CN101236818A - Making method for soft magnetic alloy compound material with high magnetic conductivity - Google Patents

Making method for soft magnetic alloy compound material with high magnetic conductivity Download PDF

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Publication number
CN101236818A
CN101236818A CNA2007101602450A CN200710160245A CN101236818A CN 101236818 A CN101236818 A CN 101236818A CN A2007101602450 A CNA2007101602450 A CN A2007101602450A CN 200710160245 A CN200710160245 A CN 200710160245A CN 101236818 A CN101236818 A CN 101236818A
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alloy
soft magnetic
flat powder
high magnetic
laid
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严密
许盼盼
罗伟
马天宇
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Zhejiang University ZJU
Hengdian Group DMEGC Magnetics Co Ltd
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Zhejiang University ZJU
Hengdian Group DMEGC Magnetics Co Ltd
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Abstract

The invention discloses a preparation method for high magnetic conductivity soft magnetic alloy composite materials, comprising the followings steps: firstly, ferrum, aluminum, silicon and titanium with a purity more than 99.9 weight percent are taken as raw materials and laid into a medium frequency vacuum induction furnace for smelting, and a master alloy is obtained; secondly, the master alloy after smelting is laid into a quick quenching device; an alloy ingot casting is quickly poured on a water-cooling roll wheel which rotates at high speed after arc remelting under the protection of high purity inert gases, and a quickly condensed sheet band or a quickly condensed sheet is obtained; thirdly, flat processing is performed by adoption of the ball milling technology, and flat powder is obtained; fourthly, the flat powder is laid into a stainless steel tube which is then vacuumized and filled with inert protective gases, and then the stainless steel tube is laid into a tube furnace for heating and cooling along with the furnace; fifthly, the flat powder and binding agents are mixed and milled for processing the flaky high magnetic conductivity soft magnetic materials which are then laid into a heat treatment furnace for heating, heat preservation and vacuum cooling. The preparation method for the high magnetic conductivity soft magnetic alloy composite materials is simple in technology and suitable for large-scale mass production; a magnet has high magnetic conductivity; the magnetic shielding effect is greatly improved.

Description

The preparation method of soft magnetic alloy compound material with high magnetic conductivity
Technical field
The present invention relates to magnetic material, especially relate to a kind of preparation method of soft magnetic alloy compound material with high magnetic conductivity.
Background technology
Continuous development along with the telecommunications industry, telecommunications device such as mobile phone, popularizing of notebook computer etc., electromagnetic interference is increasing to the influence that environment causes, the annual economic loss that causes because of electromagnetic pollution is up to 500,000,000 dollars, and the anti-electromagnetic interference material of microwave in the development ghz band scope has caused that people more and more pay attention to, simultaneously, microwave absorbing material is the basic material of develop high-tech military project, is the key point of stealth technology.No matter be civilian or military, the anti-electromagnetic interference material of microwave all had higher requirement that higher absorption efficiency and higher by frequency is the anti-electromagnetic interference Development of Materials of a microwave direction.
The saturation magnetization of metal soft magnetic material is more much bigger than ferrite, but because its conductivity is bigger, forms eddy current easily, worsens its performance.Thereby, just can develop and the anti-electromagnetic interference performance good metal of high frequency soft magnetic material if can find a formation that suppresses inner closure domain to reduce the eddy current loss of material.The research of this respect is beginning very early, be to use the alternate laminated construction of magnetic thin film and thin dielectric film the earliest, because the thickness of film is less than the skin depth of material, thereby effectively suppressed the formation of eddy current and closure domain, but this kind laminated construction can cause the formation of direct capacitance, form displacement current, the high frequency magnetic permeability that is unfavorable for material, the analysis showed that, the electrostatic capacitance that this magnetic metal/dielectric alternate laminated structure produces, depend on the size of magnetic metal body length direction, if this alternate laminated structure is divided into column structure, electrostatic capacitance then can be suppressed to insignificant degree.This column alternate laminated structure metallicl magnetic material has good magnetic characteristic under high frequency, but because the restriction of its cost, manufacture craft etc. is difficult to be suitable for the application of anti-electromagnetic interference material.Under the inspiration of this thinking, if magnetic thin film part with this alternate laminated structure kind, the flat powder that to use thickness instead be about skin depth and have big aspect ratio, flat powder uses polymer to isolate, can constitute cheap for manufacturing cost, and can realize producing in batches, and high frequency performance is similar to the anti-EMI material of alternative stacked column structure.Use the anti-electromagnetic interference material of this kind method preparation, cost is low, and technology is simple, can realize large-scale industrial production.
The Fe-Si-Al metal soft magnetic material is a kind of traditional soft magnetic material, though its comprehensive soft magnet performance is less than nano-crystal soft-magnetic series, but the composite material that Fe-Si-Al micro mist after the researcher of Japan handles flattening and organic insulating material are mixed and made into similar magnetic thin film/thin dielectric film alternating structure, find that it has good anti-emi characteristics in the quasi-microwave section, injected new vitality for again this traditional metal soft magnetic material.Simultaneously because this material does not contain strategic elements such as cobalt, nickel, particularly when approaching celestial Da Site (Sendust) alloy of its composition, have and the same magnetic permeability high under low-intensity magnetic field of perm (Perm) alloy, and saturation magnetization (M s) higher, resistivity is bigger, be more suitable for using under high frequency, so its application in anti-electromagnetic interference field more and more is subjected to people's attention.
It is that the resistivity of metal soft magnetic alloy is low that metallicl magnetic material has individual common drawback as anti-electromagnetic interference material, and used thickness reduces material thickness and can enlarge its range of application at high frequency, but also be subjected to certain limitation owing to be subjected to the restriction of skin depth.The skin depth of metal soft magnetic alloy square with its resistivity proportional, so improving resistivity is one of method that effectively improves its magnetic permeability, the Ti element can improve the resistivity of Fe-Si-Al alloy, in the Fe-Si-Al alloy, add Ti, adopt the fast melt-quenching technology and change ball-milling technology and heat treatment temperature, obtain the nano-crystalline Fe SiAlTi alloy of high magnetic permeability, the flat powder of alloy and the mixing processing and preparing of binding agent are got sheeting have high magnetic permeability.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of soft magnetic alloy compound material with high magnetic conductivity.
The preparation method of soft magnetic alloy compound material with high magnetic conductivity comprises the steps:
1) adopting purity is raw material greater than Fe, Al, Si, the Ti of 99.9wt%, puts into the melting of intermediate frequency vaccum sensitive stove, obtains foundry alloy;
2) melted foundry alloy is put into fast quenching equipment, alloy cast ingot is poured into rapidly on the running roller of high speed rotating through after the remelting under inert gas shielding, obtains the FeSiAlTi strip or the FeSiAlTi thin slice of rapid condensation, and the speed of quenching is 15~35m/s;
3) FeSiAlTi strip or FeSiAlTi thin slice being put into the ball mill ball milling carries out flattening and handles ratio of grinding media to material 3: 1~10: 1, rotating speed 200~460r/min;
4) flat powder is put into stainless steel tube, be evacuated down to 10 -2~10 -5Pa charges into the high pure nitrogen protection, and air pressure is 1 * 10 5~0.5 * 10 5Pa puts into tube furnace with stainless steel tube and is heated to 573K~873K, and insulation 30~60min cools off with stove;
5) flat powder and binding agent are mixing is processed into laminar high magnetic permeability soft magnetic material, and pressure is 20~40kN, puts into heat-treatment furnace and is heated to 100~200 ℃, insulation 30~60min, air cooling.
The percentage by weight that described foundry alloy is formed is: Fe 85-xTi xSi 9.6Al 5.40<x<15 wherein.Binding agent is epoxy resin and polyamide, and epoxy resin and polyamide weight ratio are 1: 1~0.5.
The beneficial effect that the present invention compared with prior art has: add the resistivity that the Ti element can improve the Fe-Si-Al alloy, and then improve its high-gradient magnetism energy, in the Fe-Si-Al alloy, add Ti, adopt the fast melt-quenching technology and change ball-milling technology and heat treatment temperature, acquisition has the flat powder of nano-crystalline Fe SiAlTi alloy of high magnetic permeability, has high magnetic permeability with the mixing processing and preparing gained of binding agent sheeting again.Technology of the present invention is simple, and is with low cost, is suitable for large-scale batch production, and magnet has high magnetic permeability, and Magnetic Shielding Effectiveness improves greatly.
Embodiment
Below by embodiment, technical scheme of the present invention is done further specific description.
Embodiment 1:
1) with raw material with mass ratio be: it is the intermediate frequency vaccum sensitive stove melting of crucible that iron 80%, titanium 5%, silicon 9.6%, aluminium 5.4% are put into the aluminium oxide, is evacuated down to 10 -1Pa send the electric preheating furnace charge again, to get rid of adsorbed gas, moisture and the organic substance etc. of furnace charge.At this moment, vacuum degree descends in the stove, and then is evacuated down to 10 -2More than the Pa, charging into high-purity argon gas is 0.5 * 10 to the stove internal gas pressure 5Pa, the high-power electricity that send melts furnace charge fully, pours into a mould behind the low-power refining 10min again.
2) melted FeSiAlTi foundry alloy is put into fast quenching equipment, and alloy cast ingot obtains the thin slice of rapid condensation being poured into rapidly on the running roller of high speed rotating after the remelting of process electric arc under the high-purity argon gas protection, and the speed of quenching is 15m/s;
3) the FeSiAlTi thin slice is put into ball mill and carried out ball milling flattening processing, obtain flat powder, ratio of grinding media to material 10: 1, rotating speed 200r/min;
4) flat powder is put into stainless steel tube, be evacuated down to 10 -3Pa charges into the high pure nitrogen protection, and air pressure is 0.5 * 10 5, stainless steel tube being put into tube furnace be heated to 573K, insulation 60min cools off with stove;
5) be 50: 1: 0.5 mixing anti-electromagnetic interference materials of laminar pliability that are processed into flat powder and epoxy resin and polyamide with weight ratio, mixing pressure is 20kN, and pressurize 5min puts into heat-treatment furnace and is heated to 120 ℃, insulation 50min, air cooling.
Embodiment 2:
1) with raw material with mass ratio be: it is the intermediate frequency vaccum sensitive stove melting of crucible that iron 75%, titanium 10%, silicon 9.6%, aluminium 5.4% are put into the aluminium oxide, is evacuated down to 10 -1Pa send the electric preheating furnace charge again, to get rid of adsorbed gas, moisture and the organic substance etc. of furnace charge.At this moment, vacuum degree descends in the stove, and then is evacuated down to 10 -2More than the Pa, charging into high-purity argon gas is 0.5 * 10 to the stove internal gas pressure 5Pa, the high-power electricity that send melts furnace charge fully, pours into a mould behind the low-power refining 10min again.
2) melted FeSiAlTi foundry alloy is put into fast quenching equipment, and alloy cast ingot obtains the thin slice of rapid condensation being poured into rapidly on the running roller of high speed rotating after the remelting of process electric arc under the high-purity argon gas protection, and the speed of quenching is 27.5m/s;
3) the FeSiAlTi thin slice is put into ball mill and carried out ball milling flattening processing, obtain flat powder, ratio of grinding media to material 5: 1, rotating speed 300r/min;
4) flat powder is put into stainless steel tube, be evacuated down to 10 -3Pa charges into the high pure nitrogen protection, and air pressure is 0.5 * 10 5, stainless steel tube being put into tube furnace be heated to 573K, insulation 60min cools off with stove;
5) be 50: 1: 0.75 mixing anti-electromagnetic interference materials of laminar pliability that are processed into flat powder and epoxy resin and polyamide with weight ratio, mixing pressure is 25kN, and pressurize 4min puts into heat-treatment furnace and is heated to 100 ℃, insulation 60min, air cooling.
Embodiment 3:
1) with raw material with mass ratio be: it is the intermediate frequency vaccum sensitive stove melting of crucible that iron 70%, titanium 15%, silicon 9.6%, aluminium 5.4% are put into the aluminium oxide, is evacuated down to 10 -1Pa send the electric preheating furnace charge again, to get rid of adsorbed gas, moisture and the organic substance etc. of furnace charge.At this moment, vacuum degree descends in the stove, and then is evacuated down to 10 -2More than the Pa, charging into high-purity argon gas is 0.5 * 10 to the stove internal gas pressure 5Pa, the high-power electricity that send melts furnace charge fully, pours into a mould behind the low-power refining 10min again.
2) melted FeSiAlTi foundry alloy is put into fast quenching equipment, and alloy cast ingot obtains the strip of rapid condensation being poured into rapidly on the running roller of high speed rotating after the remelting of process electric arc under the high-purity argon gas protection, and the speed of quenching is 20m/s;
3) the FeSiAlTi thin slice is put into ball mill and carried out ball milling flattening processing, obtain flat powder, ratio of grinding media to material 3: 1, rotating speed 460r/min;
4) flat powder is put into stainless steel tube, be evacuated down to 10 -3Pa charges into the high pure nitrogen protection, and air pressure is 0.5 * 10 5, stainless steel tube being put into tube furnace be heated to 673K, insulation 40min cools off with stove;
5) be 50: 1: 1 mixing anti-electromagnetic interference materials of laminar pliability that are processed into flat powder and epoxy resin and polyamide with weight ratio, mixing pressure is 30kN, and pressurize 3min puts into heat-treatment furnace and is heated to 150 ℃, insulation 40min, air cooling.
Embodiment 4:
1) with raw material with mass ratio be: it is the intermediate frequency vaccum sensitive stove melting of crucible that iron 77.5%, titanium 7.5%, silicon 9.6%, aluminium 5.4% are put into the aluminium oxide, is evacuated down to 10 -1Pa send the electric preheating furnace charge again, to get rid of adsorbed gas, moisture and the organic substance etc. of furnace charge.At this moment, vacuum degree descends in the stove, and then is evacuated down to 10 -2More than the Pa, charging into high-purity argon gas is 0.5 * 10 to the stove internal gas pressure 5Pa, the high-power electricity that send melts furnace charge fully, pours into a mould behind the low-power refining 10min again.
2) melted FeSiAlTi foundry alloy is put into fast quenching equipment, and alloy cast ingot obtains the thin slice of rapid condensation being poured into rapidly on the running roller of high speed rotating after the remelting of process electric arc under the high-purity argon gas protection, and the speed of quenching is 35m/s;
3) the FeSiAlTi thin slice is put into ball mill and carried out ball milling flattening processing, obtain flat powder, ratio of grinding media to material 7: 1, rotating speed 400r/min;
4) flat powder is put into stainless steel tube, be evacuated down to 10 -3Pa charges into the high pure nitrogen protection, and air pressure is 0.5 * 10 5, stainless steel tube being put into tube furnace be heated to 673K, insulation 40min cools off with stove;
5) be 50: 1: 1 mixing anti-electromagnetic interference materials of laminar pliability that are processed into flat powder and epoxy resin and polyamide with weight ratio, mixing pressure is 40kN, and pressurize 2min puts into heat-treatment furnace and is heated to 180 ℃, insulation 30min, air cooling.
Embodiment 5:
1) with raw material with mass ratio be: it is the intermediate frequency vaccum sensitive stove melting of crucible that iron 82.5%, titanium 12.5%, silicon 9.6%, aluminium 5.4% are put into the aluminium oxide, is evacuated down to 10 -1Pa send the electric preheating furnace charge again, to get rid of adsorbed gas, moisture and the organic substance etc. of furnace charge.At this moment, vacuum degree descends in the stove, and then is evacuated down to 10 -2More than the Pa, charging into high-purity argon gas is 0.5 * 10 to the stove internal gas pressure 5Pa, the high-power electricity that send melts furnace charge fully, pours into a mould behind the low-power refining 10min again.
2) melted FeSiAlTi foundry alloy is put into fast quenching equipment, and alloy cast ingot obtains the thin slice of rapid condensation being poured into rapidly on the running roller of high speed rotating after the remelting of process electric arc under the high-purity argon gas protection, and the speed of quenching is 15m/s;
3) the FeSiAlTi thin slice is put into ball mill and carried out ball milling flattening processing, obtain flat powder, ratio of grinding media to material 10: 1, rotating speed 300r/min;
4) flat powder is put into stainless steel tube, be evacuated down to 10 -3Pa charges into the high pure nitrogen protection, and air pressure is 0.5 * 10 5, stainless steel tube being put into tube furnace be heated to 773K, insulation 30min cools off with stove;
5) be 50: 1: 0.75 mixing anti-electromagnetic interference materials of laminar pliability that are processed into flat powder and epoxy resin and polyamide with weight ratio, mixing pressure is 20kN, and pressurize 5min puts into heat-treatment furnace and is heated to 200 ℃, insulation 30min, air cooling.
Embodiment 6:
1) with raw material with mass ratio be: it is the intermediate frequency vaccum sensitive stove melting of crucible that iron 85%, silicon 9.6%, aluminium 5.4% are put into the aluminium oxide, is evacuated down to 10 -1Pa send the electric preheating furnace charge again, to get rid of adsorbed gas, moisture and the organic substance etc. of furnace charge.At this moment, vacuum degree descends in the stove, and then is evacuated down to 10 -2More than the Pa, charging into high-purity argon gas is 0.5 * 10 to the stove internal gas pressure 5Pa, the high-power electricity that send melts furnace charge fully, pours into a mould behind the low-power refining 10min again.
2) melted FeSiAl foundry alloy is put into fast quenching equipment, and alloy cast ingot obtains the strip of rapid condensation being poured into rapidly on the running roller of high speed rotating after the remelting of process electric arc under the high-purity argon gas protection, and the speed of quenching is 17.5m/s;
3) the FeSiAl thin slice is put into ball mill and carried out ball milling flattening processing, obtain flat powder, ratio of grinding media to material 5: 1, rotating speed 460r/min;
4) flat powder is put into stainless steel tube, be evacuated down to 10 -3Pa charges into the high pure nitrogen protection, and air pressure is 0.5 * 10 5, stainless steel tube being put into tube furnace be heated to 773K, insulation 30min cools off with stove;
5) be 50: 1: 0.5 mixing anti-electromagnetic interference materials of laminar pliability that are processed into flat powder and epoxy resin and polyamide with weight ratio, mixing pressure is 35kN, and pressurize 3min puts into heat-treatment furnace and is heated to 150 ℃, insulation 30min, air cooling.
As mentioned above, can well realize the present invention.

Claims (3)

1. the preparation method of a soft magnetic alloy compound material with high magnetic conductivity is characterized in that comprising the steps:
1) adopting purity is raw material greater than Fe, Al, Si, the Ti of 99.9wt%, puts into the melting of intermediate frequency vaccum sensitive stove, obtains foundry alloy;
2) melted foundry alloy is put into fast quenching equipment, alloy cast ingot is poured into rapidly on the running roller of high speed rotating through after the remelting under inert gas shielding, obtains the FeSiAlTi strip or the FeSiAlTi thin slice of rapid condensation, and the speed of quenching is 15~35m/s;
3) FeSiAlTi strip or FeSiAlTi thin slice are put into the ball mill ball milling and carried out flattening and handle, make flat powder, ratio of grinding media to material 3: 1~10: 1, rotating speed 200~460r/min;
4) flat powder is put into stainless steel tube, be evacuated down to 10 -2~10 -5Pa charges into the high pure nitrogen protection, and air pressure is 1 * 10 5~0.5 * 10 5Pa puts into tube furnace with stainless steel tube and is heated to 573K~873K, and insulation 30~60min cools off with stove;
5) flat powder and binding agent are mixing is processed into laminar high magnetic permeability soft magnetic material, and pressure is 20~40kN, puts into heat-treatment furnace and is heated to 100~200 ℃, insulation 30~60min, air cooling.
2. the preparation method of a kind of soft magnetic alloy compound material with high magnetic conductivity according to claim 1 is characterized in that the percentage by weight that described foundry alloy is formed is: Fe 85-xTi xSi 9.6Al 5.4, 0<x<15 wherein.
3. the preparation method of a kind of soft magnetic alloy compound material with high magnetic conductivity according to claim 1 is characterized in that described binding agent is epoxy resin and polyamide, and epoxy resin and polyamide weight ratio are 1: 1~0.5.
CNA2007101602450A 2007-12-14 2007-12-14 Making method for soft magnetic alloy compound material with high magnetic conductivity Pending CN101236818A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104036941A (en) * 2014-06-10 2014-09-10 毛圣华 Preparation method of amorphous metal powder non-magnetic sheet for wireless charger
CN105834439A (en) * 2016-06-12 2016-08-10 横店集团东磁股份有限公司 Preparation method of flat soft magnetic alloy powder
CN105855555A (en) * 2016-04-05 2016-08-17 广东省钢铁研究所 Preparing method for iron and cobalt magnetically soft alloy device
CN107507689A (en) * 2016-06-14 2017-12-22 有研稀土新材料股份有限公司 The preparation method of high magnetic permeability absorbing material

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104036941A (en) * 2014-06-10 2014-09-10 毛圣华 Preparation method of amorphous metal powder non-magnetic sheet for wireless charger
CN105855555A (en) * 2016-04-05 2016-08-17 广东省钢铁研究所 Preparing method for iron and cobalt magnetically soft alloy device
CN105855555B (en) * 2016-04-05 2018-05-11 广东省钢铁研究所 A kind of preparation method of iron cobalt magnetically soft alloy device
CN105834439A (en) * 2016-06-12 2016-08-10 横店集团东磁股份有限公司 Preparation method of flat soft magnetic alloy powder
CN107507689A (en) * 2016-06-14 2017-12-22 有研稀土新材料股份有限公司 The preparation method of high magnetic permeability absorbing material
CN107507689B (en) * 2016-06-14 2019-08-13 有研稀土新材料股份有限公司 The preparation method of high magnetic permeability absorbing material

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