CN104046930A - Preparation method of Al based amorphous alloy, and amorphous strip and nanocrystalline powder thereof - Google Patents
Preparation method of Al based amorphous alloy, and amorphous strip and nanocrystalline powder thereof Download PDFInfo
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- CN104046930A CN104046930A CN201410224850.XA CN201410224850A CN104046930A CN 104046930 A CN104046930 A CN 104046930A CN 201410224850 A CN201410224850 A CN 201410224850A CN 104046930 A CN104046930 A CN 104046930A
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Abstract
The invention discloses a preparation method of Al based amorphous alloy, and an amorphous strip and a nanocrystalline powder thereof. The method is as below: selecting an Al-Ni-Y Al based amorphous system with strong amorphous formation capacity as a foundation, and adding elements conducive to amorphous alloy formation in the Al-Ni-Y in Al based amorphous system, such as 5-9% of Ni, 1-5% of Y, 0-2% of La, 0-2% of Fe, 4-6% of B, 1-5% of Zr and the balance of Al; after ingredient preparation in accordance with the nominal composition, smelting mother alloy under argon protection by vacuum arc with vacuum degree of 5*10<-3> Pa; then preparing the amorphous strip under argon protection by a single roller melt spinning machine, wherein the maximum line speed of melt spinning is 40m / s, and the vacuum degree is 2*10<-3> Pa. The components of the alloy have good amorphous formation ability, and the preparation method is simple. At the same time, an Al79Ni7Y5Fe2B4Zr3 (atomic percent) Al based amorphous system with the best amorphous formation ability is selected to prepare the Al based amorphous nanocrystalline alloy powder in a gas atomization way.
Description
Technical field
The invention belongs to metal material field, relate to a kind of preparation method with al based amorphous alloy and amorphous ribbon and the manocrystalline powders of stronger amorphous formation ability.
Background technology
Al based amorphous alloy tool high strength, low density, high thermal stability, good mechanical property, and the feature such as excellent anticorrosive performance, enjoy investigation of materials person to pay close attention to.But, the amorphous formation ability of aluminium-based amorphous alloy a little less than.The overall dimension of aluminium-based amorphous alloy is at present, [W.S.Sanders[W.S.Sanders, J.S.Warner, D.B.Miracle.StabilityofAl-richglassesinthe Al-La-Nisystem.Intermetallics, 2006, 14:349] etc. utilize wedge-shaped die successfully to prepare maximum critical thickness to reach 780 μ m aluminium-based amorphous alloy, B.J.Yang[B.J.Yang, J.H.Yao, J.Zhang, H.W.Yang, J.Q.Wang, E.Ma.Al-richbulkmetallic glasseswithplasticityandultrahigh.ScriptaMaterialia, 2009, 61:423-426.] etc. people prepared the aluminium-based amorphous alloy pole that diameter is 1mm.While Chinese patent 200310118908.4, al based amorphous alloy and preparation method thereof, disclosing composition is Ni8-10%, Zr3-7%, Cu1-5%, Y1-3%, all the other are the Al-based Amorphous Alloys of Al (atomic percent).Arc melting mother alloy in protection of inert gas atmosphere gets rid of band after melting in atmospheric environment and vacuum environment, and getting rid of band linear velocity is 23m/s, has prepared al based amorphous alloy.Chinese patent 201010195974.1, a kind of Al-Ni-Ce-La aluminum-based amorphous alloy and preparation method thereof, disclosing composition atomic percent is Al
84ni
10ce
(6-x)la
x(x=1-6, at%), Al
84ni
(10-y)ce
6la
y(y=1-3, at%) and Al
(84-z)ni
10ce
6la
zthe Al-based Amorphous Alloys of (z=1-3, at%).Under argon shield, through vacuum arc melting or vacuum induction melting, prepare mother alloy, get rid of band and prepare amorphous ribbon under argon shield, minimum line speed is 10m/s, has prepared al based amorphous alloy.Chinese patent 03111739.2, a kind of al based amorphous alloy and preparation method thereof, having announced composition atomic percent is Ni8-12%, (mass percent of mishmetal composition is mishmetal 4-6%: La35%, Ce50%, Pr5% and Nd10%), aluminium is surplus.By getting rid of band under argon shield, obtain the amorphous ribbon that thickness is 140 μ m, prepared al based amorphous alloy.These have all widened the composition of aluminium-based amorphous alloy above, significant to the development of aluminium-based amorphous alloy.But these will be applied to produce actual is far from being enough, so how to obtain the strong and high aluminium-based amorphous alloy of thermal stability of amorphous formation ability, be still problem demanding prompt solution.
Summary of the invention
The object of the invention is to be added with the element that is beneficial to formation amorphous in Al-Ni-Y aluminium-based amorphous alloy system, a kind of Alloy And Preparation Method with stronger amorphous formation ability is provided.Especially utilize the mode of aerosolization to prepare amorphous nano-crystalline powder, to improve the performance of power applications in hot spray coating.
The invention provides a kind of al based amorphous alloy, by adding and be beneficial to the element that forms non-crystaline amorphous metal in Al-Ni-Y aluminium-based amorphous alloy system, its concrete composition is Ni5-9%, Y1-5%, and La0-2%, Fe0-2%, B4-6%, Zr1-5%, surplus is Al.Comprise the following steps:
The outfit of raw material: the purity of desired raw material simple substance is all greater than 99%, prepares burden according to nominal composition.
The melting of mother alloy: after starting material are put in crucible, working chamber's vacuum tightness is 5 * 10
-3pa, before master alloy melting, first melting Ti ingot is with the oxygen in absorption furnace and other impurity, to be further purified melting atmosphere.Even for melting, all mother alloy meltings are more than 4 times.
Get rid of band and prepare amorphous ribbon: the surface scale of the alloy block that melting is obtained polishes off with sharpening machine, after being cut into small pieces, puts into silica tube, under argon shield, with single roller, get rid of the standby amorphous ribbon of band mechanism, the maximum line velocity that gets rid of band is 40m/s.
The preparation of manocrystalline powders comprises the following steps:
(1) outfit of raw material: the purity of desired raw material simple substance is all greater than 99%, prepares burden according to nominal composition, is positioned in the inductive crucible of gas-atomized powder equipment;
(2) vacuum melting: vacuumize and be filled with argon shield, melting to alloy solution is slowly at the uniform velocity poured in insulation bag under induction heating, is filled with high pressure argon gas as atomizing medium simultaneously;
(3) argon gas atomization: alloy solution flows under the impact of high pressure argon gas stream, is atomized into small droplets, final cooling formation amorphous powdered alloy; Processing parameter is: melting vacuum tightness is less than 1Pa, smelting temperature 1200-1400 ℃, and atomizing pressure 20-45 kilogram, atomizing medium is argon gas;
(4) powder sieving: amorphous powdered alloy is collected and sieved, filter out 400-500 object powdered alloy.
Al based amorphous alloy of the present invention has the following advantages:
1. to propose a kind of Al-Ni-Y be hexa-atomic al based amorphous alloy in the present invention, by adding large size atom L
aand Y, make supercooled liquid there is finer and close atom stacking provisions, make the diffusion of atom long-range become difficult, thereby suppress the forming core of crystalline state phase.Amorphous ribbon has stronger amorphous formation ability.
2. except Y element, other simple substance alloy low prices, have reduced the cost of alloy.Preparation and working method are simple.
3. the present invention has prepared a kind of amorphous nano-crystalline powder.
Accompanying drawing explanation
Accompanying drawing 1 is alloy A l
83ni
5y
5la
1fe
1b
4zr
1(1), alloy A l
79ni
9y
3la
0fe
2b
4zr
3(2), alloy A l
79ni
7y
5la
0fe
2b
4zr
3(3), alloy A l
78ni
9y
5la
0fe
2b
5z
r1and alloy A l (4)
76ni
9y
3la
2fe
1b
4zr
5(5) under on-line velocity 40m/s, get rid of the X-ray diffractogram of band
Accompanying drawing 2 is Al
79ni
7y
5la
0fe
2b
4zr
3the X-ray diffractogram of 500 order aluminium-based amorphous alloy nanometer crystal alloy powder of composition
Accompanying drawing 3 is Al
79ni
7y
5la
0fe
2b
4zr
3the SEM surface topography of 500 order aluminium-based amorphous alloy nanometer crystal alloy powder of composition
Accompanying drawing 4 is Al
79ni
7y
5la
0fe
2b
4zr
3the microzone electron diffraction figure of 500 order aluminium-based amorphous alloy nanometer crystal alloy powder of composition
1 XRD interpretation of result with reference to the accompanying drawings, the non-crystaline amorphous metal of these 5 kinds of alloying constituents prepared by the present invention is most of for non-crystal structure, has stronger amorphous formation ability.Having part precipitated phase, is ZrB through demarcating major part
2phase, Al
3zr
5phase and Ni
4b
3phase.
2 XRD interpretation of result with reference to the accompanying drawings, 500 object aluminium-based amorphous alloy nanometer crystal alloy powder amorphous components prepared by the present invention are more, and amorphous formation ability is stronger.
3 SEM surface topography with reference to the accompanying drawings, 500 object aluminium-based amorphous alloy nanometer crystal alloy powder prepared by the present invention be spherical, subsphaeroidal or class spherical, smooth surface.
4 is the microzone electron diffraction figure of 500 order aluminium-based amorphous alloy nanometer crystal alloy powder with reference to the accompanying drawings, can obviously find out, powder diffraction pattern feature is that center has a center spot of dispersing and disperses ring, this diffraction spot of dispersing is amorphous characteristic feature, illustrates and in powder, contains amorphous substance.And the surrounding at center mottle also exists a little bright spot, and these are all diffraction spots, illustrate and in powder, contain Crystallization Phases material.
By Scherrer formula (debye-Scherrer formula), calculate the size of Crystallization Phases, suc as formula D=K λ/Bcos θ.In formula, K is Scherrer Changshu, and its value is 0.89; D is grain-size (nm); B is integration halfwidth degree, in the process of calculating, need be converted into radian (rad); θ is diffraction angle; λ is X ray wavelength, is 0.154056nm, calculates the grain-size of single diffraction peak representative.The XRD figure spectrum of 500 each powder of order, each mean sizes of calculating is 37.794nm.From data, can find out, Crystallization Phases is nano particle.
Embodiment
The invention provides a kind of al based amorphous alloy, by adding and be beneficial to the element that forms non-crystaline amorphous metal in Al-Ni-Y aluminium-based amorphous alloy system, its concrete composition is Ni5-9%, Y1-5%, and La0-2%, Fe0-2%, B4-6%, Zr1-5%, surplus is Al.Choose the composition Al that content of amorphous is the highest
79ni
7y
5la
0fe
2b
4zr
3(atomic percent), aerosolization is prepared amorphous nano-crystalline powder and is mainly chosen 400-500 object powder, and below in conjunction with representative instance, the present invention will be described.
Embodiment 1: prepared composition is Al
83ni
5y
5la
1fe
1b
4zr
1the amorphous alloy of composition
The outfit of raw material: the purity of desired raw material simple substance is all greater than 99%, prepares burden according to nominal composition.
The melting of mother alloy: after starting material are put in crucible, working chamber's vacuum tightness is 5 * 10
-3pa, before master alloy melting, first melting Ti ingot is with the oxygen in absorption furnace and other impurity, to be further purified melting atmosphere.Even for melting, all mother alloy meltings are more than 4 times.
Get rid of band and prepare amorphous ribbon: the surface scale of the alloy block that melting is obtained polishes off with sharpening machine, after being cut into small pieces, puts into silica tube, under argon shield, with single roller, get rid of the standby amorphous ribbon of band mechanism, the maximum line velocity that gets rid of band is 40m/s.
By getting rid of the band obtaining after band, with X-ray diffractometer, detect, thickness is 60 μ m.
Embodiment 2: prepared composition is Al
79ni
9y
3la
0fe
2b
4zr
3the amorphous alloy of composition
The outfit of raw material: the purity of desired raw material simple substance is all greater than 99%, prepares burden according to nominal composition.
The melting of mother alloy: after starting material are put in crucible, working chamber's vacuum tightness is 5 * 10
-3pa, before master alloy melting, first melting Ti ingot is with the oxygen in absorption furnace and other impurity, to be further purified melting atmosphere.Even for melting, all mother alloy meltings are more than 4 times.
Get rid of band and prepare amorphous ribbon: the surface scale of the alloy block that melting is obtained polishes off with sharpening machine, after being cut into small pieces, puts into silica tube, under argon shield, with single roller, get rid of the standby amorphous ribbon of band mechanism, the maximum line velocity that gets rid of band is 40m/s.
By getting rid of the band obtaining after band, with X-ray diffractometer, detect, thickness is 50 μ m.
Embodiment 3: prepared composition is Al
79ni
7y
5la
0fe
2b
4zr
3the amorphous alloy of composition
The outfit of raw material: the purity of desired raw material simple substance is all greater than 99%, prepares burden according to nominal composition.
The melting of mother alloy: after starting material are put in crucible, working chamber's vacuum tightness is 5 * 10
-3pa, before master alloy melting, first melting Ti ingot is with the oxygen in absorption furnace and other impurity, to be further purified melting atmosphere.Even for melting, all mother alloy meltings are more than 4 times.
Get rid of band and prepare amorphous ribbon: the surface scale of the alloy block that melting is obtained polishes off with sharpening machine, after being cut into small pieces, puts into silica tube, under argon shield, with single roller, get rid of the standby amorphous ribbon of band mechanism, the maximum line velocity that gets rid of band is 40m/s.
By getting rid of the band obtaining after band, with X-ray diffractometer, detect, thickness is 35 μ m.
Embodiment 4: prepared composition is Al
78ni
9y
5la
0fe
2b
5zr
1the amorphous alloy of composition
The outfit of raw material: the purity of desired raw material simple substance is all greater than 99%, prepares burden according to nominal composition.
The melting of mother alloy: after starting material are put in crucible, working chamber's vacuum tightness is 5 * 10
-3pa, before master alloy melting, first melting Ti ingot is with the oxygen in absorption furnace and other impurity, to be further purified melting atmosphere.Even for melting, all mother alloy meltings are more than 4 times.
Get rid of band and prepare amorphous ribbon: the surface scale of the alloy block that melting is obtained polishes off with sharpening machine, after being cut into small pieces, puts into silica tube, under argon shield, with single roller, get rid of the standby amorphous ribbon of band mechanism, the maximum line velocity that gets rid of band is 40m/s.
By getting rid of the band obtaining after band, with X-ray diffractometer, detect, thickness is 105 μ m.
Embodiment 5: prepared composition is Al
76ni
9y
3la
2fe
1b
4zr
5the amorphous alloy of composition
The outfit of raw material: the purity of desired raw material simple substance is all greater than 99%, prepares burden according to nominal composition.
The melting of mother alloy: after starting material are put in crucible, working chamber's vacuum tightness is 5 * 10
-3pa, before master alloy melting, first melting Ti ingot is with the oxygen in absorption furnace and other impurity, to be further purified melting atmosphere.Even for melting, all mother alloy meltings are more than 4 times.
Get rid of band and prepare amorphous ribbon: the surface scale of the alloy block that melting is obtained polishes off with sharpening machine, after being cut into small pieces, puts into silica tube, under argon shield, with single roller, get rid of the standby amorphous ribbon of band mechanism, the maximum line velocity that gets rid of band is 40m/s.
By getting rid of the band obtaining after band, with X-ray diffractometer, detect, thickness is 90 μ m.
Embodiment 6: prepared composition is Al
79ni
7y
5la
0fe
2b
4zr
3the 500 order amorphous nano-crystalline powdered alloys of (atomic percent)
Composition proportion: the purity of desired raw material simple substance all, more than 99%, is prepared burden according to nominal composition, is positioned in the inductive crucible of gas-atomized powder equipment.
Vacuum melting: vacuumize and be filled with argon shield, melting to alloy solution is slowly at the uniform velocity poured in insulation bag under induction heating, is filled with high pressure argon gas as atomizing medium simultaneously.
Argon gas atomization: alloy solution flows under the impact of high pressure argon gas stream, is atomized into small droplets, final cooling formation amorphous nano-crystalline powdered alloy.
Powder sieving: amorphous nano-crystalline powdered alloy is collected and sieved.
Filter out 500 object powdered alloys.Processing parameter is that melting vacuum tightness is less than 1Pa, smelting temperature 1200-1400 ℃, and atomizing medium is argon gas.
Claims (3)
1. an al based amorphous alloy, is characterized in that adding in Al-Ni-Y aluminium-based amorphous alloy system being beneficial to the element that forms non-crystaline amorphous metal, and concrete composition is Ni5-9%, Y1-5%, and La0-2%, Fe0-2%, B4-6%, Zr1-5%, surplus is Al.
2. prepare the method for al based amorphous alloy band as claimed in claim 1, it is characterized in that comprising the following steps:
(1) outfit of raw material: the purity of desired raw material simple substance is all greater than 99%, prepares burden according to nominal composition;
(2) melting of mother alloy: after starting material are put in crucible, working chamber's vacuum tightness is 5 * 10
-3pa, before master alloy melting, first melting Ti ingot is with the oxygen in absorption furnace and other impurity, and to be further purified melting atmosphere, even for melting, all mother alloy meltings are more than 4 times;
(3) get rid of band and prepare amorphous ribbon: the surface scale of the alloy block that melting is obtained polishes off with sharpening machine, after being cut into small pieces, puts into silica tube, under argon shield, with single roller, get rid of the standby amorphous ribbon of band mechanism, the maximum line velocity that gets rid of band is 40m/s.
3. prepare the method for al based amorphous alloy powder as claimed in claim 1, it is characterized in that comprising the following steps:
(1) outfit of raw material: the purity of desired raw material simple substance is all greater than 99%, prepares burden according to nominal composition, is positioned in the inductive crucible of gas-atomized powder equipment;
(2) vacuum melting: vacuumize and be filled with argon shield, melting to alloy solution is slowly at the uniform velocity poured in insulation bag under induction heating, is filled with high pressure argon gas as atomizing medium simultaneously;
(3) argon gas atomization: alloy solution flows under the impact of high pressure argon gas stream, is atomized into small droplets, final cooling formation amorphous powdered alloy; Processing parameter is: melting vacuum tightness is less than 1Pa, smelting temperature 1200-1400 ℃, and atomizing pressure 20-45 kilogram, atomizing medium is argon gas;
(4) powder sieving: amorphous powdered alloy is collected and sieved, filter out 400-500 object powdered alloy.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106011695A (en) * | 2016-07-29 | 2016-10-12 | 中国科学院合肥物质科学研究院 | Al-base amorphous alloy block material and preparation method thereof |
| CN108130441A (en) * | 2017-05-19 | 2018-06-08 | 吉林大学 | A kind of adding technology that refining aluminum alloy is bred using non-crystaline amorphous metal |
| CN108866394A (en) * | 2018-07-20 | 2018-11-23 | 中国科学院金属研究所 | A kind of high-temperature oxidation resistant corrosion resistant coating alloy and coating |
| CN117840422A (en) * | 2024-03-08 | 2024-04-09 | 朗峰新材料启东有限公司 | Manganese-based amorphous nanocrystalline composite powder and preparation method thereof |
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| CN1566394A (en) * | 2003-06-25 | 2005-01-19 | 中国科学院金属研究所 | Polycomponent amorphous alloy with equal atomic ratio feature |
| CN101338391A (en) * | 2008-08-11 | 2009-01-07 | 北京航空航天大学 | Quick setting block aluminum alloy with high strength and high ductibility and toughness and method for preparing same |
| CN102632232A (en) * | 2012-03-30 | 2012-08-15 | 济南大学 | Aluminium base amorphous composite powder as well as preparation method and application thereof |
| CN102719769A (en) * | 2012-06-20 | 2012-10-10 | 北京科技大学 | High-strength aluminum-based bulk amorphous composite material |
-
2014
- 2014-05-26 CN CN201410224850.XA patent/CN104046930A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1566394A (en) * | 2003-06-25 | 2005-01-19 | 中国科学院金属研究所 | Polycomponent amorphous alloy with equal atomic ratio feature |
| CN101338391A (en) * | 2008-08-11 | 2009-01-07 | 北京航空航天大学 | Quick setting block aluminum alloy with high strength and high ductibility and toughness and method for preparing same |
| CN102632232A (en) * | 2012-03-30 | 2012-08-15 | 济南大学 | Aluminium base amorphous composite powder as well as preparation method and application thereof |
| CN102719769A (en) * | 2012-06-20 | 2012-10-10 | 北京科技大学 | High-strength aluminum-based bulk amorphous composite material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106011695A (en) * | 2016-07-29 | 2016-10-12 | 中国科学院合肥物质科学研究院 | Al-base amorphous alloy block material and preparation method thereof |
| CN108130441A (en) * | 2017-05-19 | 2018-06-08 | 吉林大学 | A kind of adding technology that refining aluminum alloy is bred using non-crystaline amorphous metal |
| CN108866394A (en) * | 2018-07-20 | 2018-11-23 | 中国科学院金属研究所 | A kind of high-temperature oxidation resistant corrosion resistant coating alloy and coating |
| CN117840422A (en) * | 2024-03-08 | 2024-04-09 | 朗峰新材料启东有限公司 | Manganese-based amorphous nanocrystalline composite powder and preparation method thereof |
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Application publication date: 20140917 |