treatment technology to the processing of retrofiting of sendust material; Can obtain flat sheet shape contour structures; Also make its grain refinement and obtain the nanocrystalline structure of crystallite dimension less than exchange interaction length; The microwave complex permeability real part and the imaginary part of material all are significantly increased, and dielectric constant effectively reduces.
Adopting ball-milling technology will overcome a difficult point is to guarantee that sendust surface in the process of ball milling is not oxidized; Since under the situation of ball milling high speed rotating, the grinding machine continuous operation, and the temperature in the ball milling cylindrical shell just can reach more than 180 ℃; Under such temperature; The surface of tiny metal dust can be oxidized, and the result of oxidation can cause the power consumption of powder big, and permeability reduces.And when carrying out ball milling, continue to add mass fraction is that 3～6% dispersant just can make the temperature in the ball milling bucket be reduced between 80～90 ℃, greatly reduces the degree of oxidation of powder surface; Said dispersant is the mixture of DBSA, polyethylene glycol, silane coupler and n-hexane; This dispersant has volatility, so when subsequent technique heat treatment, can vapor away the physics that can not influence powder fully, can not cause harmful effect to the quality of powder.
Heat treatment is the conventional means of magnetic material preparation, not only can remove the internal stress of magnetic alloy powder through heat treatment, can also improve its magnetic.Temperature during heat treatment is a temperature limit with the curie point of this material usually; Curie point is also claimed Curie temperature or magnetic transformation point; Be meant the temperature that material can change between ferromagnet and paramagnet, promptly ferroelectric is transformed into the phase transition temperature of para-electric coupling from ferroelectric phase.This material becomes ferromagnet when being lower than Curie-point temperature, and this moment, the magnetic field relevant with material was difficult to change.When temperature was higher than Curie-point temperature, this material became paramagnet, and the magnetic field of magnet is easy to change with the change of surrounding magnetic field.Based on this theory; Usually to the magnetic material temperature be brought up to more than the Curie temperature during heat treatment, in addition since mutually transformations need the regular hour, so when the metal works surface meets the requirements of heating-up temperature; Also must keep certain hour in this temperature; Make internal and external temperature consistent,, be called temperature retention time during this period of time so that microscopic structure changes fully.Cooling rate also is one of important parameter of Technology for Heating Processing in addition.In raw material, add after the chromium, these control parameters all will be revised.Confirmed finally that through after the test of many times temperature of holding stage is controlled to be 900～950 ℃ the inventor, cooling stage is cooled to the such technical scheme of room temperature with the cooling velocity of >=10 ℃/min.
In sum, the present invention has following beneficial effect:
1, iron-silicon-aluminum soft magnet powder of the present invention has the advantage of good magnetic;
2, the inventive method not only can be produced the iron-silicon-aluminum soft magnet powder of good quality, and has the advantage that effectively reduces production costs.
The specific embodiment
This specific embodiment only is to explanation of the present invention; It is not a limitation of the present invention; Those skilled in the art can make the modification that does not have creative contribution to present embodiment as required after reading this specification, but as long as in claim scope of the present invention, all receive the protection of Patent Law.
Embodiment one
The iron-silicon-aluminum soft magnet powder contains the silicon of 9wt% in its constituent, the aluminium of 6wt%, and 0.5% chromium, surplus is an iron.
Above-mentioned iron-silicon-aluminum soft magnet manufacturing method of power makes through following steps:
1. ferroaluminium, iron powder, silica flour and chromium powder are smelted into the alloy of siliceous 9wt%, aluminium 6wt%, chromium 0.5wt%;
2. the alloy that 1. step is made is broken into alloy block, and this alloy block is poured into ball mill and in ball mill, added the dispersant that accounts for alloy block quality 3% at this, through ball mill alloy block is ground to form the alloy powder below 100 orders then; Said dispersant is the mixture of DBSA, polyethylene glycol, silane coupler and n-hexane;
3. the alloy powder that 2. makes through step is heat-treated, heat treatment comprises heating, insulation and cooling three phases, and said three phases all carries out under the condition that with nitrogen is protective gas; The heading-length of Equipment for Heating Processing is set to 3 meters, divides 3 warm areas, and 3 warm area temperature are distinguished 700 ℃, and 800 ℃, 900 ℃; Soaking zone is set to 3 meters, divides 3 warm areas, and the unification of 3 warm area temperature is 900 ℃, and cooling section is set to 6 meters, and the method that adopts high-pressure cold water to impact high temperature alloy liquid is controlled at 10 ℃/min with cooling velocity, is cooled to room temperature.
Embodiment two
The iron-silicon-aluminum soft magnet powder contains the silicon of 9.6wt% in its constituent, the aluminium of 5.4wt%, and 0.8% chromium, surplus is an iron.
Above-mentioned iron-silicon-aluminum soft magnet manufacturing method of power makes through following steps:
1. ferroaluminium, iron powder, silica flour and chromium powder are smelted into the alloy of siliceous 9.6wt%, aluminium 5.4wt%, chromium 0.8wt%;
2. the alloy that 1. step is made is broken into alloy block, and this alloy block is poured into ball mill and in ball mill, added the dispersant that accounts for alloy block quality 5% at this, through ball mill alloy block is ground to form the alloy powder below 100 orders then; Said dispersant is the mixture of DBSA, polyethylene glycol, silane coupler and n-hexane;
3. the alloy powder that 2. makes through step is heat-treated, heat treatment comprises heating, insulation and cooling three phases, and said three phases all carries out under the condition that with nitrogen is protective gas; The heading-length of Equipment for Heating Processing is set to 3 meters, divides 3 warm areas, and 3 warm area temperature are distinguished 700 ℃, and 800 ℃, 900 ℃; Soaking zone is set to 3 meters, divides 3 warm areas, and the unification of 3 warm area temperature is 930 ℃, and cooling section is set to 6 meters, and the method that adopts high-pressure cold water to impact high temperature alloy liquid is controlled at 15 ℃/min with cooling velocity, is cooled to room temperature.
Embodiment three
The iron-silicon-aluminum soft magnet powder contains the silicon of 10wt% in its constituent, the aluminium of 5wt%, and the chromium of 1wt%, surplus is an iron.
Above-mentioned iron-silicon-aluminum soft magnet manufacturing method of power makes through following steps:
1. ferroaluminium, iron powder, silica flour and chromium powder are smelted into the alloy of siliceous 10wt%, aluminium 6wt%, chromium 1wt%;
2. the alloy that 1. step is made is broken into alloy block, and this alloy block is poured into ball mill and in ball mill, added the dispersant that accounts for alloy block quality 6% at this, through ball mill alloy block is ground to form the alloy powder below 100 orders then; Said dispersant is the mixture of DBSA, polyethylene glycol, silane coupler and n-hexane;
3. the alloy powder that 2. makes through step is heat-treated, heat treatment comprises heating, insulation and cooling three phases, and said three phases all carries out under the condition that with nitrogen is protective gas; The heading-length of Equipment for Heating Processing is set to 3 meters, divides 3 warm areas, and 3 warm area temperature are distinguished 700 ℃, and 800 ℃, 900 ℃; Soaking zone is set to 3 meters, divides 3 warm areas, and the unification of 3 warm area temperature is 950 ℃, and cooling section is set to 6 meters, and the method that adopts high-pressure cold water to impact high temperature alloy liquid is controlled at 20 ℃/min with cooling velocity, is cooled to room temperature.
Comparative Examples
Ingot iron, silicon metal, fine aluminium are dropped in the Efco-Northrup furnace of 50 kilograms of nominals and smelt; Being cast into chemical composition is the alloy cast ingot of iron 84.80%, silicon 9.53%, aluminium 5.62%; With mechanical means the alloy cast ingot coarse crushing is become the material piece below 25 millimeters; Insert in the general reduction furnace with hydrogen shield atmosphere these material pieces and cooling after being incubated about 2 hours under the temperature conditions about 700 ℃; Further these material pieces are broken into the material piece less than 6 millimeters with clever formula disintegrating machine again; Be ground into the alloy powder below 100 orders with vibratory milling again, this alloy powder inserted in the general reduction furnace with hydrogen shield atmosphere under the temperature conditions about 900 ℃ insulation and carried out stress annealing in 1 hour and handle screening afterwards.
Claims (1)
1. the iron-silicon-aluminum soft magnet manufacturing method of power is characterized in that, may further comprise the steps:
1. ferroaluminium, iron powder, silica flour and chromium powder are smelted into siliceous 9～10wt%, aluminium 5～6wt%, chromium 0.5～1wt%,
Surplus is the alloy of iron;
2. the alloy that 1. step is made is broken into alloy block, and this alloy block is poured into ball mill and added in ball mill at this
Account for the dispersant of alloy block quality 3～6%, through ball mill alloy block is ground to form the alloy powder below 100 orders then;
Said dispersant is the mixture of DBSA, polyethylene glycol, silane coupler and n-hexane;
3. the alloy powder that 2. makes through step is heat-treated, heat treatment comprises heating, insulation and cooling three phases,
Said three phases all carries out under the condition that with nitrogen is protective gas, and the temperature of holding stage is controlled to be 900～950 ℃, and cooling stage is cooled to room temperature with the cooling velocity of >=10 ℃/min; Said cooling is to adopt high-pressure cold water to impact the cooling means of high temperature alloy liquid.
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| CN102303116B (en) * | 2011-08-12 | 2013-08-07 | 天通控股股份有限公司 | Manufacturing method of mu40 ferrum silicon aluminum magnetic powder core |
| CN103769580B (en) * | 2014-02-19 | 2016-03-30 | 南京林业大学 | A kind of preparation method of modified Nano iron powder |
| CN104361968A (en) * | 2014-09-29 | 2015-02-18 | 惠州市科力磁元有限公司 | Preparation method of low-loss high permeability Fe-Si-Al magnetic powder core |
| CN108555306B (en) * | 2016-06-02 | 2021-05-14 | 泉州天智合金材料科技有限公司 | Iron-silicon-chromium soft magnetic powder and application thereof |
| CN107299290A (en) * | 2017-06-27 | 2017-10-27 | 湖州知维技术服务有限公司 | A kind of soft magnetic powder and preparation method thereof |
| CN110405195A (en) * | 2019-08-08 | 2019-11-05 | 航天科工武汉磁电有限责任公司 | A kind of Fe base compound particle heatproof absorbent and preparation method thereof |
| CN111375782B (en) * | 2019-12-16 | 2021-06-18 | 横店集团东磁股份有限公司 | Preparation method of iron-nickel-molybdenum soft magnetic powder |
| CN112735802A (en) * | 2020-12-25 | 2021-04-30 | 中钢集团南京新材料研究院有限公司 | Microwave insulation coating method for iron-silicon-aluminum magnetic powder core and insulation coated magnetic powder core |
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| CN101064207A (en) * | 2006-03-27 | 2007-10-31 | Tdk株式会社 | Flaky soft magnetic metal powder and magnetic core member for RFID antenna |
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| CN101064207A (en) * | 2006-03-27 | 2007-10-31 | Tdk株式会社 | Flaky soft magnetic metal powder and magnetic core member for RFID antenna |
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| JP特开2008-50644A 2008.03.06 |
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