CN101236812A - Making method for electromagnetic wave interference resisting iron ,silicon, aluminum and nickel alloy - Google Patents
Making method for electromagnetic wave interference resisting iron ,silicon, aluminum and nickel alloy Download PDFInfo
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- CN101236812A CN101236812A CNA2007101602431A CN200710160243A CN101236812A CN 101236812 A CN101236812 A CN 101236812A CN A2007101602431 A CNA2007101602431 A CN A2007101602431A CN 200710160243 A CN200710160243 A CN 200710160243A CN 101236812 A CN101236812 A CN 101236812A
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Abstract
The invention discloses a preparation method for electromagnetic wave interference resistant iron silicon aluminum nickel alloys. The invention comprises the following steps: firstly, ferrum, aluminum, silicon and nickel 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, the sheet band or the sheet is laid into a ball mill for ball milling flat processing, and flat powder is obtained; fourthly, the flat powder is laid into a stainless steel tube which is then vacuumized and filled with high purity inert gases for protection, and then the stainless steel tube is laid into a tube furnace for heating, heat preservation and cooling along with the furnace; fifthly, the flat powder and binding agents are mixed and milled for processing the sheet. The preparation method for the electromagnetic wave interference resistant iron silicon aluminum nickel alloys adds adequate nickel into Sendust alloys, thereby the processability of the alloys is improved; the ball milling time is reduced; the cost of industrial production is saved; simultaneously the magnetic conductivity can be improved and the magnetic shielding effect can be improved.
Description
Technical field
The present invention relates to a kind of magnetic material, especially relate to a kind of preparation method of electromagnetic wave interference resisting iron, silicon, aluminum and nickel alloy.
Background technology
Electromagnetic interference (EMI) is generally acknowledged by countries in the world to the harm of PE and personal safety, European electromagnetic compatibility standard (EN) is implemented from January, 1996 in Europe, shows that the electric product that enters the European market all must meet RFI/EMI and noise immunity requirement.The electromagnetic compatibility problem involvement aspect is very wide, and its core is to manage to reduce electromagnetic interference that self produces and the ability that improves anti-electromagnetic interference.At present general EMC Design technology has three kinds of ground connection, shielding, filtering in electronic equipment and system, is referred to as to suppress three big technology of electromagnetic interference usually.Ground connection is that interference signal is introduced earth terminal; Shielding is to utilize shield to stop or the electromagnetic transmission of the interference signal that decays; Filtering is to stop the interfering frequency signal by allowing a kind of technology of passing through with frequency signal.Cardinal principle is to utilize certain functional material to make anti-EMI device electromagnetic loss is suppressed EMI.Soft magnetic material is the preferred material of anti-EMI as the material that not only has dielectric loss but also have a magnetic loss always.
The nanocrystalline metal soft magnetic material is not owing to be subjected to the restriction of Snooker (Snock) limit, and frequency of utilization can be very high, and mix the back with organic insulating material and improve its resistance, therefore at high frequency region (GHz wave band), anti-EMI excellent performance, and also quality is less.The 9.6wt%Si-5.4wt%Al-balFe alloy that is named as celestial Da Site (Sendust) alloy is found in 20th century the '30s.Its raw material cheaply is easy to get, and the same with permalloy have high magnetic permeability and a saturation induction density B
s, the electricalresistivity is higher, this alloy is very suitable for doing magnetic head material, but to be quality too crisp is not easy to cold working for the shortcoming of its maximum, limited it and apply in a very long time.But along with the progress of technology of preparing and the development need of high density magnetic recording and video Magnetographic Technology, this alloy was subjected to extensive concern and yielded unusually brilliant results afterwards.Why the 9.6wt%Si-5.4wt%Al-balFe alloy has very high magnetic permeability, mainly is because when this composition, its magnetic anisotropy constant K
1With magnetostriction coefficient λ
sAll go to zero.In addition, researchers also by add the method for trace rare-earth element or other alloying element in alloy, have improved the corrosion-resistant of alloy and other performance.For example add nickel and adjust silicon and the content of aluminium, obtain the 6wt%Si-4wt%Al-3.5wt%Ni-balFe quaternary alloy, be called super celestial platform Si Tegao permeability magnetic alloy (SuperSendust), its magnetic and processability all improve, and especially resistance to wear has more significantly raising.
The Fe-Si-Al magnetically soft alloy is as anti-EMI material, and the chemical composition of its electromagnetic performance and alloy, the size of micro mist and flattening degree, treatment process etc. are closely related.The Japanology person finds that the Fe-Si-Al magnetically soft alloy is after flattening is handled, become anti-electromagnetic interference material with organic substances such as rubber are mixing, since the GHz wave band has anti-preferably electromagnetic interference performance, people have done a lot of elaborations, to foundry alloy preparation, flattening treatment process, micro-structural and the electromagnetic performance of Fe-Si-Al magnetically soft alloy, done improvement and expansion in various degree.At present, the Fe-Si-Al alloy is as soft magnetic material, and general composition proportion is the composition proportion Si round celestial Da Site (Sendust) alloy
9.6-Al
5.4-Fe
BalDo to adjust by a small margin.Because the Fe-Si-Al alloy is too crisp, is not easy to ball-milling treatment, long and flat change poor effect of the alloyed powder time that obtain added Ni in the Fe-Si-Al alloy, improve its processing characteristics, reduces the ball milling time, saves production cost, and also improves magnetic property simultaneously.The ball milling flattening was handled after the present invention adopted the rapid hardening belt-rejecting technology to prepare alloy thin band, had obtained to have the nano-crystalline Fe SiAlNi alloy of excellent high frequency performance.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of electromagnetic wave interference resisting iron, silicon, aluminum and nickel alloy.
Comprise the steps:
1) adopting purity is raw material greater than Fe, Al, Si, the Ni 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 being poured into rapidly on the water-cooled running roller of high speed rotating after the remelting of process electric arc under the high-purity argon gas protection, obtain the FeSiAlNi strip or the FeSiAlNi thin slice of rapid condensation, the speed of quenching is 15~35m/s;
3) FeSiAlNi strip or FeSiAlNi thin slice are put into ball mill and carried out the ball milling flattening and handle, obtain 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 0.5 * 10
5~1 * 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) the mixing thin slice that is processed into 2~5mm of flat powder and binding agent, pressure is 20~40kN, puts into heat-treatment furnace and heats 100~200 ℃, insulation 30~60min, air cooling.
The weight ratio that described foundry alloy is formed is: iron 84~90%, silicon 4~8%, aluminium 2~6%, nickel 1.5~5.5%; Binding agent is epoxy resin and polyamide, and the weight ratio of epoxy resin and polyamide is 1: 1~0.5.
The beneficial effect that the present invention compared with prior art has is: add an amount of Ni in the FeSiAl alloy, can improve its processing characteristics, reduce the ball milling time, save production cost, also can improve magnetic property simultaneously.Adopt the rapid hardening belt-rejecting technology to prepare rapid tempering belt, handle in conjunction with the ball-milling technology flattening again, can obtain to have the nano-crystalline Fe SiAlNi alloy of excellent high frequency performance.The present invention can improve the alloy processing characteristics, reduces the ball milling time, saves industrial cost, also can improve magnetic permeability simultaneously, improves Magnetic Shielding Effectiveness.
Description of drawings
Fig. 1 is 20 hours SEM figure of the embodiment of the invention 1 ball milling;
Fig. 2 is 20 hours SEM figure of the embodiment of the invention 2 ball millings;
Fig. 3 is 20 hours SEM figure of the embodiment of the invention 3 ball millings;
Fig. 4 is 20 hours SEM figure of the embodiment of the invention 4 ball millings;
Fig. 5 is 20 hours SEM figure of the embodiment of the invention 5 ball millings;
Fig. 6 is 20 hours SEM figure of the embodiment of the invention 6 ball millings;
Fig. 7 is 20 hours SEM figure of the embodiment of the invention 7 ball millings;
Fig. 8 is 70 hours SEM figure of the embodiment of the invention 7 ball millings;
Embodiment
Below by embodiment, and in conjunction with the accompanying drawings, 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 85.5%, silicon 4%, aluminium 5%, nickel 5.5% 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 FeSiAlNi 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 FeSiAlNi 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: 0.75 mixing anti-electromagnetic interference materials of laminar pliability that are processed into 3mm with flat powder and epoxy resin and polyamide with weight ratio, mixing pressure is 35kN, and pressurize 2min 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 84%, silicon 8%, aluminium 4.5%, nickel 3.5% 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 FeSiAlNi 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 25m/s;
3) the FeSiAlNi strip 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
-2Pa 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 40min cools off with stove;
5) be 50: 1: 0.5 mixing anti-electromagnetic interference materials of laminar pliability that are processed into 2mm with flat powder and epoxy resin and polyamide with weight ratio, mixing pressure is 35kN, and pressurize 2min puts into heat-treatment furnace and is heated to 160 ℃, insulation 40min, 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 90%, silicon 6%, aluminium 2.5%, nickel 1.5% 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 FeSiAlNi 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 FeSiAlNi strip 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
-5Pa 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 873K, insulation 30min cools off with stove;
5) be 50: 1: 0.75 mixing anti-electromagnetic interference materials of laminar pliability that are processed into 4mm with flat powder and epoxy resin and polyamide with weight ratio, mixing pressure is 35kN, and pressurize 2min puts into heat-treatment furnace and is heated to 100 ℃, insulation 60min, 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 86.5%, silicon 5%, aluminium 6%, nickel 2.5% 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 FeSiAlNi foundry alloy is put into fast quenching equipment, and alloy cast ingot obtains the strip or 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 30m/s;
3) the FeSiAlNi strip 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 300r/min;
4) flat powder is put into stainless steel tube, be evacuated down to 10
-4Pa 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 50min cools off with stove;
5) be 50: 1: 1 mixing anti-electromagnetic interference materials of laminar pliability that are processed into 5mm with flat powder and epoxy resin and polyamide with weight ratio, mixing pressure is 35kN, and pressurize 2min puts into heat-treatment furnace and is heated to 150 ℃, insulation 40min, 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 85%, silicon 7%, aluminium 3.5%, nickel 4.5% 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 FeSiAlNi 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 FeSiAlNi 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 40min cools off with stove;
5) be 50: 1: 0.5 mixing anti-electromagnetic interference materials of laminar pliability that are processed into 3mm with flat powder and epoxy resin and polyamide with weight ratio, mixing pressure is 20kN, and pressurize 2min 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 7%, aluminium 3.5%, nickel 4.5% 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 FeSiAlNi 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 FeSiAlNi 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
-4Pa 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: 1 mixing anti-electromagnetic interference materials of laminar pliability that are processed into 5mm with flat powder and epoxy resin and polyamide with weight ratio, mixing pressure is 35kN, and pressurize 2min puts into heat-treatment furnace and is heated to 200 ℃, insulation 30min, air cooling.
Embodiment 7:
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 27.5m/s;
3) the FeSiAl strip 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 773K, insulation 60min cools off with stove;
5) be 50: 1: 0.75 mixing anti-electromagnetic interference materials of laminar pliability that are processed into 5mm with flat powder and epoxy resin and polyamide with weight ratio, mixing pressure is 35kN, and pressurize 2min puts into heat-treatment furnace and is heated to 200 ℃, insulation 30min, air cooling.
Claims (3)
1. the preparation method of an electromagnetic wave interference resisting iron, silicon, aluminum and nickel alloy is characterized in that comprising the steps:
1) adopting purity is raw material greater than Fe, Al, Si, the Ni 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 being poured into rapidly on the water-cooled running roller of high speed rotating after the remelting of process electric arc under the high purity inert gas protection, obtain the FeSiAlNi strip or the FeSiAlNi thin slice of rapid condensation, the speed of quenching is 15~35m/s;
3) FeSiAlNi strip or FeSiAlNi thin slice are put into ball mill and carried out the ball milling flattening and handle, obtain 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 purity inert gas protection, and air pressure is 0.5 * 10
5~1 * 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) the mixing thin slice that is processed into 2~5mm of flat powder and binding agent, pressure is 20~40kN, puts into heat-treatment furnace and heats 100~200 ℃, insulation 30~60min, air cooling.
2. a kind of anti-electromagnetic wave according to claim 1 disturbs the preparation method who mixes this special alloy of nickel celestial platform, it is characterized in that the weight ratio that described foundry alloy is formed is: iron 84~90%, silicon 4~8%, aluminium 2~6%, nickel 1.5~5.5%;
3. the preparation method of a kind of electromagnetic wave interference resisting iron, silicon, aluminum and nickel alloy according to claim 1 is characterized in that described binding agent is epoxy resin and polyamide, and the weight ratio of epoxy resin and polyamide is 1: 1~0.5.
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CN113351883A (en) * | 2021-08-11 | 2021-09-07 | 天津大学 | Method for preparing CuCrZr/316L connecting piece based on laser additive manufacturing technology |
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