CN101705443A - Block Fe-based amorphous alloy with high Fe content and preparation method thereof - Google Patents
Block Fe-based amorphous alloy with high Fe content and preparation method thereof Download PDFInfo
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Abstract
Block Fe-based amorphous alloy with high Fe content and a preparation method thereof belong to the technical field of preparation of block Fe-based amorphous alloy. Chemical formula thereof is as follows: TM1(a)-TM2(b)-AM1(c)-AM2(d)-AM3(e)-AM4(f), wherein TM1 is Fe, TM2 is Mo, AM1 is P, AM2 is C, AM3 is B, and AM4 is Si. The preparation method comprises the following steps: smelting prepared materials into master alloy, burning to prepare a boron oxide coating agent; when the boron oxide coating agent is clear and has no air bubbles, arranging the master alloy therein; conducting purification repeatedly at the temperature higher than the melting point of the alloy by 50K to 250K until an alloy interface has no air bubbles and is stable; and placing the purified master alloy in an induction furnace so as to be melted, and then injecting or suction-casting the melted master alloy into a copper mould so as to be cooled, thus obtaining the block Fe-based amorphous alloy. The alloy has the characteristics of high formation capability, high strength, excellent soft magnetic property and the like.
Description
Technical field
The invention belongs to the block Fe-based amorphous alloy preparing technical field, particularly a kind ofly be mainly used in having high-strong toughness, soft magnetism and well forming the novel high Fe content iron-base amorphous alloy material of ability of soft magnetic materials, structured material and corrosion resistant material.
Background technology
Ferrous materials is because of its cheap price, rich in natural resources, characteristics widespread uses such as recyclable utilization and workability more than 3000 year.In recent years, along with development of science and technology, having novel structural performance and " hi-tech " material of functional performance concurrently becomes one of focus in the Materials science research day by day.By alloy composition is formed special amorphous structure from the non-crystaline amorphous metal of gaseous state or liquid rapid solidification preparation because of not having the long-range atomic ordered, the special mechanical properties that this amorphous structure has caused non-crystaline amorphous metal to have being different from the conventional crystal alloy, magnetic property, solidity to corrosion, electrical property etc. make non-crystaline amorphous metal become very important field in the investigation of materials.
After nineteen sixty-five it is found that the Fe-P-C Fe-based amorphous alloy has ferromegnetism, the ferromegnetism non-crystaline amorphous metal caused that people pay close attention to greatly, and the very fast Fe-based amorphous alloy of having found a series of (Fe-P), (Fe-C), (Fe-B) base.These non-crystaline amorphous metals and the nanometer crystal alloy material that obtains on its basis have remarkable soft magnetism, as high saturated magnetic induction, high magnetic permeability and low-coercivity, low-loss, also have characteristics such as high strength, high corrosion resistance simultaneously, therefore be considered to the most attractive a kind of Industrial Metal material.Countries such as Japan, the U.S., China have begun to adopt the core material of these material preparation strips as transformer etc., and simple because of its complete processing, loss is low, volume is little, the efficient advantages of higher obtains huge economic benefit and social benefit.But because the amorphous formation ability of these alloys is low, the preparation non-crystaline amorphous metal needs very high (10
6More than the K/s) rate of cooling, the thickness of the strip by the preparation of single-roller method or double roller therapy is usually less than 0.1mm.So the stacking factor by the transformer core of these strips preparation has only 75-85%, is starkly lower than 95% of the about 0.3mm siliconized plate of traditional thickness laminated core.Therefore, for promoting the further commercial applications of amorphous alloy material on devices such as transformer, press for the appearance of Fe-based amorphous alloy with high amorphous formation ability.
Since the nineties in last century, many material researchers are devoted to the research and development of block Fe-based amorphous alloy always, and Fe-(Al, Ga)-(P, C, B, Si), Fe-(Zr, Hf, Nb, Ta)-and B, Fe-(Cr, Mo)-successfully prepared a series of millimetre-sized block amorphous alloys in the alloy systems such as C-B-P.But, being accompanied by the raising that Fe-based amorphous alloy forms ability, the content of ferro element reduces because of interpolation, the replacement of other elements in the ferrous alloy.Iron content is far below commerce strip non-crystaline amorphous metal (80-81at%, atomic percent) in present most iron-base block amorphous alloy, and iron level is smaller or equal to 70at% usually.And, temporarily not between report develop iron-holder and be higher than～77% iron-base block amorphous alloy material.Because ferro element is the main ferromagnetic element in the Fe-based amorphous alloy, the reduction of iron content has a strong impact on the excellent magnetic energy and the mechanical property of Fe-based amorphous alloy.Therefore, one of the new iron-based block amorphous alloy material that exploitation has high Fe content, high-strong toughness, excellent soft magnetism, high amorphous formation ability is rich in challenge, while by the research work with huge magnetism, because this novel high Fe content iron-base block amorphous alloy material not only can be used as the fine structure material because of it has high-strong toughness, and can utilize its excellent soft magnetism and erosion resistance main raw as magnetic devices such as miniature transformers.Therefore development of new high Fe content Fe-based amorphous alloy will have boundless prospects for commercial application.
Summary of the invention
The present invention proposes a kind of iron-base block amorphous alloy material with high Fe content (iron level is greater than 77at%), high-strong toughness, excellent soft magnetism, high amorphous formation ability, this novel high Fe content iron-base block amorphous alloy material will can be used as magnetic materials such as fine structure material, miniature transformer.
The chemical expression of the block Fe-based amorphous alloy of high Fe content of the present invention is:
TM
1(a)-TM
2(b)-AM
1(c)-AM
2(d)-AM
3(e)-AM
4(f)
TM wherein
1=Fe; TM
2=Mo; AM
1=P; AM
2=C; AM
3=B; AM
4=Si;
A wherein, b, c, d, e, f are the atomic percent of each constituent element, span is respectively 78≤a≤81, b=1,7.5≤c≤9,5.5≤d≤6.5,2≤e≤3.5,2≤f≤3;
And 18≤c+d+e+f≤21, a+b+c+d+e+f=100.
The preparation method of the block Fe-based amorphous alloy of high Fe content of the present invention contains following steps:
1) prepares burden according to the alloying constituent proportioning;
2) in vacuum induction melting furnace, mother alloy is made in the raw material melt back;
3) with the boron oxide coating under vacuum condition, under the temperature of 1200K～1400K, be incubated, remove moisture;
4) limpid and when not having bubble when the boron oxide coating, under vacuum condition, above-mentioned mother alloy is placed the boron oxide coating; And under vacuum condition, be higher than under the temperature condition of alloy melting point 50K～250K and purifying, in purification process, allow alloy melt be cooled to and solidify and then the fusing purification that heats up, and repeat above-mentioned solidifying and melting process, alloy interface does not have the bubble generation when melting once more, and till the interface stability;
5) the good mother alloy of will purifying places the induction furnace of quick solidification apparatus to melt, and the fusing back is sprayed or inhaled and casts onto that cooling obtains described block Fe-based amorphous alloy in the copper mold.
In the described step 4), mother alloy is under vacuum condition, and the time of purifying in the boron oxide coating is more than 2 hours.
Experiment showed, that block iron non-crystaline amorphous metal that the present invention prepares has high formation ability, low melting temperature, high strength, plastic deformation ability preferably, therefore excellent characteristics such as soft magnetism have excellent mechanical property and soft magnetic performance simultaneously.
Description of drawings
Fig. 1 is Fe
78Mo
1P
9C
6.5B
3.5Si
2Non-crystaline amorphous metal bar surface topography photo and the X ray diffracting spectrum of 2mm diameter specimen;
Fig. 2 is Fe
78Mo
1P
9C
6.5B
3.5Si
2Alloy diameter 1mm non-crystaline amorphous metal sample stress under compression strain curve;
Fig. 3 is Fe
78Mo
1P
9C
6.5B
3.5Si
2The non-crystaline amorphous metal magnetic hysteresis loop;
Fig. 4 is Fe
80Mo
1P
8C
6B
2Si
3Non-crystaline amorphous metal bar and purification stepmother alloy surface pattern photo, with and the X-ray diffractogram of bar sample;
Fig. 5 is Fe
80Mo
1P
8C
6B
2Si
3The non-crystaline amorphous metal thermal analysis curve;
Fig. 6 is Fe
80Mo
1P
8C
6B
2Si
3The non-crystaline amorphous metal magnetic hysteresis loop;
Fig. 7 is Fe
81Mo
1P
7.5C
5.5B
2Si
3Non-crystaline amorphous metal bar and purification stepmother alloy surface pattern photo, with and the X-ray diffractogram of bar sample;
Fig. 8 is Fe
81Mo
1P
7.5C
5.5B
2Si
3The non-crystaline amorphous metal magnetic hysteresis loop.
Embodiment
The present invention is a kind of iron-base block amorphous alloy material with plasticity and soft magnetism, and the constitutional chemistry expression formula of described Fe-based amorphous alloy is as follows:
TM
1(a)-TM
2(b)-AM
1(c)-AM
2(d)-AM
3(e)-AM
4(f)
TM
1＝Fe；
TM
2＝Mo；
AM
1＝P；
AM
2＝C；
AM
3＝B；
AM
4＝Si；
A wherein, b, c, d, e, f are the atomic percent (at%) of each constituent element, its span is respectively 78≤a≤81, b=1,7.5≤c≤9,5.5≤d≤6.5,2≤e≤3.5,2≤f≤3;
And 18≤c+d+e+f≤21, a+b+c+d+e+f=100.
Preparation method of the present invention is that Fe-P prealloy and other raw materials that will prepare in proportion earlier place the vacuum induction melting furnace smelting nut alloy.Then mother alloy is placed burned boron oxide coating, under vacuum condition, be higher than purify under the temperature condition of the about 50 ~ 245K of its fusing point about more than 2 hours.Allow alloy melt be cooled in purification process and solidify, purify in the fusing that heats up then, and repeat above-mentioned solidifying-melting process, alloy interface does not have till bubble generation, the interface stability when melting once more.Place the induction furnace of quick solidification apparatus to melt the mother alloy after purifying, by the copper mold castmethod, employing injection or suction casting mode are cast into the mode in the copper mold, directly obtain the amorphous alloy block specimen material; The also available band method of getting rid of prepares amorphous alloy ribbon.
The block iron non-crystaline amorphous metal for preparing has high formation ability.In the zone of alloy composition composition, it can be prepared the non-crystaline amorphous metal bar more than the 1mm, regional area can obtain the non-crystaline amorphous metal bar of 2mm.In addition, this Fe-based amorphous alloy for preparing has high iron level (78-81at%), low temperature of fusion (1190K-1250K), and high intensity (breaking tenacity is greater than 2500MPa), and show tangible viscous deformation (deflection 0.5-6%).This Fe-based amorphous alloy also has excellent soft magnetism simultaneously, shows high saturation induction density (153～166emu/g) and low-down coercive force (Hci is less than 10A/m).Therefore, the novel high Fe content Fe-based amorphous alloy of the present invention's proposition has very strong prospects for commercial application because of having excellent mechanical property and soft magnetic performance simultaneously.
Below in conjunction with embodiment the specific embodiment of the present invention is described.
Embodiment 1: preparation Fe
78Mo
1P
9C
6.5B
3.5Si
2The non-crystaline amorphous metal bar
At first prepare burden according to the chemical ingredients proportioning, mother alloy is made in melt back in vacuum induction melting furnace then.The boron oxide coating under the vacuum condition, be incubated under the condition of about 1230K, is removed moisture.Limpid and when not having bubble when the boron oxide coating, can under vacuum condition, mother alloy be placed the boron oxide coating, under vacuum condition, be higher than purify under the temperature condition of the about 80～200K of alloy melting point about more than 2 hours.Allow alloy melt be cooled in purification process and solidify, purify in the fusing that heats up then, and repeat above-mentioned solidifying-melting process, alloy interface does not have till bubble generation, the interface stability when melting once more.Place the induction furnace of quick solidification apparatus to make its fusing the mother alloy well of purifying, the fusing back is sprayed or is inhaled to cast onto to cool off in the copper mold and obtains the amorphous alloy rod, tests its thermodynamic stability.
Fig. 1 is Fe for composition among the embodiment
78Mo
1P
9C
6.5B
3.5Si
2Ferrous alloy be the bar outside surface pattern photo of 1.5mm and 2mm by the diameter that the copper mold casting process obtains, and the 2mm sample X ray diffracting spectrum shown in the illustration.Can see to cast specimen surface smooth finish very high, and the X ray collection of illustrative plates only has the diffuse scattering peak of a steamed bun shape, shows its complete non-crystal structure.Its THERMAL STABILITY is the result show, this non-crystaline amorphous metal has lower glass transformation temperature (718K) and temperature of fusion is 1190K, and has good thermodynamic stability, and stable supercooled liquid interval is 18K.
Carry out Mechanics Performance Testing to implementing the non-crystaline amorphous metal sample, the stress-strain(ed) curve in its compression process as shown in Figure 2.This non-crystaline amorphous metal has high breaking tenacity (about 3140MPa) as can be seen, also shows tangible viscous deformation (deflection about 6%) simultaneously, is more satisfactory fine structure material.
Carry out hardness test to implementing the non-crystaline amorphous metal sample, be about 900Kg/mm
2In addition, it is carried out the magnetic test, its magnetic hysteresis loop as shown in Figure 3.This non-crystaline amorphous metal has lower coercive force and higher magnetic permeability as can be seen, and (the about 153emu/g of specific magnetization, saturation induction density～1.45T) are very excellent soft magnetic performance materials to show higher saturation induction density simultaneously.
Embodiment 2: preparation Fe
80Mo
1P
8C
6B
2Si
3The non-crystaline amorphous metal bar
At first prepare burden according to the chemical ingredients proportioning, mother alloy is made in melt back in vacuum induction melting furnace then.With the boron oxide coating under vacuum condition, about 1300K insulation, remove moisture.Limpid and when not having bubble when the boron oxide coating, the boron oxide coating that can under vacuum condition, mother alloy be placed, under vacuum condition, be higher than purify under the temperature condition of the about 100～200K of alloy melting point about more than 2 hours.Allow alloy melt be cooled in purification process and solidify, purify in the fusing that heats up then, and repeat above-mentioned solidifying-melting process, alloy interface does not have till bubble generation, the interface stability when melting once more.Place the induction furnace of quick solidification apparatus to make its fusing the mother alloy well of purifying, the fusing back is sprayed or is inhaled to cast onto to cool off in the copper mold and obtains the amorphous alloy rod, tests its thermodynamic stability.
Fig. 4 is Fe for composition among the embodiment
80Mo
1P
8C
6B
2Si
3The diameter of ferrous alloy by the acquisition of copper mold casting process be outside surface pattern photo after the bar of 1mm and mother alloy thereof are purified, be 1mm sample X ray diffracting spectrum shown in the illustration.Can see to cast specimen surface smooth finish very high, and the X ray collection of illustrative plates only has the diffuse scattering peak of a steamed bun shape, shows its complete non-crystal structure.Fig. 5 is that composition is Fe
80Mo
1P
8C
6B
2Si
3The thermal analysis curve of Fe-based amorphous alloy, comprise the heating curve of heat-processed and the temperature lowering curve of fusing postcooling process.The result shows to its THERMAL STABILITY, though this non-crystaline amorphous metal does not have tangible glass transition phenomenon, have tangible crystallization process, and its temperature of fusion is lower, is 1219K, has good thermodynamic stability.
Carry out hardness test to implementing the non-crystaline amorphous metal sample, find that this value far above the ordinary steel iron material, is about 780Kg/mm
2In addition it is carried out the magnetic test, its magnetic hysteresis loop as shown in Figure 6.This non-crystaline amorphous metal has lower coercive force and higher magnetic permeability as can be seen, shows higher saturation induction density (the about 166emu/g of specific magnetization, the about 1.63T of saturation induction density) simultaneously, is very excellent soft magnetic performance material.
Embodiment 3: preparation Fe
81Mo
1P
7.5C
5.5B
2Si
3The non-crystaline amorphous metal bar
At first prepare burden according to the chemical ingredients proportioning, mother alloy is made in melt back in vacuum induction melting furnace then.With the boron oxide coating under vacuum condition, about 1450K insulation, remove moisture.Limpid and when not having bubble when the boron oxide coating, as can to place at Jiang's mother alloy under vacuum condition boron oxide coating, under vacuum condition, be higher than purify under the temperature condition of the about 150～230K of alloy melting point about more than 2 hours.Allow alloy melt be cooled in purification process and solidify, purify in the fusing that heats up then, and repeat above-mentioned solidifying-melting process, alloy interface does not have till bubble generation, the interface stability when melting once more.Place the induction furnace of quick solidification apparatus to make its fusing the mother alloy well of purifying, the fusing back is sprayed or is inhaled to cast onto to cool off in the copper mold and obtains the amorphous alloy rod, tests its thermodynamic stability.
Fig. 7 is Fe for composition among the embodiment
81Mo
1P
7.5C
5.5B
2Si
3The diameter of ferrous alloy by the acquisition of copper mold casting process be outside surface pattern photo after the bar of 1mm and mother alloy thereof are purified, be 1mm sample X ray diffracting spectrum shown in the illustration.As seen purify the back mother alloy and to cast specimen surface smooth finish very high, and the X ray collection of illustrative plates also only has the diffuse scattering peak of a steamed bun shape, shows its complete non-crystal structure.Its THERMAL STABILITY is the result show, this non-crystaline amorphous metal temperature of fusion is 1250K, and do not have tangible supercooled liquid interval.
Carry out hardness test to implementing the non-crystaline amorphous metal sample, be about 760Kg/mm
2In addition, it is carried out the magnetic test, the magnetic test, its magnetic hysteresis loop is as shown in Figure 8.This non-crystaline amorphous metal has lower coercive force and higher magnetic permeability as can be seen, shows higher saturation induction density (the about 167emu/g of specific magnetization, the about 1.64T of saturation induction density) simultaneously, is very excellent soft magnetic performance material.
Claims (3)
1. the block Fe-based amorphous alloy of a high Fe content is characterized in that, its chemical expression is:
TM
1(a)-TM
2(b)-AM
1(c)-AM
2(d)-AM
3(e)-AM
4(f)
TM wherein
1=Fe; TM
2=Mo; AM
1=P; AM
2=C; AM
3=B; AM
4=Si;
A wherein, b, c, d, e, f are the atomic percent of each constituent element, span is respectively 78≤a≤81, b=1,7.5≤c≤9,5.5≤d≤6.5,2≤e≤3.5,2≤f≤3;
And 18≤c+d+e+f≤21, a+b+c+d+e+f=100.
2. the preparation method of block Fe-based amorphous alloy as claimed in claim 1 is characterized in that, contains following steps:
1) prepares burden according to the alloying constituent proportioning;
2) in vacuum induction melting furnace, mother alloy is made in the raw material melt back;
3) with the boron oxide coating under vacuum condition, under the temperature of 1200K～1400K, be incubated, remove moisture;
4) limpid and when not having bubble when the boron oxide coating, under vacuum condition, above-mentioned mother alloy is placed the boron oxide coating; And under vacuum condition, be higher than under the temperature condition of alloy melting point 50K～250K and purifying, in purification process, allow alloy melt be cooled to and solidify and then the fusing purification that heats up, and repeat above-mentioned solidifying and melting process, alloy interface does not have the bubble generation when melting once more, and till the interface stability;
5) the good mother alloy of will purifying places the induction furnace of quick solidification apparatus to melt, and the fusing back is sprayed or inhaled and casts onto that cooling obtains described block Fe-based amorphous alloy in the copper mold.
3. the preparation method of block Fe-based amorphous alloy as claimed in claim 2 is characterized in that, in the described step 4), mother alloy is under vacuum condition, and the time of purifying in the boron oxide coating is more than 2 hours.
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| CN103320723A (en) * | 2013-05-28 | 2013-09-25 | 江苏迈盛新材料有限公司 | Repeated fusion-solidification treating method for raising alloy amorphous forming ability |
| CN103484747A (en) * | 2013-05-28 | 2014-01-01 | 江苏迈盛新材料有限公司 | Method for preparing iron-based amorphous alloy with supersoft ferromagnetic property |
| CN103882347A (en) * | 2014-03-05 | 2014-06-25 | 清华大学 | Blocky and stripped ferrum-based amorphous alloy with high magnetic element content, and preparation method |
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| TWI532855B (en) | 2015-12-03 | 2016-05-11 | 財團法人工業技術研究院 | Iron-based alloy coating and method for manufacturing the same |
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| CN100476009C (en) * | 2005-09-13 | 2009-04-08 | 北京航空航天大学 | High strength and high toughness nanometer Fe-base amorphous alloy composite material |
| CN101589169B (en) * | 2007-02-28 | 2011-08-03 | 新日本制铁株式会社 | Fe-based amorphous alloy having excellent soft magnetic characteristics |
| CN100457955C (en) * | 2007-04-16 | 2009-02-04 | 安泰科技股份有限公司 | Ferrum-base block non-crystalline alloy material |
| CN100529146C (en) * | 2007-11-15 | 2009-08-19 | 北京航空航天大学 | Iron-base amorphous alloy material with high saturation magnetic induction density |
| CN101206943B (en) * | 2007-11-16 | 2011-02-02 | 北京航空航天大学 | Iron base amorphous magnetically-soft alloy having high saturated magnetic induction and excellent toughness |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103320723A (en) * | 2013-05-28 | 2013-09-25 | 江苏迈盛新材料有限公司 | Repeated fusion-solidification treating method for raising alloy amorphous forming ability |
| CN103484747A (en) * | 2013-05-28 | 2014-01-01 | 江苏迈盛新材料有限公司 | Method for preparing iron-based amorphous alloy with supersoft ferromagnetic property |
| CN103882347A (en) * | 2014-03-05 | 2014-06-25 | 清华大学 | Blocky and stripped ferrum-based amorphous alloy with high magnetic element content, and preparation method |
| CN103882347B (en) * | 2014-03-05 | 2016-11-16 | 清华大学 | The block of high magnetic element content and ribbon Fe-based amorphous alloy and preparation method |
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