CN100365746C - A Bulk Amorphous Nanocrystalline Two-Phase Composite Soft Magnetic Alloy - Google Patents
A Bulk Amorphous Nanocrystalline Two-Phase Composite Soft Magnetic Alloy Download PDFInfo
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- CN100365746C CN100365746C CNB2004100532527A CN200410053252A CN100365746C CN 100365746 C CN100365746 C CN 100365746C CN B2004100532527 A CNB2004100532527 A CN B2004100532527A CN 200410053252 A CN200410053252 A CN 200410053252A CN 100365746 C CN100365746 C CN 100365746C
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- amorphous
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- soft magnetic
- magnetic alloy
- phase composite
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- 239000002131 composite material Substances 0.000 title claims abstract description 14
- 229910001004 magnetic alloy Inorganic materials 0.000 title claims abstract description 14
- 229910052802 copper Inorganic materials 0.000 claims abstract description 8
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 4
- 229910052796 boron Inorganic materials 0.000 claims abstract description 4
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 4
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract 2
- 239000013078 crystal Substances 0.000 claims description 9
- 229910045601 alloy Inorganic materials 0.000 abstract description 15
- 239000000956 alloy Substances 0.000 abstract description 15
- 238000005245 sintering Methods 0.000 abstract description 13
- 238000002360 preparation method Methods 0.000 abstract description 9
- 239000000843 powder Substances 0.000 abstract description 8
- 230000006698 induction Effects 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 3
- 241001062472 Stokellia anisodon Species 0.000 abstract description 2
- 230000007123 defense Effects 0.000 abstract 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract 1
- 238000010791 quenching Methods 0.000 abstract 1
- 230000000171 quenching effect Effects 0.000 abstract 1
- 238000004781 supercooling Methods 0.000 abstract 1
- 229910052721 tungsten Inorganic materials 0.000 abstract 1
- 238000000498 ball milling Methods 0.000 description 9
- 239000010949 copper Substances 0.000 description 9
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052774 Proactinium Inorganic materials 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000011162 core material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007578 melt-quenching technique Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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- Powder Metallurgy (AREA)
- Soft Magnetic Materials (AREA)
Abstract
本发明为一种块体非晶纳米晶双相复合软磁合金。该软磁合金由Fe、Zr、Nb、B、Cu、X按一定的质量配比组成，其中，X为Si、Al、V、Mo、W之一种或几种。其制备方法是，先在真空中频感应炉中冶炼母合金，再用单辊急冷甩带机制备非晶带，然后低温球磨制得非金粉末，最后在非晶粉末过冷区温度范围内进行高压快速烧结而成。本发明产品具有高的饱和磁感应强度，可用于电机磁芯、配电变压器、大功率开关电源等国防和民用产品中。The invention is a bulk amorphous and nanocrystalline dual-phase composite soft magnetic alloy. The soft magnetic alloy is composed of Fe, Zr, Nb, B, Cu and X in a certain mass ratio, wherein X is one or more of Si, Al, V, Mo and W. The preparation method is to first smelt the master alloy in a vacuum intermediate frequency induction furnace, then use a single-roller quenching strip machine to prepare an amorphous strip, then use a low-temperature ball mill to obtain a non-gold powder, and finally carry out the process in the temperature range of the supercooling zone of the amorphous powder. High pressure rapid sintering. The product of the invention has high saturation magnetic induction intensity, and can be used in national defense and civilian products such as motor magnetic cores, distribution transformers, and high-power switching power supplies.
Description
Technical field
The invention belongs to technical field of magnetic materials, particularly a kind of bulk amorphous alloy nanometer crystal double-phase composite soft magnetic alloy.
Background technology
For adapting to miniaturization, the high performance requirement of motor, press for and develop core material with high saturated magnetic induction.For special machines, require its magnetic circuit to have special spatial distribution, thereby core material to be block usually, and complex-shaped.Yet the amorphous and nanocrystalline soft magnetic alloy of practical application is at present normally obtained by fast melt-quenching+amorphous crystallization process, and its shape and size are subjected to great restriction, only can provide shapes such as strip, powder, filament, can not satisfy the needs that engineering is used.
Summary of the invention
The object of the present invention is to provide and a kind ofly have high saturated magnetic induction and than the amorphous bulk nanometer crystal double-phase composite soft magnetic alloy of low production cost.
The bulk amorphous alloy nanometer crystal double-phase composite soft magnetic alloy that the present invention proposes is the Fe-Zr-Nb magnetically soft alloy, and its component proportioning by weight is as follows:
Fe:83.5-89%, Zr:3-7%, Nb:3-7%, B:3-9%, Cu:0.5-1%, X:1-5%, total amount satisfies 100%, and X is an intensified element, is one or more of Si, Al, V, Mo, W.
The preparation method of the amorphous bulk nanometer crystal double-phase composite soft magnetic alloy that the present invention proposes is as follows: smelting nut alloy in the induction furnace frequently at first in a vacuum, get rid of band mechanism amorphous ribbon fully with single roller chilling again; With ball mill to the amorphous ribbon of gained under the Ar gas shiled, carry out-a 100-0 ℃ low temperature ball milling prepares amorphous powder; In amorphous powder is crossed the cold-zone temperature range, carry out the high pressure Fast Sintering under the 3.5-5.5Gpa sintering pressure, prepare the bulk amorphous alloy nanometer crystal double-phase composite soft magnetic alloy at last.
In the said method, when freezing the refining foundry alloy, utilize vacuum medium frequency induction furnace to smelt Fe, Zr, Nb ingot earlier, be melted to 1000 ℃ ± 100 ℃, add all the other elements (as B, Si, Al, Cu etc.) again, cast makes master alloy ingot.Getting rid of band mechanism with single roller chilling and be equipped with amorphous ribbon, is behind fusion foundry alloy under the Ar Buchholz protection, is injected into amorphous ribbon, and pressure is 450-550Pa, copper roller linear velocity 40～70m/s, quartz nozzle width 30mm.Low temperature ball mill ball milling amorphous ribbon makes amorphous powder, and its temperature is-100 ℃～0 ℃, and rotating speed is 250～540r/min, and ratio of grinding media to material is 10～30, and the ball milling time is 10～30h.The high pressure Fast Sintering makes the bulk amorphous alloy nanometer crystal double-phase composite soft magnetic alloy, and its sintering temperature is 350 ℃～550 ℃, and sintering pressure is 3.5～5.5GPa, and sintering time is 3～10min, dwell time 3min.Also to heat-treat Ar gas shiled, 250 ℃～400 ℃ of temperature, time 0.5～1h as last.
Novel block Fe-Zr-Nb of the present invention is that amorphous nanometer crystal double-phase composite soft magnetic alloy has been broken through the restriction of original nano-crystal soft magnetic alloy on size and dimension, has high saturation induction density, can be used for the national defence and the product for civilian use, as: motor core, distribution transformer, high power switching power supply, pulse transformer, magnetic amplifier, intermediate frequency transformer and inverter iron core or the like.Preparation technology of the present invention has simply, cost is low, be easy to realize characteristics such as industrialization, has wide research and market application foreground.
Embodiment
The invention is further illustrated by the following examples.
Embodiment 1: the compound Fe of the nanocrystalline two-phase of amorphous bulk
86.5Zr
4Nb
3B
3Si
2Al
1Cu
0.5Magnetically soft alloy.The preparation technology of bulk alloy as previously mentioned.During vacuum metling, vacuum degree is 6 * 10
-3Pa, in the amorphous ribbon preparation, protective gas is Ar, and copper roller linear velocity is 50m/s, and the amorphous thin ribbon that obtains is thick to be 14 microns, wide 20 millimeters.With planetary low temperature ball mill amorphous ribbon is broken into the about 14 microns amorphous powder of particle diameter, the ball milling temperature is-20 ℃, and rotating speed is 400r/min, and ratio of grinding media to material is 10, ball milling time 15h.The high-pressure sinter temperature is 450 ℃, sintering pressure 5.5GPa, sintering time 3min.The nanocrystalline two-phase composite alloy of bulk amorphous alloy that obtains is of a size of that Φ 25 * 10mm, relative density are 98.9%, average nanocrystalline grain size is 15.7nm, and saturation magnetization Ms is 1.60T.
Embodiment 2: the compound Fe of the nanocrystalline two-phase of amorphous bulk
84Zr
3Nb
3Mo
1B
8Cu
1Magnetically soft alloy.The preparation of bulk alloy as previously mentioned.During vacuum metling, vacuum degree is 6 * 10
-3Pa, in the amorphous ribbon preparation, protective gas is Ar, and copper roller linear velocity is 40m/s, and the amorphous thin ribbon that obtains is thick to be 15 microns, wide 20 millimeters.With planetary low temperature ball mill amorphous ribbon is broken into the about 15 microns amorphous powder of particle diameter, the ball milling temperature is-40 ℃, and rotating speed is 450r/min, and ratio of grinding media to material is 15, ball milling time 10h.The high-pressure sinter temperature is 480 ℃, sintering pressure 5.5GPa, sintering time 3min.The nanocrystalline two-phase composite alloy of bulk amorphous alloy that obtains is of a size of that Φ 25 * 10mm, relative density are 98.7%, average nanocrystalline grain size is 15.3nm, and saturation magnetization Ms is 1.49T.
Embodiment 3: the compound Fe of the nanocrystalline two-phase of amorphous bulk
83.5Zr
3Nb
3.5V
0.9W
0.5B
7.6Cu
1Magnetically soft alloy.The preparation of bulk alloy as previously mentioned.During vacuum metling, vacuum degree is 6 * 10
-3Pa, in the amorphous ribbon preparation, protective gas is Ar, and copper roller linear velocity is 60m/s, and the amorphous thin ribbon that obtains is thick to be 13 microns, wide 20 millimeters.With planetary low temperature ball mill amorphous ribbon is broken into the about 13 microns amorphous powder of particle diameter, the ball milling temperature is-0 ℃, and rotating speed is 300r/min, and ratio of grinding media to material is 20, ball milling time 20h.The high-pressure sinter temperature is 430 ℃, sintering pressure 5.5GPa, sintering time 3min.The nanocrystalline two-phase composite alloy of bulk amorphous alloy that obtains is of a size of that Φ 25 * 10mm, relative density are 98.9%, average nanocrystalline grain size is 16.5nm, and saturation magnetization Ms is 1.43T.
In the foregoing description, the index number of element is the weight percent content of this element.
Claims (1)
1. an amorphous bulk nanometer crystal double-phase composite soft magnetic alloy is characterized in that being made up of Fe, Zr, Nb, B, Cu, X, and the quality proportioning of each component is as follows:
Fe：83.5-89％，
Zr：3-7％，
Nb：3-7％，
B：3-9％，
Cu：0.5-1％，
X：1-5％，
Total amount satisfies 100%, and X is one or more among Si, Al, V, Mo, the W here.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100532527A CN100365746C (en) | 2004-07-29 | 2004-07-29 | A Bulk Amorphous Nanocrystalline Two-Phase Composite Soft Magnetic Alloy |
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| CNB2004100532527A CN100365746C (en) | 2004-07-29 | 2004-07-29 | A Bulk Amorphous Nanocrystalline Two-Phase Composite Soft Magnetic Alloy |
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| Publication Number | Publication Date |
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| CN1588580A CN1588580A (en) | 2005-03-02 |
| CN100365746C true CN100365746C (en) | 2008-01-30 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321216C (en) * | 2005-06-23 | 2007-06-13 | 安泰科技股份有限公司 | Low cost iron based nano crystal alloy possessing improved fabricating properties, and manufacutring method |
| CN101768677B (en) * | 2010-02-09 | 2012-08-29 | 江苏大学 | Preparation method of high-performance room temperature complex-phase magnetic cooling material |
| CN102102167B (en) * | 2010-12-23 | 2012-09-05 | 南京航空航天大学 | Iron-based nanocrystalline soft magnetic alloy with high quenching state toughness and wide annealing temperature range |
| CN103219145B (en) * | 2012-01-19 | 2015-07-29 | 北京大学 | The preparation method of a kind of SmCo and iron cobalt built-up magnet |
| CN102962465B (en) * | 2012-11-22 | 2015-02-04 | 德清森腾电子科技有限公司 | Low magnetic permeability, low power consumption sendust soft magnetic material and preparation method thereof |
| CN103060723B (en) * | 2012-12-02 | 2014-11-05 | 上海理工大学 | Amorphous nanocrystalline magnetically soft alloy and preparation method thereof |
| CN111850431B (en) * | 2019-09-23 | 2022-02-22 | 宁波中科毕普拉斯新材料科技有限公司 | Iron-based amorphous alloy containing sub-nanoscale ordered clusters, preparation method and nanocrystalline alloy derivative thereof |
| CN114360883B (en) * | 2021-12-31 | 2022-11-01 | 华南理工大学 | A kind of high magnetic induction magnetic powder core based on amorphous crystallization bifunctional element and its preparation method and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1173608A (en) * | 1997-08-29 | 1999-03-16 | Alps Electric Co Ltd | Inductive head |
| JP2001152301A (en) * | 1999-11-19 | 2001-06-05 | Alps Electric Co Ltd | Soft magnetic glassy alloy |
| JP2002194514A (en) * | 2000-12-22 | 2002-07-10 | Japan Science & Technology Corp | Soft magnetic, high strength Fe-Co-Ni based metallic glass alloy |
| CN1450570A (en) * | 2003-04-10 | 2003-10-22 | 同济大学 | Nano crystal soft magnetic alloy superthin belt and mfg method thereof |
-
2004
- 2004-07-29 CN CNB2004100532527A patent/CN100365746C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1173608A (en) * | 1997-08-29 | 1999-03-16 | Alps Electric Co Ltd | Inductive head |
| JP2001152301A (en) * | 1999-11-19 | 2001-06-05 | Alps Electric Co Ltd | Soft magnetic glassy alloy |
| JP2002194514A (en) * | 2000-12-22 | 2002-07-10 | Japan Science & Technology Corp | Soft magnetic, high strength Fe-Co-Ni based metallic glass alloy |
| CN1450570A (en) * | 2003-04-10 | 2003-10-22 | 同济大学 | Nano crystal soft magnetic alloy superthin belt and mfg method thereof |
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