CN104878327A - Ferrum-based amorphous magnetically-soft alloy material and preparation method therefor - Google Patents
Ferrum-based amorphous magnetically-soft alloy material and preparation method therefor Download PDFInfo
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Abstract
The invention relates to a ferrum-based amorphous magnetically-soft alloy material and a preparation method therefor and belongs to the technical field of new materials. The material simultaneously contains seed constituent elements, i.e., Fe, B, Si and Hf in atomic percentage content: 0.5-5.0at.% of Hf, 3.0-13.0at.% of Si, 5.0-20.0at.% of B and the balance of Fe (higher than 70.0at.%). Process flows for preparing strip and block samples of the material are simple, convenient and efficient, prepared magnetically-soft amorphous alloy is good in formability and has an obvious glass transition temperature spot Tg and a relatively wide supercold liquid-phase range [delta]Tx, and the problem of brittleness of the traditional magnetically-soft amorphous alloy is overcome. The material has the characteristics of high amorphous forming ability, high saturation magnetic induction density and low coercive force, and the maximum critical diameter of formed block amorphous alloy reaches 3mm; the maximum saturation magnetic induction density of Fe-B-Si-Hf magnetically-soft amorphous alloy exceeds 1.65T, and each coercive force is lower than 2A/m; the material can serve as materials for power distribution transformer cores or other electronic power devices.
Description
Technical field
The present invention relates to a kind of iron base amorphous magnetically-soft alloy material and preparation method thereof, belong to new material technology field.
Background technology
From Fe in 1967
75p
15c
10since (atomic percent composition) soft magnetic amorphous alloy is successfully prepared, magnetic AMORPHOUS ALLOY is subject to extensive concern always.Magnetic amorphous alloy material known at present mainly contains: VIII metal-eka-gold genotype non-crystaline amorphous metal; VIII metal-transition metal type non-crystaline amorphous metal and VIII metal-rare earth metal type non-crystaline amorphous metal.Here, VIII metal is Fe, Co, Ni element; Metalloid is mainly B, C, P, Si; Transition metal is Ta, Nb, Zr, Hf, Y and composition thereof mainly; The rare earth metal then mainly element such as Gd, Tb, Dy, Nd.Due to the with low cost and soft magnetic performance had of Fe, the soft magnetic amorphous alloy being matrix with it obtains application.
But the amorphous formation ability of traditional magnetic alloy is lower, its critical cooling rate forming amorphous is usually 10
5more than K/s, need could obtain by melt spinning the band non-crystalline material that thickness is no more than 0.1mm, preparation condition is relatively harsh, and relevant non-crystal bar is more crisp, and this constrains the application and development of soft magnetic amorphous alloy to a great extent.Until nineteen nineties, the people such as Japanese scholars Inoue take the lead in using copper mold casting to take the lead in preparing Fe-(Al, Ga)-(P, C, B) iron-base block amorphous alloy, just overcome the deficiency of soft magnetic amorphous alloy stripping.So far, people have developed the iron-base block amorphous system of multiple type.Such as, Fe-M-(P, C, B, Si) (M=Al, Ga, Mo), Fe-Cr-Mo-C-B-Ln (rare earth element) and Fe-B-Si-(Zr, Nb) etc.Visible, people are mostly the amorphous formation abilities promoting Fe base alloy by adding various nonmagnetic elements, but adding of these elements often makes the saturation induction density of original non-crystaline amorphous metal obviously reduce, and causes its magnetic performance to worsen.Therefore, exploitation there is high amorphous formation ability, the novel Fe base noncrystal alloy of high saturated magnetic induction have important practical be worth.
The Fe-based amorphous alloy with large-amorphous forming capacity generally has more than 3 constituent elements, causes the complicacy of such design of alloy and optimization.The non-crystaline amorphous metal of best Forming ability composition, from " cluster+connection atom " model of the desirable non-crystaline amorphous metal of wound, is described as [cluster] (connection atom) x, x with " cluster formula " unity of form and gets 1 or 3 by us.Associate organic to the composition of non-crystaline amorphous metal, structure and Forming ability thereof smoothly, the quantitative Composition Design of non-crystaline amorphous metal can be realized with this.The present invention is by this certain amount of composition design method, based on Fe-B-Si band amorphous, introduce paramagnetic alloying constituent element Hf, to find in Fe-B-Si-Hf alloy system first and to prepare the Fe of large-amorphous forming capacity base block amorphous, and optimize the iron base amorphous magnetically-soft alloy series with high saturated magnetic induction and low-coercivity.
Summary of the invention
The technical problem to be solved in the present invention is: (1) obtains the Fe-based amorphous soft magnetic materials simultaneously with large-amorphous forming capacity, high saturated magnetic induction and low-coercivity; (2) complicacy simplifying the screening of multicomponent alloy system amorphous component and optimize; (3) provide that a kind of cost is low, the simple high Fe content soft magnetism Applied Materials of preparation method.
The technical solution used in the present invention is: a kind of Fe-B-Si-Hf soft magnetic amorphous alloy material having high saturated magnetic induction, low-coercivity and large-amorphous forming capacity concurrently, the chemical constitution of this material is: Fe
100-x-y-zb
xsi
yhf
z, wherein x, y, z is atomic percent (at. %), 5.0%≤x≤20.0%, and 3.0 %≤y≤13.0%, 0.5%≤z≤5.0%, Fe atomic percent is higher than 70.0%.Its maximum saturation magnetic induction density is more than 1.65T, and coercive force is all lower than 2A/m; Can be used as type substation transformer iron core or other power electronic component ideal material.
Containing the preparation method of Hf iron base amorphous magnetically-soft alloy material, comprise composition proportion, weighing, alloy melting, get rid of band and copper mold casting, concrete technology step comprises:
(1) get the raw materials ready: according to the chemical constitution Fe of this material
100-x-y-zb
xsi
yhf
z, convert the atomic percent (at. %) of Fe, B, Si, Hf to weight percent (wt. %), then take each constituent element raw metal by weight percentage, stand-by; In chemical constitution, x, y, z is atomic percent, 5.0%≤x≤20.0%, 3.0 %≤y≤13.0%, 0.5%≤z≤5.0%, and Fe atomic percent is higher than 70.0%; Raw metal purity used is all not less than technical pure;
(2) melting of alloy pig: by each constituent element raw metal mixing weighed, put into the water jacketed copper crucible of non-consumable arc-melting furnace, carry out alloy melting, melt back three to four times under pure argon protection, obtain the alloy pig of uniform composition; Rate of weight loss before and after alloy pig melting controls within 5/1000ths;
(3) sample preparation: alloy pig is prepared into Tape samples or block sample;
The preparation process of Tape samples: alloy pig is broken, put into the silica tube that nozzle is long 8mm × wide 1mm, single roller is used to get rid of band technology, by induction heating technique by the alloy material fusing in silica tube, and with high-purity argon gas, alloy melt is blown out, make it be ejected on the water-cooled copper roller of high speed rotating, make alloy strip sample; The linear resonance surface velocity of described water-cooled copper roller is 15 ~ 50m/s;
The preparation process of block sample: alloy pig be placed in silica tube induction melting and be incubated, opens in quenching temperature and blows casting device, allow alloy melt spray in cylindrical water cooled copper mould die cavity, be cooled to room temperature, obtain block sample; Or alloy pig is directly melted by electric arc, then suck under negative pressure in cylindrical water cooled copper mould die cavity, be cooled to room temperature and obtain block sample.
Below provide experiment detection technique means of the present invention.
First, X-ray diffractometer (Bruker D8) is utilized to carry out structure detection to obtained band or block sample.If what diffracting spectrum shows completely typical non-crystalline state feature disperses steamed bun peak, then show that alloy is homogeneous amorphous structure, and can confirm via transmission electron microscopy.Then, differential thermal analyzer (TA Q600) is utilized to measure the thermodynamical coordinate of amorphous sample, wherein glass transformation temperature
t g and crystallization temperature
t x be the characteristic parameter of characterizing metal thermal stability, its value shows that more greatly the anti-crystallization ability of amorphous sample is stronger, and thermostability is higher.Finally, the coercivity H of soft magnetic amorphous alloy and saturation magnetization Bs are measured by MATS-2010SD Hysteresis-graph and LakeShore-7407 type vibrating sample magnetometer respectively, all cryogenic vacuum anneal is carried out before sample test, annealing temperature is Tx-80K, soaking time is 5 ~ 15 minutes, to remove unrelieved stress wherein.
The invention has the beneficial effects as follows: (1) is compared with the soft magnetic amorphous material of traditional F e-B-Si system band, Fe-B-Si-Hf alloy of the present invention contains a small amount of Hf(0.5-5at.%), amorphous formation ability significantly improves, and can form bar-shaped block amorphous alloy, and its maximum critical size reaches 3 mm; (2) Fe-B-Si-Hf is the brand-new system forming block amorphous alloy, and its composition has high Fe content characteristics, and atom percentage content is more than 70at.%; Because the amorphous formation ability of alloy is large, the cooling rate scope thus preparing amorphous sample (comprising band) broadens, cause amorphous sample preparation process simple, and can avoid the sample fragility that the alloy amorphous Forming ability deficiency of traditional F e base causes; (3) new amorphous has excellent saturation induction density (the maximum saturation magnetic induction density of amorphous bulk sample is 1.65 T, the maximum saturation magnetic induction density of relevant band amorphous sample is 1.78 T) and low coercive force (coercive force of all amorphous is all lower than 2 A/m), can be used as new distribution transformer core and other power electronic component material.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described.
Fig. 1 is the X-ray diffraction spectrum of the typical AMORPHOUS ALLOY RIBBONS of Fe-B-Si-Hf system and rod-like samples.
Fig. 2 is the differential thermal analysis curve example of Fe-B-Si-Hf system AMORPHOUS ALLOY RIBBONS and rod-like samples.
Fig. 3 is Fe
72.5b
16.7si
8.3hf
2.5the magnetzation curve (measuring saturation magnetization Bs value) of amorphous ribbon.
Fig. 4 is Fe
72.5b
16.7si
8.3hf
2.5the magnetic hysteresis loop (measuring coercivity H value) of amorphous ribbon.
Embodiment
Here is the common prescription table of the soft magnetic amorphous material of Fe-B-Si-Hf system:
The following detailed description of the embodiment of the soft magnetic amorphous material of typical Fe-B-Si-Hf system in the present invention.Now with Fe
72.5b
16.7si
8.3hf
2.5, Fe
76.4b
14.3si
7.2hf
2.1, Fe
84.3b
9.5si
4.8hf
1.4three compositions are example, and the fabrication & properties test process that Fe-B-Si-Hf is soft magnetic amorphous is described.
embodiment 1fe
72.5b
16.7si
8.3hf
2.5soft magnetic amorphous alloy
Step one: component weighs and alloy pig melting
By Fe
72.5b
16.7si
8.3hf
2.5alloy (atomic percent) conversion is weight percentage composition:
Adopt technical purity constituent element, carry out weigh batching by the weight percent of alloy; Be placed in the water jacketed copper crucible of non-consumable arc-melting furnace by load weighted raw metal mixing, under high-purity argon gas protection, carry out melting, then spun upside down by alloy pig, melt back like this 3 times, obtains the alloy pig of uniform composition;
Step 2: the preparation of band and bar-shaped block sample
Put into silica tube by after alloy pig fragmentation, silica tube jet size diameter is about 1 ~ 1.5 mm.Silica tube after charging is placed in load coil; use vacuum copper roller to get rid of band technology, under high-purity argon gas protection, alloy test portion is melted and is ejected on water-cooled copper roller that linear velocity is 40 m/s; obtain alloy strip sample, typical sizes is: wide 2 mm × thick 30 μm.Meanwhile, also the alloy melt in silica tube can be blown and cast block sample and spray in the cylindrical water cooled copper mould die cavity of different size by alloy melt, be cooled to room temperature, obtain the block sample of diameter 1 ~ 3 mm; Or utilize water cooled copper mould suction casting method, directly alloy pig is melted by electric arc, then alloy melt is sucked in cylindrical water cooled copper mould die cavity, obtain bar-shaped block sample.
Step 3: the thermal analyses of contextual analysis of organization and amorphous sample and magnetism testing
Germany is utilized to produce Bruker D8 Focus X-ray diffractometer (Cu K
α radiation, λ=0.15406nm) and TecnaiG
220 type high-resolution-ration transmission electric-lens detect Fe
72.5b
16.7si
8.3hf
2.5the structure of alloy strip and rod-like samples and tissue, result shows Fe
72.5b
16.7si
8.3hf
2.5the bar-shaped block sample that band and diameter are no more than 2.5 mm is non-crystalline state single phase structure (with reference to accompanying drawing 1).As shown in Figure 2, via the Fe that DTA records
72.5b
16.7si
8.3hf
2.5the glass transformation temperature of amorphous
t g and crystallization temperature
t x be respectively 852K and 885K, supper cooled liquid region Δ
t x (=
t g -
t x ) width reaches 33 K.
By the amorphous ribbon that obtains and bar-shaped block sample 3 × 10
-3carry out anneal under Pa vacuum tightness, annealing temperature is 530 DEG C, is warming up to set annealing temperature and is incubated 5 minutes, cool to room temperature with the furnace subsequently with 150 DEG C/min; Then the annealing specimen after removal stress is placed on MATS-2010SD Hysteresis-graph and LakeShore-7407 type vibrating sample magnetometer and measures its magnetic property.Result shows Fe
72.5b
16.7si
8.3hf
2.5amorphous ribbon is substantially identical with the magnetic property of block sample, and their coercivity H and saturation magnetization Bs value are respectively 1.5 A/m and 1.56 T, as shown in accompanying drawing 3 and Fig. 4.
embodiment 2fe
76.4b
14.3si
7.2hf
2.1soft magnetic amorphous alloy
Step one: component weighs and alloy pig melting
With the step one in embodiment one.
Step 2: the preparation of band and bar-shaped block sample
With the step 2 in embodiment one.
Step 3: contextual analysis of organization and amorphous sample magnetism testing
With the step 3 in embodiment one.The annealing temperature of vacuum annealing process is here 450 DEG C, and soaking time is 5min.
Result shows Fe
76.4b
14.3si
7.2hf
2.1the bar-shaped block sample that band and diameter are no more than 1 mm can form single-phase amorphous microstructure (with reference to accompanying drawing 1); Fe is recorded via DTA
76.4b
14.3si
7.2hf
2.1the glass transformation temperature of band amorphous
t g and crystallization temperature
t x be respectively 824K and 847K, supper cooled liquid region Δ
t x width reaches 23 K.The Fe recorded
76.4b
14.3si
7.2hf
2.1the coercivity H of band amorphous and saturation magnetization Bs value are respectively 1.8 A/m and 1.63 T.
embodiment 3fe
84.3b
9.5si
4.8hf
1.4soft magnetic amorphous alloy
Step one: component weighs and alloy pig melting
With the step one in embodiment one.
Step 2: the preparation of band and bar-shaped block sample
With the step 2 in embodiment one.
Step 3: contextual analysis of organization and amorphous sample magnetism testing
With the step 3 in embodiment one.The annealing temperature of vacuum annealing process is here 400 DEG C, and soaking time is 5min.
Result shows: for Fe
84.3b
9.5si
4.8hf
1.4alloy, only Tape samples can form single-phase amorphous microstructure (with reference to accompanying drawing 1), and this one-tenth office can not form large amorphous bulk sample.
DTA records Fe
84.3b
9.5si
4.8hf
1.4the glass transformation temperature of band amorphous
t g and crystallization temperature
t x be respectively 800K and 815K, its supper cooled liquid region Δ
t x width is 15 K; Coercivity H and the saturation magnetization Bs value of this band amorphous are respectively 2.0 A/m and 1.78T.
In sum, Fe-B-Si-Hf amorphous soft magnet novel material provided by the invention, have that amorphous formation ability is large, saturation induction density is high and the feature such as low-coercivity, and compare traditional soft magnetic amorphous alloy, they also demonstrates obvious glass transition temp point
t g , wider supper cooled liquid region Δ
t x with good amorphous formation ability, these cause it to have the technical superioritys such as preparation easy, fragility is little, good moldability, are expected to be used as new distribution transformer fe core material, and have broad prospect of application in fields such as power electronic components.
Claims (2)
1. an iron base amorphous magnetically-soft alloy material, is characterized in that: the chemical constitution of this material is: Fe
100-x-y-zb
xsi
yhf
z, wherein x, y, z is atomic percent, 5.0%≤x≤20.0%, 3.0 %≤y≤13.0%, 0.5%≤z≤5.0%, and Fe atomic percent is higher than 70.0%.
2. the preparation method of a kind of iron base amorphous magnetically-soft alloy material according to right 1, is characterized in that, comprise the following steps:
(1) get the raw materials ready: according to the chemical constitution Fe of this material
100-x-y-zb
xsi
yhf
z, convert the atomic percent of Fe, B, Si, Hf to weight percent, then take each constituent element raw metal by weight percentage, stand-by; In chemical constitution, x, y, z is atomic percent, 5.0%≤x≤20.0%, 3.0 %≤y≤13.0%, 0.5%≤z≤5.0%, and Fe atomic percent is higher than 70.0%; Described raw metal purity is all not less than technical pure;
(2) melting of alloy pig: by each constituent element raw metal mixing weighed, put into the water jacketed copper crucible of non-consumable arc-melting furnace, carry out alloy melting, melt back three to four times under pure argon protection, obtain the alloy pig of uniform composition; Mass loss rate before and after alloy pig melting controls within 5/1000ths;
(3) sample preparation: alloy pig is prepared into Tape samples or block sample;
The preparation process of Tape samples: alloy pig is broken, put into the silica tube that nozzle is long 8mm × wide 1mm, single roller is used to get rid of band technology, by induction heating technique by the alloy material fusing in silica tube, and with high-purity argon gas, alloy melt is blown out, make it be ejected on the water-cooled copper roller of high speed rotating, make alloy strip sample; The linear resonance surface velocity of described water-cooled copper roller is 15 ~ 50m/s;
The preparation process of block sample: alloy pig be placed in silica tube induction melting and be incubated, opens in quenching temperature and blows casting device, allow alloy melt spray in cylindrical water cooled copper mould die cavity, be cooled to room temperature, obtain block sample; Or alloy pig is directly melted by electric arc, then suck under negative pressure in cylindrical water cooled copper mould die cavity, be cooled to room temperature and obtain block sample.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724886A (en) * | 2019-09-11 | 2020-01-24 | 中国石油集团川庆钻探工程有限公司长庆井下技术作业公司 | High-hardness iron-based amorphous alloy and preparation method thereof |
| CN115821174A (en) * | 2022-12-12 | 2023-03-21 | 广东电网有限责任公司 | Fe-Co-Zr-Mo-Ni-B bulk amorphous alloy with high glass forming capability and preparation method thereof |
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|---|---|---|---|---|
| US20050161122A1 (en) * | 2002-03-01 | 2005-07-28 | Japan Science And Technology Agency | Soft magnetic metallic glass alloy |
| CN1869276A (en) * | 2006-06-26 | 2006-11-29 | 大连理工大学 | Fe base block amorphous alloy based on Fe-B-Y cluster |
| CN102071370A (en) * | 2011-01-11 | 2011-05-25 | 大连理工大学 | High-anticorrosion Zr-Al-Ni-Nb block amorphous alloy |
-
2015
- 2015-06-09 CN CN201510312048.0A patent/CN104878327A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050161122A1 (en) * | 2002-03-01 | 2005-07-28 | Japan Science And Technology Agency | Soft magnetic metallic glass alloy |
| CN1869276A (en) * | 2006-06-26 | 2006-11-29 | 大连理工大学 | Fe base block amorphous alloy based on Fe-B-Y cluster |
| CN102071370A (en) * | 2011-01-11 | 2011-05-25 | 大连理工大学 | High-anticorrosion Zr-Al-Ni-Nb block amorphous alloy |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724886A (en) * | 2019-09-11 | 2020-01-24 | 中国石油集团川庆钻探工程有限公司长庆井下技术作业公司 | High-hardness iron-based amorphous alloy and preparation method thereof |
| CN115821174A (en) * | 2022-12-12 | 2023-03-21 | 广东电网有限责任公司 | Fe-Co-Zr-Mo-Ni-B bulk amorphous alloy with high glass forming capability and preparation method thereof |
| CN115821174B (en) * | 2022-12-12 | 2024-05-07 | 广东电网有限责任公司 | Fe-Co-Zr-Mo-Ni-B bulk amorphous alloy with high glass forming capability and preparation method thereof |
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