CN103122429A - Massive aluminum base noncrystal/nanocrystal composite material and preparation method thereof - Google Patents
Massive aluminum base noncrystal/nanocrystal composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of non-crystalline material preparation, particularly relates to a massive aluminum base noncrystal/nanocrystal composite material and a preparation method thereof, and particularly relates to a method for preparing the massive aluminum base noncrystal/nanocrystal composite material by adopting a spray deposition forming method. The massive aluminum base noncrystal/nanocrystal composite material comprises the following components in percentage by weight: 86% of aluminum, 0.5% of silicon, 4.06% of nickel, 2.94% of cobalt, 6% of yttrium and 0.5% of lanthanum and is in a composite structure which comprises a nanocrystal alpha-Al and an amorphous base. The composite material disclosed by the invention is in a noncrystal/nanocrystal composite structure and excellent in mechanical property, breaks through the bottleneck of the preparation size of the composite material in the prior art, can achieve the macroscopic size to 200 mm and is suitable for industrialized application; and the preparation process of the massive aluminum base noncrystal/nanocrystal composite material is simple, convenient to operate and favorable to the industrial popularization.
Description
Technical field
The invention belongs to the non-crystalline material preparation field, be specifically related to a kind of bulk aluminium-based amorphous alloy/nanocrystalline composite material and preparation method thereof, relate in particular to the method that adopts the standby bulk aluminium-based amorphous alloy/nanocrystalline composite material of jet deposition formation legal system.
Background technology
Studies show that, the matrix material that the nanoparticle disperse is distributed in the aluminium-based amorphous alloy matrix has excellent mechanical property.For example, the tensile strength of aluminium-based amorphous alloy/nanocrystalline composite material can reach 900～1200MPa, partially-crystallized Al
88Ni
9Ce
2Fe
1The tensile strength of matrix material strip can reach 1560MPa, is conventional aluminum alloy 2024T3 and 7075T6 tensile strength (approximately 600MPa left and right) 2～4 times.The Testing Tensile Strength at Elevated Temperature of aluminium-based amorphous alloy/nanocrystalline composite material still reaches 970MPa when 573K, is 15～20 times of conventional aluminum alloy.
The factors such as at present preparation aluminium-based amorphous alloy and nanometer crystal alloy mainly adopt melt supercooled and mechanical alloying method, and to form amorphous limited in one's ability because of aluminium alloy, strict to the composition that forms amorphous, and alloying time is long, and yield rate is low have limited its widespread use greatly.
In recent years, people utilize various forming techniques to attempt having prepared aluminium-based amorphous alloy/nanocrystalline composite material.For example, patent (publication number: CN102618807A) introduced a kind of aluminium-based amorphous alloy/nanocrystalline composite material and preparation method thereof.Material is elementary composition by Al, Cu and three kinds of Ti, and its atomic percent is followed successively by 65: 16.5: 18.5, and the amorphous volume fraction is 70～90%.Described material preparation step is as follows: (1) obtains amorphous powdered alloy by mechanical alloying; (2) utilize discharge plasma sintering to obtain aluminium-based amorphous alloy/nanocrystalline composite material, obtain cylindrical sintered specimen, sample is of a size of diameter 10x10mm; Patent (CN1431334) discloses a kind of aluminium-based amorphous alloy of high-strength low-density/Nanocomposite material and preparation method thereof.The atomic percent of material component is: nickel 8～10%, and lanthanum 1.5～2.1%, cerium 2.2～4%, praseodymium 0.1～0.8%, neodymium 0.2～1.1%, aluminium are surplus.Adopt spray to cast, copper mold cooled with liquid nitrogen method to prepare aluminium-based amorphous alloy/nanocrystalline composite diphase material, the composite diphase material thickness of this invention preparation is 1.5 millimeters.Statistic data shows, since 1988, numerous scientific research group studies hundreds of alloy systems, reach several thousand alloying constituents, but the critical size of aluminium-based amorphous alloy does not still break through the bottleneck of 1mm.In sum, although the aluminium-based amorphous alloy that these methods obtain/nanocrystalline composite material excellent property, size is limited, is difficult to obtain through engineering approaches and uses.Therefore, research block aluminum-base bulk amorphous alloys becomes current science anxious to be resolved and technical barrier.
The method that obtains at present block aluminum-base amorphous/nanocrystalline matrix material is mainly by controlling the liquid phase solidification rate, making nanoparticle directly separate out from melt.This method both can reduce the requirement to the aluminium-based amorphous alloy high solidification rate, can make again preparation process relatively simple.The greatest difficulty that this method runs into is, when the sample sectional dimension is larger, be difficult to guarantee that the heat with melt " sheds " fast, cause bulk aluminium-based amorphous alloy matrix crystallization or the nanocrystalline phase size of separating out is grown up, lost the excellent properties of aluminium-based amorphous alloy/nanocrystalline composite material.
The spray forming technology is widely used in the high performance rapidly solidified material Jin Shuhuohejinrongtiyi104～106℃/s of research and development in recent years.The innovative point that this technology is the most outstanding is, the atomizing of liquid metal and the deposition of atomized droplet are combined naturally, is a kind of short flow process rapid solidification body material new preparation technology.The formation of the fine and close part of jet deposition formation block is process of setting under given conditions.Its basic characteristics are to form one deck liquid film as thin as a wafer at deposition surface, and the formation of the fine and close part of block is the process that this liquid film constantly solidifies, advances.The Track character that forms Layer by layer solidification, propelling based on the fine and close part of jet deposition formation block, as long as choose alloy system and composition, control liquid phase solidification rate and separating out of nanometer crystalline phase and growing up of grain-size, adopt the jet deposition formation technology just might find a new approach for solving simultaneously above-mentioned two problems.
Summary of the invention
The technical problem to be solved in the present invention is, invent a kind of new aluminium-based amorphous alloy/nanocrystalline composite material, this material is conducive to prepare bulk aluminium-based amorphous alloy/nanocrystalline composite material, and propose a kind of preparation method and be mated, due to its limitation of size, be difficult to obtain the problem that through engineering approaches is used in the solution prior art.
For addressing the above problem, the present invention by the following technical solutions.
A kind of bulk aluminium-based amorphous alloy/nanocrystalline composite material, described material is comprised of aluminium, silicon, nickel, cobalt, yttrium, lanthanum, the atomic percent of each component is: aluminium 86%, silicon 0.5%, nickel 4.06%, cobalt 2.94%, yttrium 6%, lanthanum 0.5, it has the composite structure of nanocrystalline α-Al and noncrystal substrate composition.
The preferred version of matrix material of the present invention is, described nanocrystalline volume fraction is 5～25%, and the amorphous volume mark is 75～95%.
The preferred version of matrix material of the present invention is, macroscopical diameter of described matrix material is 100～200mm, and thickness is 1～11mm.
The preferred version of matrix material of the present invention is, described nanometer crystalline phase is α-Al phase, and it is of a size of 20-50nm.
A kind of preparation method of bulk aluminium-based amorphous alloy/nanocrystalline composite material comprises following preparation process:
The preparation of a, mother alloy: in atomic percent, according to Al
86Si
0.5Ni
4.06Co
2.94Y
6La
0.5Chemical formula carries out raw material ratio, adopts vacuum induction furnace to carry out melting.
B, composite manufacture: after the described master alloy ingot of step a is put into the remelting of medium-frequency induction furnace crucible, adopt the standby bulk aluminium-based amorphous alloy/nanocrystalline composite material of jet deposition formation legal system.
Preparation method's of the present invention preferred version is, starting material described in step a are high-purity material, and its purity is respectively higher than following numerical value, and Al is that 99.9wt%, Si are that 98wt%, Ni are that 99.9wt%, Co are that 99.9wt%, Y are that 99.9wt%, La are 99.9wt%.
Preparation method's of the present invention preferred version is, the described melting of step a is being carried out in the high-purity argon gas atmosphere of superfusion titanium oxygen consumption, and its purity is 99.999%.
Preparation method's of the present invention preferred version is that the described melting of step a is alloy cast ingot melt back 4 times.
Preparation method's of the present invention preferred version is that the processing parameter of the method for jet deposition formation described in step b is: atomizing gas: argon gas; Atomizing pressure: 0.6～0.8MPa; Deposition distance: 550～650mm; Draft-tube diameter: 3.5～4.5mm; Receive baseplate material: carbon steel or red copper.
The present invention adopts the spray forming technology, be mainly because: the first, in the liquid metal atomization process, each undersized drop can be thought the inclusion-free drop, during deposition, they do not contact spray chamber solid wall.This moment, the forming core of melt came own fluctuation of energy and structure to rise and fall fully, and the crystallization behavior of melt will be converted into homogeneous nucleation by heterogeneous forming core, and the melt undercooling degree is increased greatly.Second, the liquid metal jet deposition is to the substrate the time, the melt cooling speed of next-door neighbour's substrate is exceedingly fast, (liquid film is enough thin and the upper surface of melt thin layer and side do not contact with substrate, to such an extent as to can not be destroyed by gravitation and mass force, prevented the molten metal transverse flow), can be similar to as solidifying without container, effectively reduced the possibility of heterogeneous forming core.The 3rd, in Models of Spray Deposition, although rapid solidification mainly occurs in the molten drop flight course, in deposition process, because deposition surface is subjected to the forced convection of colder jet-stream wind cooling, rate of cooling still can reach 10
2K/s.This and the methods such as shrend and die cast are produced and are required when large block amorphous alloy melt integral body to reach lower critical cooling rate to be essentially different.
Undeniable, utilize the spray forming technology to prepare bulk aluminium-based amorphous alloy/nanocrystalline composite material and also have a critical thickness problem.Therefore, choose alloy system and composition, control liquid phase solidification rate and nanometer crystalline phase to separate out with growing up of grain-size be that the present invention possesses one of obvious creativeness.
Compare the present invention with existing preparation aluminium-based amorphous alloy/nanocrystalline composite material technology and have following beneficial effect: described matrix material has the amorphous/nanocrystalline composite structure, and its mechanical property is excellent; Broken through the bottleneck on this material preparation size in the prior art, its macro-size can reach 200mm, is suitable for industrial applications; The preparation technology of this bulk aluminium-based amorphous alloy/nanocrystalline composite material is simple, convenient operation, is conducive to industry and promotes.
Description of drawings
Fig. 1 is Al in the embodiment of the present invention 3
86Si
0.5Ni
4.06Co
2.94Y
6La
0.5Matrix material deposit preform macro morphology, vertical section, maximum ga(u)ge 12mm.
Fig. 2 is Al in the embodiment of the present invention 3
86Si
0.5Ni
4.06Co
2.94Y
6La
0.5Matrix material deposit preform exterior appearance, diameter 200mm.
Fig. 3 is the XRD spectral line of embodiment 3 matrix materials.
Fig. 4 is the DSC curve of embodiment 3 matrix materials.
Fig. 5 is that embodiment 1 matrix material blank medullary ray is apart from the TEM photo of the matrix material of lower surface 1mm place's sampling.
Fig. 6 is embodiment 2 matrix material blanks apart from the HRTEM photo of the α of the matrix material of medullary ray lower surface 3mm place's sampling-Al phase.
Fig. 7 is that embodiment 3 matrix material blank medullary rays are apart from the SEM photo of lower surface 11mm place's sampling.
Fig. 8 is the intensified image in white box zone in Fig. 7.
Embodiment
The present invention is described further below in conjunction with accompanying drawing.
Embodiment 1
According to Al
86Si
0.5Ni
4.06Co
2.94Y
6La
0.5Chemical formula carries out raw material ratio, adopts vacuum induction furnace to prepare the Al-Si-Ni-Co-Y-La mother alloy, and melting is being carried out in the high-purity argon gas atmosphere of superfusion titanium oxygen consumption, and its purity is 99.999%; Described starting material are high-purity material, and its purity is respectively, and Al is that 99.9wt%, Si are that 98wt%, Ni are that 99.9wt%, Co are that 99.9wt%, Y are that 99.9wt%, La are 99.9wt%.With above-mentioned master alloy ingot remelting 4 times, prepare bulk aluminium-based amorphous alloy/nanocrystalline composite material with the jet deposition formation method.Processing parameter is selected as follows: atomizing gas: argon gas; Atomizing pressure: 0.6MPa; Deposition distance: 550mm; Draft-tube diameter: 3.5mm; Receive baseplate material: carbon steel.Deposit preform size: diameter 80mm, thickness 2mm.Sample forms (Fig. 5) by nanocrystalline α-Al+ noncrystal substrate, and α-Al phase size is 20-50nm, and amorphous content reaches 93%.The Young's modulus of material and microhardness are respectively 80GPa and 4.13GPa.
According to Al
86Si
0.5Ni
4.06Co
2.94Y
6La
0.5Chemical formula carries out raw material ratio, adopts vacuum induction furnace to prepare the Al-Si-Ni-Co-Y-La mother alloy, and melting is being carried out in the high-purity argon gas atmosphere of superfusion titanium oxygen consumption, and its purity is 99.999%; Described starting material are high-purity material, and its purity is respectively, and Al is that 99.95wt%, Si are that 98.5wt%, Ni are that 99.95wt%, Co are that 99.95wt%, Y are that 99.95wt%, La are 99.9wt%.With above-mentioned master alloy ingot remelting, prepare bulk aluminium-based amorphous alloy/nanocrystalline composite material with the jet deposition formation method.Processing parameter is selected as follows: atomizing gas: argon gas; Atomizing pressure: 0.7MPa; Deposition distance: 600mm; Draft-tube diameter: 4.0mm; Receive baseplate material: red copper.Deposit preform size: diameter 130mm, maximum ga(u)ge 5mm.Sample is comprised of nanocrystalline α-Al+ noncrystal substrate, and α-Al phase size is 35-50nm(Fig. 6), amorphous content reaches 81%.
Embodiment 3
According to Al
86Si
0.5Ni
4.06Co
2.94Y
6La
0.5Chemical formula carries out raw material ratio, adopt vacuum induction furnace to prepare the Al-Si-Ni-Co-Y-La mother alloy, described starting material are high-purity material, and its purity is respectively, and Al is that 99.9wt%, Si are that 98wt%, Ni are that 99.9wt%, Co are that 99.9wt%, Y are that 99.9wt%, La are 99.9wt%.With above-mentioned master alloy ingot remelting, prepare bulk aluminium-based amorphous alloy/nanocrystalline composite material with the jet deposition formation method.Processing parameter is selected as follows: atomizing gas: argon gas; Atomizing pressure: 0.8MPa; Deposition distance: 650mm; Draft-tube diameter: 4.5mm; Receive baseplate material: red copper.Deposit preform size: diameter 200mm, maximum ga(u)ge 12mm(Fig. 1, Fig. 2).Take the deposit preform medullary ray as benchmark, measure from the bottom 1 and 6mm place sample form (Fig. 3) by nanocrystalline α-Al+ noncrystal substrate, 11mm place sample is by α-Al+Al
4The NiY+ noncrystal substrate forms (Fig. 7, Fig. 8).From the bottom 1,6 and the amorphous content of 11mm place sample reach respectively 91.7%, 78% and 54.3%(Fig. 4).Research further shows, when deposit thickness exceeds the amorphous formation critical thickness, α-Al phase alligatoring can occur and separate out other Crystallization Phases (Al in the tissue of deposit preform top
4NiY) problem (Fig. 7, Fig. 8).
Claims (9)
1. bulk aluminium-based amorphous alloy/nanocrystalline composite material, it is characterized in that: described material is comprised of aluminium, silicon, nickel, cobalt, yttrium, lanthanum, the atomic percent of each component is: aluminium 86%, silicon 0.5%, nickel 4.06%, cobalt 2.94%, yttrium 6%, lanthanum 0.5%, it has the composite structure of nanocrystalline α-Al and noncrystal substrate composition.
2. a kind of bulk aluminium-based amorphous alloy/nanocrystalline composite material according to claim 1, it is characterized in that: described nanocrystalline volume fraction is 5～25%, the amorphous volume mark is 75～95%.
3. a kind of bulk aluminium-based amorphous alloy/nanocrystalline composite material according to claim 1, it is characterized in that: macroscopical diameter of described matrix material is 80～200mm, thickness is 1～11mm.
4. a kind of bulk aluminium-based amorphous alloy/nanocrystalline composite material according to claim 1, it is characterized in that: described nanometer crystalline phase is α-Al phase, and it is of a size of 20-50nm.
5. the preparation method of a bulk aluminium-based amorphous alloy/nanocrystalline composite material is characterized in that: comprise following preparation process:
The preparation of a, mother alloy: in atomic percent, according to Al
86Si
0.5Ni
4.06Co
2.94Y
6La
0.5Chemical formula carries out raw material ratio, adopts vacuum induction furnace to carry out melting;
B, composite manufacture: after the described master alloy ingot of step a is put into the remelting of medium-frequency induction furnace crucible, adopt the standby bulk aluminium-based amorphous alloy/nanocrystalline composite material of jet deposition formation legal system.
6. preparation method according to claim 5, it is characterized in that: starting material described in step a are high-purity material, its purity is respectively higher than following numerical value, and Al is that 99.9wt%, Si are that 98wt%, Ni are that 99.9wt%, Co are that 99.9wt%, Y are that 99.9wt%, La are 99.9wt%.
7. the preparation method of bulk aluminium-based amorphous alloy/nanocrystalline composite material according to claim 5, is characterized in that, the described melting of step a is being carried out in the high-purity argon gas atmosphere of superfusion titanium oxygen consumption, and its purity is 99.999%.
8. the preparation method of bulk aluminium-based amorphous alloy/nanocrystalline composite material according to claim 5, it is characterized in that: the described melting of step a is alloy cast ingot melt back 4 times.
9. preparation method according to claim 5, it is characterized in that: the processing parameter of the method for jet deposition formation described in step b is: atomizing gas: argon gas; Atomizing pressure: 0.6～0.8MPa; Deposition distance: 550～650mm; Draft-tube diameter: 3.5～4.5mm; Receive baseplate material: carbon steel or red copper.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104357781A (en) * | 2014-11-07 | 2015-02-18 | 河海大学 | Marine environmental corrosion-resistant cored wire for aluminium-based amorphous nanocrystalline coating |
| CN105385966A (en) * | 2014-08-22 | 2016-03-09 | 华为技术有限公司 | Aluminum-based amorphous alloy, preparation method and applications thereof |
| CN107779683A (en) * | 2017-11-02 | 2018-03-09 | 济南大学 | A kind of Al base noncrystal alloys and preparation method thereof |
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| US5318641A (en) * | 1990-06-08 | 1994-06-07 | Tsuyoshi Masumoto | Particle-dispersion type amorphous aluminum-alloy having high strength |
| CN1245222A (en) * | 1998-08-19 | 2000-02-23 | 中国科学院金属研究所 | Al-base nm/non-crystal heterogeneous material |
| CN101451208A (en) * | 2008-12-30 | 2009-06-10 | 北京航空航天大学 | Block body aluminum-based alloy and preparation method thereof |
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2012
- 2012-12-31 CN CN2012105932766A patent/CN103122429A/en active Pending
Patent Citations (3)
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| US5318641A (en) * | 1990-06-08 | 1994-06-07 | Tsuyoshi Masumoto | Particle-dispersion type amorphous aluminum-alloy having high strength |
| CN1245222A (en) * | 1998-08-19 | 2000-02-23 | 中国科学院金属研究所 | Al-base nm/non-crystal heterogeneous material |
| CN101451208A (en) * | 2008-12-30 | 2009-06-10 | 北京航空航天大学 | Block body aluminum-based alloy and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| LONGCHAO ZHUO,ET AL: "Spray formed Al-based amorphous matrix nanocomposite plate", 《JOURNAL OF ALLOY AND COMPOUNDS》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105385966A (en) * | 2014-08-22 | 2016-03-09 | 华为技术有限公司 | Aluminum-based amorphous alloy, preparation method and applications thereof |
| CN105385966B (en) * | 2014-08-22 | 2017-09-12 | 华为技术有限公司 | A kind of Al-based Amorphous Alloys and its preparation method and application |
| CN104357781A (en) * | 2014-11-07 | 2015-02-18 | 河海大学 | Marine environmental corrosion-resistant cored wire for aluminium-based amorphous nanocrystalline coating |
| CN107779683A (en) * | 2017-11-02 | 2018-03-09 | 济南大学 | A kind of Al base noncrystal alloys and preparation method thereof |
| CN107779683B (en) * | 2017-11-02 | 2019-08-27 | 济南大学 | A kind of Al base noncrystal alloy and preparation method thereof |
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Application publication date: 20130529 |