CN1613584A - Preparation for blocking nanometer crystal soft magnetic alloy - Google Patents
Preparation for blocking nanometer crystal soft magnetic alloy Download PDFInfo
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- CN1613584A CN1613584A CN 200410066613 CN200410066613A CN1613584A CN 1613584 A CN1613584 A CN 1613584A CN 200410066613 CN200410066613 CN 200410066613 CN 200410066613 A CN200410066613 A CN 200410066613A CN 1613584 A CN1613584 A CN 1613584A
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Abstract
A process for preparing nano-crystal block of soft-magnetic alloy includes such steps as using the mechanical alloying method to prepare nano-crystal powder, and low-temp high-pressure fast shaping by hexagonal hydraulic technique. Its advantages are simple process and high density.
Description
Technical field
The invention belongs to the nano-crystal soft magnetic alloy technical field that relates in the functional material, be specifically related to a kind of preparation method of bulk nano-crystalline magnetically soft alloy.
Background technology
For the miniaturization that adapts to motor, the requirement of high performance, press for and develop the core material that has high saturated magnetic induction and excellent soft magnetic characteristic simultaneously.For special machines, particularly require its magnetic circuit to have special spatial distribution, requiring core material usually is block, and complex-shaped.Fe-Si-B-Nb-Cu system and Fe-(Zr, Hf, Nb)-B system nano-crystal alloy has than more outstanding soft magnetic characteristic of Fe base noncrystal alloy and high saturation induction density, therefore, from discovery Fe such as Yoshizawa in 1988
73.5Si
13.5B
9Nb
3Cu
1Behind the nanometer crystal alloy, this class nanometer crystal alloy has caused the great attention of countries in the world always.
Yet the nano-crystal soft magnetic alloy of practical application is normally obtained by fast melt-quenching control amorphous crystallization process, and its shape and size are subjected to very big restriction, only can provide shapes such as strip, powder, filament.At present, the existing report that adopts high pressure concretion method, warm extrusion, explosive forming method, discharge plasma sintering method (being called for short SPS) successfully to prepare amorphous or nano-crystal soft-magnetic block alloy, but relevant mechanical alloying (being called for short MA) the nano-crystal soft magnetic alloy powder that adopts of Shang Weijian obtains the report of nano-crystal soft-magnetic block alloy.In these powder metallurgy process, the high pressure concretion method is considered to a kind of preparation method of comparatively ideal bulk nanocrystalline alloy, but, it needs special high-tension apparatus usually, and, the shape and size of block also are subjected to very big restriction, are difficult to obtain big block nano-crystal soft magnetic alloy, can not satisfy the needs that engineering is used.
Summary of the invention
The objective of the invention is to propose the method for the nano-crystal soft-magnetic block alloy of a kind of technology preparation high-compactness simple, with low cost, can not prepare the problem of blocks of large nano-crystal soft magnetic alloy to solve conventional high-tension equipment.
The preparation method of the brilliant magnetically soft alloy of the lumpy nanometer that the present invention proposes prepares manocrystalline powders by mechanical alloying method, prepares the bulk nano-crystalline magnetically soft alloy through the cryogenic high pressure rapid shaping again.
Concrete steps are as follows:
Mechanical alloying method prepares the nanometer crystal alloy powder:
The component element powder of nano-crystal soft magnetic alloy is pressed prealloy composition quality proportion ingredient; put into ball grinder; under the Ar Buchholz protection, carry out high-energy ball milling; realize prepared by mechanical alloy nano-crystal soft magnetic alloy powder; the ball grinder rotating speed is 250～450rpm, and the mechanical alloying time is 15～75h.Here, the unit of magnetically soft alloy have Fe, Co, Zr, Mn, Cu, W, B, S etc., can require to adjust according to difference, and the particle diameter of each element powders is that 50-85 μ m is better.
The cryogenic high pressure rapid shaping:
Adopt pyrophillite high-pressure chamber device shown in Figure 1, carry out pre-molding in the graphite boat of earlier amorphous or nano-crystal soft magnetic alloy powder being packed into, pressure is 10～30MPa, carries out vacuum degassing subsequently.The graphite boat that fills the pre-molding alloy powder is loaded in the pyrophillite high-pressure chamber by structural group shown in Figure 1, on the high hydraulic test of cubic apparatus, carry out the cryogenic high pressure rapid shaping, prepare the bulk nano-crystalline magnetically soft alloy, briquetting pressure is 3.5～5.5GPa, dwell time is 3～10min, the delay dwell time is 2-4min, and the cryogenic high pressure quick shaping process is seen shown in Figure 2.
At last, under the Ar Buchholz protection bulk nano-crystalline magnetically soft alloy is heat-treated to eliminate residual stress and to adjust heterogeneous microstructure, the reprocessing heating-up temperature is 350～550 ℃, and be 0.5～1.5h heating time.
The pyrophillite high-pressure chamber device that the present invention uses, its structure is made up of leaf film stone chamber wall, graphite boat, steel bowl as shown in Figure 1, and wherein, graphite boat 2 places steel bowl 5, and the upper and lower opening place of graphite boat 1 is provided with pad 3, between each steel bowl titanium sheet 4 is arranged, and separates.Steel bowl 5 is assembled in the pyrophillite cavity, and leaf film masonry is the pressure transmission medium.
Because nanometer powder has high surface activation energy, though can obviously improve the sintering densification actuating force, reduce sintering temperature, also significantly improve the growth rate of nanocrystal simultaneously inevitably.In the normal sintering process, because the existence of micropore, these bigger micropores need higher temperature or longer sintering time could realize the closed pore process, cause sintering densification speed to be significantly less than the growth rate of crystal grain, grain growth trend is obvious, is difficult to obtain bulk nanometer material.High sintering pressure can be eliminated large-sized pore effectively, thereby obviously improves sintering densification speed.High pressure can also reduce the surface activation energy significantly, promotes the diffusion process of granular boundary atom, and sintering temperature is reduced greatly.For the MA manocrystalline powders, though crystallite dimension is in nanoscale, but powder particle size still is in micron order, in addition, exist distortion of lattice in the powder and store energy, usually therefore the growth rate that causes nanocrystal, adopts the prior powder metallurgy method to be difficult to obtain the bulk nanocrystalline alloy of high densification apparently higher than sintering densification speed.But, under high sintering pressure, accelerated sintering closed pore process on the one hand, shorten the densification time, can obviously increase the activation energy of diffusion in Fe (or Co) matrix such as alloying element such as Nb, Zr etc. on the other hand, have and obviously delay the effect that nanocrystal is grown up.Compare with condition of normal pressure, obtain the nanocrystal tissue easily.
The invention provides a kind of preparation method who adopts the high hydraulic technique of cubic apparatus to prepare the nano-crystal soft-magnetic block alloy, solved the problem that conventional high-tension equipment can not be prepared the blocks of large nano-crystal soft magnetic alloy.The block alloy of high densifications such as acquisition simultaneously compared with prior art, technology of the present invention is simple, with low cost, be easy to suitability for industrialized production.
Description of drawings
Fig. 1 is a pyrophillite cavity body structure schematic diagram.
Fig. 2 is a cryogenic high pressure quick shaping process curve.
Number in the figure: 1 is the pyrophillite cavity wall, and 2 is graphite boat, and 3 is pad, and 4 is the titanium sheet, and 5 is the steel bowl, and 6 is alloy powder.
Embodiment
Embodiment 1:
Select that purity is higher than 99%, Fe, Nb, W pure element and Fe-20B (wt%) the intermediate alloy powder of the about 75 μ m of particle diameter for use, press alloy composition Fe
84Nb
4W
3B
9Proportion ingredient is that 450rad/min, ratio of grinding media to material are that ball milling 60h carries out mechanical alloying under 20: 1 the condition at the ball grinder rotating speed, preparation Fe
84Nb
4W
3B
9The nano-crystal soft magnetic alloy powder.In the pyrophillite cavity body structure, on the high hydraulic test of cubic apparatus, carry out the cryogenic high pressure rapid shaping, pressure P=5.5GPa, heating power P
w=980W, heating time, t=3min obtained being of a size of Φ 25 * 10, relative density d=98.2%, average grain size is the bulk nano-crystalline magnetically soft alloy material of 17.2nm, its saturation magnetization M
sBe 1.55T.
Embodiment 2:
Select that purity is higher than 99%, Fe, Nb, Cu, Si and the B pure element powder of the about 85 μ m of particle diameter for use, press alloy composition proportioning Fe
73.5Cu
1Nb
3Si
13.5B
9Batching is that 450rad/min, ratio of grinding media to material are that ball milling 70h carries out prepared by mechanical alloy Fe under 20: 1 the condition at the ball grinder rotating speed
73.5Cu
1Nb
3Si
13.5B
9The nano-crystal soft magnetic alloy powder.In the pyrophillite cavity body structure, on the high hydraulic test of cubic apparatus, carry out the cryogenic high pressure rapid shaping, pressure P=3.5GPa, heating power P
w=980W, heating time, t=5min obtained being of a size of Φ 25 * 10, relative density d=98.4%, average grain size is the bulk nano-crystalline magnetically soft alloy material of 12.4nm, its saturation magnetization M
sBe 1.23T.
Embodiment 3:
Select that purity is higher than 99%, Fe, Nb and Fe-20B (wt%) the intermediate alloy powder of the about 75 μ m of particle diameter for use, press alloy composition proportioning Fe
73.5Cu
1Nb
3Si
13.5B
9Batching is that 400rad/min, ratio of grinding media to material are that ball milling 70h carries out prepared by mechanical alloy Fe under 25: 1 the condition at the ball grinder rotating speed
73.5Cu
1Nb
3Si
13.5B
9The nano-crystal soft magnetic alloy powder.In the pyrophillite cavity body structure, on the high hydraulic test of cubic apparatus, carry out the cryogenic high pressure rapid shaping, pressure P=5GPa, heating power P
w=980W, heating time, t=3min obtained being of a size of Φ 25 * 10, relative density d=97.9%, average grain size is the bulk nano-crystalline magnetically soft alloy material of 13.2nm, its saturation magnetization M
sBe 1.56T.
Claims (3)
1, a kind of preparation method of bulk nano-crystalline magnetically soft alloy is characterized in that concrete steps are as follows:
(1) the each component element powders of nano-crystal soft magnetic alloy is put into ball grinder, under the Ar Buchholz protection, carry out high-energy ball milling, realize prepared by mechanical alloy nano-crystal soft magnetic alloy powder, the ball grinder rotating speed is 250～450rpm, and the mechanical alloying time is 15～75h;
(2) adopt pyrophillite high-pressure chamber device, in the graphite boat of earlier the nano-crystal soft magnetic alloy powder that makes being packed into, carry out pre-molding, pressure is 10～30MPa, carries out vacuum degassing then; The graphite boat that fills the pre-molding alloy powder is assembled in the pyrophillite high-pressure chamber, on the high hydraulic test of cubic apparatus, carry out the cryogenic high pressure rapid shaping, make the bulk nano-crystalline magnetically soft alloy, here briquetting pressure is 3.5～5.5GPa, dwell time is 3～10min, and the delay dwell time is 2-4min.
2, preparation method according to claim 1 is characterized in that the element of described magnetically soft alloy comprises Fe, Co, Zr, Mn, Cu, W, B, S, and the powder diameter of element is 50-85 μ m.
3, preparation method according to claim 1 is characterized in that the block magnetically soft alloy that makes is heat-treated under the Ar Buchholz protection, and heat treatment temperature is 350～550 ℃, and the time is 0.5～1.5h.
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|---|---|---|---|
| CN 200410066613 CN1613584A (en) | 2004-09-23 | 2004-09-23 | Preparation for blocking nanometer crystal soft magnetic alloy |
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|---|---|---|---|
| CN 200410066613 CN1613584A (en) | 2004-09-23 | 2004-09-23 | Preparation for blocking nanometer crystal soft magnetic alloy |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456075B (en) * | 2007-12-14 | 2010-11-24 | 比亚迪股份有限公司 | Preparation method of nano-crystal soft magnetic alloy elements |
| CN101930840A (en) * | 2009-06-25 | 2010-12-29 | 越峰电子（昆山）有限公司 | Soft magnetic ferrite magnetic core forming method and forming die thereof |
| CN108447642A (en) * | 2018-05-18 | 2018-08-24 | 同济大学 | A kind of preparation method of soft-magnetic composite material |
| CN109023184A (en) * | 2018-09-03 | 2018-12-18 | 湘潭大学 | A method of preparing the iron-nickel alloy containing shot-range ordered structure |
| CN109097657A (en) * | 2018-10-23 | 2018-12-28 | 中南大学 | A kind of Mo nano-particle reinforcement CoCrNi medium entropy alloy composite materials and preparation method thereof |
-
2004
- 2004-09-23 CN CN 200410066613 patent/CN1613584A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456075B (en) * | 2007-12-14 | 2010-11-24 | 比亚迪股份有限公司 | Preparation method of nano-crystal soft magnetic alloy elements |
| CN101930840A (en) * | 2009-06-25 | 2010-12-29 | 越峰电子（昆山）有限公司 | Soft magnetic ferrite magnetic core forming method and forming die thereof |
| CN108447642A (en) * | 2018-05-18 | 2018-08-24 | 同济大学 | A kind of preparation method of soft-magnetic composite material |
| CN109023184A (en) * | 2018-09-03 | 2018-12-18 | 湘潭大学 | A method of preparing the iron-nickel alloy containing shot-range ordered structure |
| CN109097657A (en) * | 2018-10-23 | 2018-12-28 | 中南大学 | A kind of Mo nano-particle reinforcement CoCrNi medium entropy alloy composite materials and preparation method thereof |
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