CN103898422B - A kind of Al-Ni-Er aluminum-based amorphous alloy material and preparation method thereof - Google Patents

A kind of Al-Ni-Er aluminum-based amorphous alloy material and preparation method thereof Download PDF

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CN103898422B
CN103898422B CN201410083838.1A CN201410083838A CN103898422B CN 103898422 B CN103898422 B CN 103898422B CN 201410083838 A CN201410083838 A CN 201410083838A CN 103898422 B CN103898422 B CN 103898422B
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程兴旺
尹嘉明
薛云飞
才鸿年
王本鹏
沈永华
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Beijing Institute of Technology BIT
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Abstract

A kind of Al-Ni-Er aluminum-based amorphous alloy of the present invention material and preparation method thereof, belongs to non-ferrous metal technical field.In alloy material of the present invention, the mole atom percentage composition of each component is: Al:80-95%; Ni:1-15%; Er:3-18%.The preparation method of alloy material of the present invention, first mixes metal A l, Ni, Er after carrying out oxide skin disengaging and cleaning, obtains mother alloy raw material; Then being oxygen absorbent with titanium, is under the condition of protection gas with argon gas, and adopted by mother alloy raw material arc melting 3 ~ 6 times to ensure that alloying constituent is even, then naturally cooling under argon gas atmosphere is protected, prepares the uniform mother alloy of melting; Finally under the atmosphere of argon shield gas, heat remelting to 900-1400K, after mother alloy melts completely, mother alloy melt is ejected into copper roller surface cool, obtained amorphous thin ribbon.Amorphous alloy good stability of the present invention, tensile strength is high, and composition cost is low, and preparation method is simple, has broad application prospects at formation light aluminum alloy Material Field.

Description

A kind of Al-Ni-Er aluminum-based amorphous alloy material and preparation method thereof
Technical field
The invention belongs to non-ferrous metal technical field, be specifically related to a kind of Al-Ni-Er aluminum-based amorphous alloy material and preparation method thereof.
Background technology
Since the sixties in 20th century, Duwes prepared Au-Si system non-crystaline amorphous metal by the method for melt spinning method first, the preparations and applicatio of amorphous alloy causes the great interest of domestic and international material supplier author.In recent years, along with the maturation gradually of ferromegnetism AMORPHOUS ALLOY, and the developing rapidly of space flight and aviation and transportation means lightness, people start research work attention being turned to high-strength low-density material, especially al based amorphous alloy and nano combined al based amorphous alloy, as emerging engineering materials, with excellent properties such as its high strength, low density, good solidity to corrosion and wear resistancies, arouse widespread concern, development in recent years is very rapid.
Prepare al based amorphous alloy at present and mainly adopt quench and mechanical alloying method.Quench and rapid solidification method, that commonly uses now has three kinds: melt-quenching method, gas atomization, surface melting and reinforcement, wherein the most frequently used preparation method is melt-quenching method.The successful preparation of aluminium-based amorphous alloy, breaches aluminium alloy and is difficult to form amorphous obstacle, achieves variation prepared by aluminum alloy organization (amorphous, nanocrystalline, nanometer/amorphous multiphase structure etc.), has increased substantially the performance of aluminium alloy.Research shows, is the non-crystaline amorphous metal of 84 ~ 86% containing Al atomic percent, and its tensile strength intensity can reach 1000MPa, exceedes the order of magnitude of the ultra-high-strength aluminum alloy 700MPa in crystalline material, is 2 ~ 4 times of general conventional aluminum strength of alloy.
Weighing one of the most direct method of amorphous formation ability is measure the critical size (thickness) of non-crystaline amorphous metal.The critical size of non-crystaline amorphous metal is larger, also just means that the amorphous formation ability of this alloy is stronger.Research shows, by appropriate design, in non-crystaline amorphous metal system, composition constituent element is more, and the amorphous formation ability of non-crystaline amorphous metal is also stronger to a certain extent.But because al based amorphous alloy system amorphous formation ability is undesirable, the ternary aluminium-based amorphous alloy thickness obtained at present is only strip or the powdered samples of about 30 ~ 100 μm mostly.In addition, amorphous alloy material belongs to metastable state, and in laser heating process, when reaching crystallization temperature, nuclear power overcomes potential barrier and resets, and crystallization occurs, is converted into crystalline material, therefore weighs the important indicator that thermostability is also non-crystaline amorphous metal.Evaluation for amorphous thermostability uses differential thermal analysis (DSC) to measure the glass transition temperature (T of non-crystaline amorphous metal mostly g) and crystallization temperature (T x), T gand T xhigher, non-crystaline amorphous metal thermally-stabilised also better.But the crystallization temperature of most of al based amorphous alloy only has between 400 ~ 500K, and low glass forming ability and thermostability all significantly limit the application of al based amorphous alloy.Therefore improve Al-based Amorphous Alloys glass forming ability and thermostability, improving the critical size of al based amorphous alloy, is current problem demanding prompt solution.
Summary of the invention
The object of the present invention is to provide a kind of reasonable mixture ratio of components, the Al-Ni-Er system al based amorphous alloy material with good amorphous formation ability and preparation method thereof.
The object of the invention is to be achieved through the following technical solutions:
A kind of Al-Ni-Er aluminum-based amorphous alloy material of the present invention, in described alloy material, the mole atom percentage composition of each component is as follows:
Al：80-95%，
Ni：1-15%，
Er：3-18%。
The preparation method of a kind of Al-Ni-Er aluminum-based amorphous alloy material of the present invention, comprises the following steps: the first step: batching
After metal A l, Ni, Er are carried out oxide skin disengaging and cleaning, carry out preparing burden and mixing after following atom content per-cent is scaled mass percent, obtain mother alloy raw material;
Al：80-95%，
Ni：1-15%，
Er：3-18%。
Second step: prepare mother alloy
Being oxygen absorbent with titanium, is under the condition of protection gas with argon gas, and the mother alloy raw material that the first step prepared adopts arc melting 3 ~ 6 times to ensure that alloying constituent is even, and then naturally cooling under argon gas atmosphere is protected, prepares the uniform mother alloy of melting;
3rd step: get rid of the obtained non-crystaline amorphous metal of band
Mother alloy obtained for second step is carried out oxide skin to depart from and to process and after cleaning; use single roller quick solidification apparatus; mother alloy is positioned in the silica tube of the lower end grinding out being wound with induction heating wire coil; remelting is heated to 900-1400K under the atmosphere of argon shield gas; after mother alloy melts completely; mother alloy melt is ejected into the copper roller surface cool that linear velocity is 8-20m/s, obtained amorphous thin ribbon, melt jet pressure is 0.01 ~ 0.03MPa.
The present invention has following beneficial effect:
(1) a kind of Al-Ni-Er aluminum-based amorphous alloy of the present invention's proposition, transition element Ni in alloy and rare earth element er have more special outer electronic structure (d or f orbitals are not full of completely), stable hybridized orbital is formed with Al atom, improve the linkage force between alloy constituent element, in addition because transition element Ni and rare earth element er differ larger with the size of Al atom, improve the density of the random stacking provisions of alloy, increase the viscosity of alloy, inhibit the motion of constituent element atom when solidifying, thus improve amorphous conversion temp and the crystallization temperature of non-crystaline amorphous metal, thus be convenient to form metastable non-crystaline amorphous metal.
(2) a kind of Al-Ni-Er aluminum-based amorphous alloy of the present invention's proposition, due to adding of rare earth element er, makes the enthalpy of mixing in alloy system between each element significantly reduce, thus comprehensively improves the amorphous formation ability of alloy; Can prepare by melt-quenching method the amorphous thin ribbon that thickness reaches 280 μm, be 1 ~ 2 times of general aluminium-based amorphous alloy strip thickness.
(3) a kind of Al-Ni-Er aluminum-based amorphous alloy of proposing of the present invention, composition cost is low, and preparation method is simple, and technical pure metal A l, Ni and Er can be adopted as raw material, tensile strength up to 1200MPa,
It is made to have broad application prospects at formation light aluminum alloy Material Field.
Accompanying drawing explanation
Fig. 1 the present invention is the Al that embodiment 1 obtains 85ni 8er 7amorphous alloy ribbon XRD figure spectrum analysis result figure;
Fig. 2 the present invention is the Al that embodiment 1 obtains 85ni 8er 7the DSC tracing analysis result figure of amorphous alloy ribbon;
The Al that Fig. 3 embodiment of the present invention 1 obtains 85ni 8er 7the TEM photo of amorphous alloy ribbon.
Embodiment
Below in conjunction with embodiment, content of the present invention is described further.
Embodiment 1:Al 85ni 8er 7the preparation of amorphous alloy ribbon
1) commercially available pure Al, Ni, Er metal blocks is selected to make raw material, first pure metal block surface is carried out oxide skin to depart from and ultrasonic surface cleaning, according to atom percentage content Al85%, Ni8%, Er7% prepares burden, and uses electronic balance to take quality and is respectively Al20.4049g, Ni4.7181g, Er10.4169g, mixes alloy block afterwards;
2) being oxygen absorbent with titanium, is under the condition of protection gas with argon gas, by the 1st) the mother alloy raw material for preparing of step adopts arc melting 6 times, and to ensure that alloying constituent is even, then naturally cooling under argon gas atmosphere protection, prepares the uniform mother alloy of melting;
3) by the 2nd) the obtained mother alloy of step is after surperficial mechanical grinding and cleaning; be placed in the silica tube being wound with wire coil of lower end ground; heating remelting is to 1000K; after mother alloy melts completely; copper roller surface cool mother alloy melt being ejected into rotation obtains amorphous alloy ribbon; heat remelting and get rid of band process and carry out under argon gas atmosphere protection, copper roller linear velocity is 16m/s, and melt jet pressure is 0.03MPa.
The thickness prepared according to the method described above is the Al of 280 μm 85ni 8er 7band is through X ray diffracting spectrum (XRD), and transmission electron microscope (TEM) and differential thermal analyzer (DSC) are analyzed.For crystalline material, XRD figure spectrum signature is the spectral line with one group of sharp peak; And non-crystalline material, XRD figure spectrum is then for having the spectral line of " steamed bun peak " feature.Analyze known through transmission electron microscope (TEM), there is no the contrast in crystalline material in TEM image, and electron diffraction pattern is also be made up of several " halo " with one heart specific to non-crystalline material, the border of each halo is very fuzzy.By XRD and tem analysis known, Al 85ni 8er 7band is amorphous alloy material; By dsc analysis, Al 85ni 8er 7band crystallization temperature T x=510K, has good thermostability.By Resarch on A New Type, Al 85ni 8er 7the tensile strength of band, up to 1200MPa, has excellent mechanical property.
Embodiment 2:Al 85ni 9er 6amorphous alloy ribbon
Commercially available pure Al, Ni, Er metal blocks is selected to make raw material, first pure metal block surface is carried out oxide skin to depart from and ultrasonic surface cleaning, according to atom percentage content Al85%, Ni9%, Er6% prepares burden, and uses electronic balance to take quality and is respectively Al20.9840g, Ni4.8337g, Er9.1822g, mixes alloy block afterwards; Be oxygen absorbent with titanium, be under the condition of protection gas with argon gas, the mother alloy raw material the first step prepared adopts arc melting 6 times, and to ensure that alloying constituent is even, then naturally cooling under argon gas atmosphere protection, prepares the uniform mother alloy of melting; By mother alloy obtained for second step after surperficial mechanical grinding and cleaning, be placed in the silica tube being wound with wire coil of lower end ground, heating remelting is to about 950K, and after mother alloy melts completely, copper roller surface cool mother alloy melt being ejected into rotation obtains Al 85ni 9er 6amorphous alloy ribbon, heat remelting and get rid of band process and carry out under argon gas atmosphere protection, copper roller linear velocity is 20m/s, and melt jet pressure is 0.02MPa.The Al prepared according to the method described above 85ni 9er 6band is non-crystalline material through XRD, TEM, DSC detection validation.
Embodiment 3:Al 86ni 9er 5amorphous alloy ribbon
Commercially available pure Al, Ni, Er metal blocks is selected to make raw material, first pure metal block surface is carried out oxide skin to depart from and ultrasonic surface cleaning, according to atom percentage content Al86%, Ni9%, Er5% prepares burden, and uses electronic balance to take quality and is respectively Al22.00391g, Ni5.0177g, Er7.9431g, mixes alloy block afterwards; Be oxygen absorbent with titanium, be under the condition of protection gas with argon gas, the mother alloy raw material the first step prepared adopts arc melting 6 times, and to ensure that alloying constituent is even, then naturally cooling under argon gas atmosphere protection, prepares the uniform mother alloy of melting; By mother alloy obtained for second step after surperficial mechanical grinding and cleaning, be placed in the silica tube being wound with wire coil of lower end ground, heating remelting is to about 1100K, and after mother alloy melts completely, copper roller surface cool mother alloy melt being ejected into rotation obtains Al 86ni 9er 5amorphous alloy ribbon, heat remelting and get rid of band process and carry out under argon gas atmosphere protection, copper roller linear velocity is 17m/s, and melt jet pressure is 0.02MPa.The Al prepared according to the method described above 86ni 9er 5band is non-crystalline material through XRD, TEM, DSC detection validation.
Embodiment 4:Al 86ni 6er 8amorphous alloy ribbon
Commercially available pure Al, Ni, Er metal blocks is selected to make raw material, first pure metal block surface is carried out oxide skin to depart from and ultrasonic surface cleaning, according to atom percentage content Al86%, Ni6%, Er8% prepares burden, and uses electronic balance to take quality and is respectively Al20.2494g, Ni3.0735g, Er11.6769g, mixes alloy block afterwards; Be oxygen absorbent with titanium, be under the condition of protection gas with argon gas, the mother alloy raw material the first step prepared adopts arc melting 6 times, and to ensure that alloying constituent is even, then naturally cooling under argon gas atmosphere protection, prepares the uniform mother alloy of melting; By mother alloy obtained for second step after surperficial mechanical grinding and cleaning, be placed in the silica tube being wound with wire coil of lower end ground, heating remelting is to about 1150K, and after mother alloy melts completely, copper roller surface cool mother alloy melt being ejected into rotation obtains Al 86ni 6er 8amorphous alloy ribbon, heat remelting and get rid of band process and carry out under argon gas atmosphere protection, copper roller linear velocity is 15m/s, and melt jet pressure is 0.01MPa.The Al prepared according to the method described above 86ni 6er 8band is non-crystalline material through XRD, TEM, DSC detection validation.
Embodiment 5:Al85Ni6Er9 amorphous alloy ribbon
Commercially available pure Al, Ni, Er metal blocks is selected to make raw material, first pure metal block surface is carried out oxide skin to depart from and ultrasonic surface cleaning, according to atom percentage content Al85%, Ni6%, Er9% prepares burden, and uses electronic balance to take quality and is respectively Al19.3376g, Ni2.9696g, Er12.6926g, mixes alloy block afterwards; Be oxygen absorbent with titanium, be under the condition of protection gas with argon gas, the mother alloy raw material the first step prepared adopts arc melting 6 times, and to ensure that alloying constituent is even, then naturally cooling under argon gas atmosphere protection, prepares the uniform mother alloy of melting; By mother alloy obtained for second step after surperficial mechanical grinding and cleaning; be placed in the silica tube being wound with wire coil of lower end ground; heating remelting is to about 1180K; after mother alloy melts completely; copper roller surface cool mother alloy melt being ejected into rotation obtains Al85Ni6Er9 amorphous alloy ribbon; heat remelting and get rid of band process and carry out under argon gas atmosphere protection, copper roller linear velocity is 19m/s, and melt jet pressure is 0.03MPa.The Al85Ni6Er9 band prepared according to the method described above is non-crystalline material through XRD, TEM, DSC detection validation.

Claims (1)

1. a preparation method for Al-Ni-Er aluminum-based amorphous alloy material, is characterized in that: comprise the following steps:
The first step: batching
After metal A l, Ni, Er are carried out oxide skin disengaging and cleaning, carry out preparing burden and mixing after following atom content per-cent is scaled mass percent, obtain mother alloy raw material;
Al：80-95％，
Ni：1-15％，
Er：3-18％；
Second step: prepare mother alloy
Being oxygen absorbent with titanium, is under the condition of protection gas with argon gas, and the mother alloy raw material that the first step prepared adopts arc melting 3 ~ 6 times to ensure that alloying constituent is even, and then naturally cooling under argon gas atmosphere is protected, prepares the uniform mother alloy of melting;
3rd step: get rid of the obtained non-crystaline amorphous metal of band
Mother alloy obtained for second step is carried out oxide skin to depart from and to process and after cleaning; remelting is heated to 900-1400K under the atmosphere of argon shield gas; after mother alloy melts completely; mother alloy melt is ejected into the copper roller surface cool that linear velocity is 8-20m/s; obtained amorphous thin ribbon, melt jet pressure is 0.01 ~ 0.03MPa.
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CN104388843A (en) * 2014-12-23 2015-03-04 内蒙古科技大学 Al-MR-TM-TE aluminum-based amorphous alloy and preparation method thereof
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