CN101886234A - Bulk amorphous alloys of Zr-Cu-Al-Be series and preparation method thereof - Google Patents

Bulk amorphous alloys of Zr-Cu-Al-Be series and preparation method thereof Download PDF

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CN101886234A
CN101886234A CN201010231050.2A CN201010231050A CN101886234A CN 101886234 A CN101886234 A CN 101886234A CN 201010231050 A CN201010231050 A CN 201010231050A CN 101886234 A CN101886234 A CN 101886234A
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alloy
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block amorphous
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刘雄军
陈国良
惠希东
吕昭平
陈晓华
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University of Science and Technology Beijing USTB
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C45/00—Amorphous alloys
    • C22C45/10—Amorphous alloys with molybdenum, tungsten, niobium, tantalum, titanium, or zirconium or Hf as the major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C1/00—Making non-ferrous alloys
    • C22C1/11—Making amorphous alloys

Abstract

The invention relates to bulk amorphous alloys of Zr-Cu-Al-Be series with an extra-wide supercooling liquid phase region. The series of alloys take Zr52Cu40Al8 as basic ingredients, and take the metallic element Be with the minimum atomic radius as the alloying element. The composition of the series of alloy is determined through the following formula: (Zr52Cu40Al8)xBey, wherein x is the molar content of Zr52Cu40Al8, y is the molar content of Be, 80<=x<=100, 0<=y<=20, and x+y=100. The series of alloys can generate bulk amorphous alloys with the critical dimension not less than 3mm, the maximum supercooling liquid phase region reaching 123K and with excellent thermal stability. The series of alloys integrate better glass-forming ability and extra-wide supercooling liquid phase region, and can be widely used in the fields of precise parts, microelectronic components and the like.

Description

A kind of Zr-Cu-Al-Be Al-Cu-Zn block amorphous alloy and preparation method thereof
Technical field
The invention belongs to non-crystaline amorphous metal or metallic glass field, specifically relate to a kind of Zr-Cu-Al-Be Al-Cu-Zn block amorphous alloy and preparation method thereof
Background technology
Amorphous alloy (metallic glass) is the first-generation metal material that being expected to of occurring in recent years used as 26S Proteasome Structure and Function.Owing to have the weird atom arrangement architecture that is different from crystal alloy, amorphous alloy shows the excellent properties such as Ultrahigh Specific Strength, big elastic deformability, low thermal coefficient of expansion, superelevation solidity to corrosion and wear resistance that traditional crystal alloy can't be realized.These superior performances make amorphous alloy have broad application prospects in a lot of fields.
Though have above-mentioned excellent properties, the high rigidity of amorphous alloy and room temperature fragility make that it is carried out cold working becomes difficult, thereby have seriously limited it in industrial application.Recently, discover that non-crystaline amorphous metal has excellent supercooled liquid superplasticity, promptly (is higher than its glass transformation temperature T between its supercooling liquid phase region gAnd less than its initial crystallization temperature T xScope) non-crystaline amorphous metal can carry out thermoplasticity machine-shaping as common plastics.This specific character of non-crystaline amorphous metal makes the accurate clean forming technique of nano level become possibility, is expected to be applied at aspects such as information storage, nano die, accurate zero device fabrication.At present, the micron order non-crystaline amorphous metal gear that adopts thermoplastic molding's prepared military project and civilian on obtain Preliminary Applications.Have the excellent superplastic non-crystaline amorphous metal of supercooled liquid and must satisfy following condition: (1) has good thermostability.Non-crystaline amorphous metal is in the thermodynamics metastable state, the trend that always oriented thermodynamics stable state-crystalline state changes, and this transition temperature is exactly crystallization temperature T xIn order to prevent that non-crystaline amorphous metal from thermoplastic molding's process crystallization taking place, guarantee that the product that obtains after the processing remains non-crystalline state, just need to improve the thermostability of non-crystaline amorphous metal, the alloy system of exploitation high thermal stability.(2) has broad supercooling liquid phase region Δ T (=T x-T g).Because non-crystaline amorphous metal only just demonstrates the superplastic forming ability in supercooling liquid phase region, therefore, just need a bigger Δ T in order in bigger temperature range, to carry out thermoplasticity processing.(3) has glass forming ability preferably.Carrying out thermoplastic molding's processing needs the non-crystaline amorphous metal of large-size, because too for a short time being not easy to of sample size processed it.Amorphous alloy be alloy melt by being cooled fast to below the glass transformation temperature, avoid crystallization and solidify the solid alloy of formation.Therefore form non-crystaline amorphous metal and need speed of cooling faster.The alloying constituent that only possesses better glass forming ability could (as: copper mold casting, shrend etc.) obtain bulk amorphous alloy under the ordinary process condition.In fact, the glass forming ability by composition design raising alloy is one of hot issue of studying in this field always.
Owing to have preferably the relative advantage such as cheap of glass forming ability, high strength (breaking tenacity can surpass 2000Mpa), high tenacity with cost, the Zr-Cu-Al bulk amorphous alloys has caused the extensive concern of scientific circles and industry member, also is one of comparatively sophisticated non-crystaline amorphous metal at present.But the supercooling liquid phase region of this system alloy less (having only 48-73K) makes that its superplasticity working ability is relatively poor, thereby has seriously limited its application on industrial production.Therefore how to guarantee that the Zr-Cu-Al alloy has now under the prerequisite of advantage, the supercooling liquid phase region that improves above-mentioned alloy is that one of major issue to be solved is arranged at present.
Summary of the invention
Among the present invention by a large amount of experimental studies have found that, with the metallic element Be of an amount of atomic radius minimum
Figure BSA00000197083300021
Add in the Zr-Cu-Al alloy, not only can increase its supercooling liquid phase region, can also improve its glass forming ability simultaneously.Because Zr, Cu and Al atoms of elements radius are respectively
Figure BSA00000197083300022
Figure BSA00000197083300023
With
Figure BSA00000197083300024
The adding of Be element can be so that the various elementides that form in the alloy be fine and close more, thereby improve the viscosity of alloy melt, cause the raising of glass forming ability of alloy and the increase of supercooling liquid phase region.Though discover that adding the Be element can make the supercooling liquid phase region of this non-crystaline amorphous metal increase, but because Be is the unfriendly element of environment, the excessive interpolation of Be element can cause the toxic of non-crystaline amorphous metal, also can destroy simultaneously some excellent properties (for example: the interpolation of excessive Be element can reduce the toughness of alloy) that Zr-Cu-Al itself is had, and the Be element costs an arm and a leg, and therefore reduces the Financial cost that Be content has reduced described non-crystaline amorphous metal on the one hand; Can improve the security of described alloy on the other hand.Thereby the technical issues that need to address are exactly how to make the balance that reaches a suitable industrial application between Be content and the supercooling liquid phase region at present, that is: make the supercooling liquid phase region of this non-crystaline amorphous metal bigger, and Be content is also lower, and its toxicity almost can be ignored.In sum, the technical problem to be solved in the present invention is: develop and a kind ofly both had the Zr-Cu-Al alloy and have advantages such as high strength, high tenacity, the non-crystaline amorphous metal of industrial process applications has bigger supercooling liquid phase region and better glass forming ability again so that also will be taken into account the economy and the security of this non-crystaline amorphous metal simultaneously.
The objective of the invention is to adopt following technical scheme to realize:
Current experiments result shows that the Be element that adds certain content can strengthen the supercooling liquid phase region of Zr-Cu-Al base large amorphous alloy.We are by a large amount of experimental studies have found that among the present invention, by the suitable proportioning of adjusting Zr, Cu and three kinds of elements of Al, guaranteeing that this alloy has under the situation of big supercooling liquid phase region width and glass forming ability, by adding an amount of Be element, to obtain non-crystaline amorphous metal at this all good net effect aspect three of industrial processes performance, economy and security.
A kind of Zr-Cu-Al-Be Al-Cu-Zn block amorphous alloy, this Al-Cu-Zn block amorphous alloy comprise percent by volume and are not less than 95% amorphous phase, and this is that the main component of alloy is Zr, Cu, Al and Be, the following formulate of its composition: (Zr 52Cu 40Al 8) xBe y, wherein 80≤x≤100,0≤y≤20, and x+y=100.
Work as x=97, it is 6mm that y=3, this alloy can form large block amorphous critical size, and the width of supercooling liquid phase region is 108K.
Work as x=95, it is 10mm that y=5, this alloy can form large block amorphous critical size, and the width of supercooling liquid phase region is 112K.
Work as x=93, it is 10mm that y=7, this alloy can form large block amorphous critical size, and the width of supercooling liquid phase region is 119K.
The invention provides a kind of preparation method of above-mentioned Zr-Cu-Al-Be Al-Cu-Zn block amorphous alloy, concrete steps comprise:
Step 1: with purity is the metallic Z r of 99.0%-99.99wt%, Cu, and Al and Be are raw material, according to (Zr 52Cu 40Al 8) xBe yThe component ratio of regulation is prepared burden, wherein 80≤x≤100,0≤y≤20, and x+y=100, and this component ratio is a mol ratio;
Step 2: above-mentioned food ingredient mixed put into electric arc furnace, carry out arc melting in the argon gas atmosphere of titanium absorption, cooling obtains mother alloy ingot;
Step 3: with the refuse under these conditions of the above-mentioned mother alloy ingot that obtains, utilize the absorbing and casting device in the electric arc furnace, the mother alloy melt is drawn in the water cooled copper mould, obtain (Zr 52Cu 40Al 8) xBe yBulk amorphous alloys.
Beneficial effect of the present invention is:
(1) this alloy system has bigger supercooling liquid phase region, helps superplastic forming processing, is applicable to industrial processes, has improved the industrial applicability of alloy.
(2) Zr-Cu-Al-Be Al-Cu-Zn block amorphous alloy of the present invention has low Be content, and the supercooling liquid phase region width of alloy and not obviously reduction of glass forming ability.Because Be costs an arm and a leg, so the Zr-Cu-Al-Be alloy among the application has guaranteed economy under the prerequisite that guarantees industrial application.
(3) the concrete alloying constituent (Zr that relates among the present invention 52Cu 40Al 8) 95Be 5(Zr 52Cu 40Al 8) 97Be 7The glass forming ability of the two is best, and all can obtain diameter is the large block amorphous bar of 10mm, can satisfy the dimensional requirement in the processed and applied field of described non-crystaline amorphous metal, and supercooling liquid phase region is also very wide, help superplastic forming processing, Be content is lower, has guaranteed security and economy.
(4) purity of the required raw material Zr of preparation Zr-Cu-Al-Be Al-Cu-Zn block amorphous alloy of the present invention is 99.5wt%, can be the zirconium sponge of technical grade, and its price is much cheaper than high-purity Zr, thereby has further saved the cost of processing and manufacturing.
Description of drawings
The XRD figure of the Zr-Cu-Al Al-Cu-Zn block amorphous alloy of Fig. 1 embodiment of the invention 1 preparation
The DSC figure of the Zr-Cu-Al Al-Cu-Zn block amorphous alloy of Fig. 2 embodiment of the invention 1 preparation
The XRD figure of the Zr-Cu-Al-Be Al-Cu-Zn block amorphous alloy of Fig. 3 embodiment of the invention 2-4 preparation
The DSC figure of the Zr-Cu-Al-Be Al-Cu-Zn block amorphous alloy of Fig. 4 embodiment of the invention 2-4 preparation
Embodiment
Embodiment 1: preparation Zr 52Cu 40Al 8Bulk amorphous alloys
Step 1: with purity is the Zr of 99.5wt%, the Cu of 99.95wt%, and the Al of 99.7wt% is according to Zr 52Cu 40Al 8The mol ratio of regulation is prepared burden;
Step 2: above-mentioned food ingredient mixed put into electric arc furnace, carry out arc melting in the argon gas atmosphere of titanium absorption, cooling obtains mother alloy ingot;
Step 3: with the refuse under these conditions of the above-mentioned mother alloy ingot that obtains, utilize the absorbing and casting device in the electric arc furnace, the mother alloy melt is drawn in the water cooled copper mould that internal diameter is 3mm, obtain Zr 52Cu 40Al 8Bulk amorphous alloys.
Detect the constitutional features of bulk amorphous alloys with X-ray diffraction method (XRD).The XRD result of this alloy as shown in Figure 1.
Adopt dsc (DSC) this alloy to be carried out thermomechanical analysis, the thermodynamical coordinate that obtains being correlated with.The DSC curve of this alloy as shown in Figure 2, concrete thermodynamical coordinate is as shown in table 1.
Embodiment 2: preparation (Zr 52Cu 40Al 8) 97Be 3Bulk amorphous alloys
Step 1: with purity is the Zr of 99.5wt%, the Cu of 99.95wt%, and the Al of 99.7wt% and the Be of 99.0wt% are according to (Zr 52Cu 40Al 8) 97Be 3The mol ratio of regulation is prepared burden;
Step 2: above-mentioned food ingredient mixed put into electric arc furnace, carry out arc melting in the argon gas atmosphere of titanium absorption, cooling obtains mother alloy ingot;
Step 3: with the refuse under these conditions of the above-mentioned mother alloy ingot that obtains, utilize the absorbing and casting device in the electric arc furnace, the mother alloy melt is drawn in the water cooled copper mould that internal diameter is 6mm, obtain (Zr 52Cu 40Al 8) 97Be 3Bulk amorphous alloys.
Detect the constitutional features of bulk amorphous alloys with X-ray diffraction method (XRD).The XRD result of this alloy as shown in Figure 3.
Adopt dsc (DSC) this alloy to be carried out thermomechanical analysis, the thermodynamical coordinate that obtains being correlated with.The DSC curve of this alloy as shown in Figure 4, concrete thermodynamical coordinate is as shown in table 1.Embodiment 3: preparation (Zr 52Cu 40Al 8) 95Be 5Bulk amorphous alloys
Step 1: with purity is the Zr of 99.5wt%, the Cu of 99.95wt%, and the Al of 99.7wt% and the Be of 99.0wt% are according to (Zr 52Cu 40Al 8) 95Be 5The mol ratio of regulation is prepared burden;
Step 2: above-mentioned food ingredient mixed put into electric arc furnace, carry out arc melting in the argon gas atmosphere of titanium absorption, cooling obtains mother alloy ingot;
Step 3: with the refuse under these conditions of the above-mentioned mother alloy ingot that obtains, utilize the absorbing and casting device in the electric arc furnace, the mother alloy melt is drawn in the water cooled copper mould that internal diameter is 10mm, obtain (Zr 52Cu 40Al 8) 95Be 5Bulk amorphous alloys.
Detect the constitutional features of bulk amorphous alloys with X-ray diffraction method (XRD).The XRD result of this alloy as shown in Figure 3.
Adopt dsc (DSC) this alloy to be carried out thermomechanical analysis, the thermodynamical coordinate that obtains being correlated with.The DSC curve of this alloy as shown in Figure 4, concrete thermodynamical coordinate is as shown in table 1.
Embodiment 4: preparation (Zr 52Cu 40Al 8) 93Be 7Bulk amorphous alloys
Step 1: with purity is the Zr of 99.5wt%, the Cu of 99.95wt%, and the Al of 99.7wt% and the Be of 99.0wt% are according to (Zr 52Cu 40Al 8) 93Be 7The mol ratio of regulation is prepared burden;
Step 2: above-mentioned food ingredient mixed put into electric arc furnace, carry out arc melting in the argon gas atmosphere of titanium absorption, cooling obtains mother alloy ingot;
Step 3: with the refuse under these conditions of the above-mentioned mother alloy ingot that obtains, utilize the absorbing and casting device in the electric arc furnace, the mother alloy melt is drawn in the water cooled copper mould that internal diameter is 10mm, obtain (Zr 52Cu 40Al 8) 93Be 7Bulk amorphous alloys.
Detect the constitutional features of bulk amorphous alloys with X-ray diffraction method (XRD).The XRD result of this alloy as shown in Figure 3.
Adopt dsc (DSC) this alloy to be carried out thermomechanical analysis, the thermodynamical coordinate that obtains being correlated with.The DSC curve of this alloy as shown in Figure 4, concrete thermodynamical coordinate is as shown in table 1.
Embodiment 5-8 prepares the (Zr of various proportionings 52Cu 40Al 8) xBe yBulk amorphous alloys
Prepare the bulk amorphous alloys of various proportionings according to embodiment 2 described methods, its form and thermodynamical coordinate as shown in table 1.
Table 1: the composition of Zr-Cu-Al-Be bulk amorphous alloys of the present invention and thermodynamical coordinate
Figure BSA00000197083300051

Claims (5)

1. Zr-Cu-Al-Be Al-Cu-Zn block amorphous alloy is characterized in that: this Al-Cu-Zn block amorphous alloy comprises percent by volume and is not less than 95% amorphous phase, and this is that alloying constituent is Zr, Cu, Al and Be, the following formulate of its composition: (Zr 52Cu 40Al 8) xBe y, wherein 80≤x≤100,0≤y≤20, and x+y=100.
2. (Zr according to claim 1 52Cu 40Al 8) xBe yAl-Cu-Zn block amorphous alloy is characterized in that: x=97, y=3, (Zr 52Cu 40Al 8) 97Be 3It is 6mm that alloy can form large block amorphous critical size, and the width of supercooling liquid phase region is 108K.
3. according to the described (Zr of claim 1 52Cu 40Al 8) xBe yAl-Cu-Zn block amorphous alloy is characterized in that: x=95, y=5, (Zr 52Cu 40Al 8) 95Be 5It is 10mm that alloy can form large block amorphous critical size, and the width of supercooling liquid phase region is 112K.
4. according to the described (Zr of claim 1 52Cu 40Al 8) xBe yAl-Cu-Zn block amorphous alloy is characterized in that: x=93, y=7, (Zr 52Cu 40Al 8) 93Be 7It is 10mm that alloy can form large block amorphous critical size, and the width of supercooling liquid phase region is 119K.
5. according to the preparation method of the described Zr-Cu-Al-Be Al-Cu-Zn block amorphous alloy of claim 1-4, it is characterized in that comprising following concrete steps:
Step 1: with purity is the metallic Z r of 99.0%-99.99wt%, Cu, and Al and Be are raw material, according to (Zr 52Cu 40Al 8) xBe yThe component ratio of regulation is prepared burden, wherein 80≤x≤100,0≤y≤20, and x+y=100, and this component ratio is a mol ratio;
Step 2: above-mentioned food ingredient mixed put into electric arc furnace, carry out arc melting in the argon gas atmosphere of titanium absorption, cooling obtains mother alloy ingot;
Step 3: with the refuse under these conditions of the above-mentioned mother alloy ingot that obtains, utilize the absorbing and casting device in the electric arc furnace, the mother alloy melt is drawn in the water cooled copper mould, obtain (Zr 52Cu 40Al 8) xBe yBulk amorphous alloys.
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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN102268618A (en) * 2011-08-01 2011-12-07 清华大学 High specific strength light titanium-based amorphous alloy
CN102418053A (en) * 2011-12-09 2012-04-18 湖南科技大学 Zr-Cu-Ni-Al amorphous alloy containing trace boron and preparation method thereof
CN102563006A (en) * 2011-12-15 2012-07-11 比亚迪股份有限公司 Gear
CN103773977A (en) * 2014-01-26 2014-05-07 浙江大学 High-plasticity ZrCuAgAlBe bulk metal glass and preparation method thereof
WO2014151715A3 (en) * 2013-03-15 2015-08-06 Apple Inc. Bulk metallic glasses with low concentration of beryllium
CN106756647A (en) * 2016-12-12 2017-05-31 北京科技大学 A kind of high-ductility zirconium-based bulk amorphous alloy without nickel and preparation method thereof without beryllium
CN107841692A (en) * 2017-11-13 2018-03-27 东莞宜安科技股份有限公司 A kind of method that β type amorphous situ composite materials are prepared using iteration thought

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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
CN101538690A (en) * 2008-03-21 2009-09-23 比亚迪股份有限公司 Amorphous alloy and preparation method thereof
CN101580904A (en) * 2009-06-22 2009-11-18 北京科技大学 Method for preparing bulk amorphous alloy under non-vacuum condition and equipment

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Publication number Priority date Publication date Assignee Title
CN1511970A (en) * 2002-12-30 2004-07-14 中国科学院物理研究所 Copper base lump non-crystalline alloy
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
CN101538690A (en) * 2008-03-21 2009-09-23 比亚迪股份有限公司 Amorphous alloy and preparation method thereof
CN101580904A (en) * 2009-06-22 2009-11-18 北京科技大学 Method for preparing bulk amorphous alloy under non-vacuum condition and equipment

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102268618A (en) * 2011-08-01 2011-12-07 清华大学 High specific strength light titanium-based amorphous alloy
CN102268618B (en) * 2011-08-01 2012-12-19 清华大学 High specific strength light titanium-based amorphous alloy
CN102418053A (en) * 2011-12-09 2012-04-18 湖南科技大学 Zr-Cu-Ni-Al amorphous alloy containing trace boron and preparation method thereof
CN102563006A (en) * 2011-12-15 2012-07-11 比亚迪股份有限公司 Gear
CN102563006B (en) * 2011-12-15 2016-09-07 比亚迪股份有限公司 Gear
WO2014151715A3 (en) * 2013-03-15 2015-08-06 Apple Inc. Bulk metallic glasses with low concentration of beryllium
CN103773977A (en) * 2014-01-26 2014-05-07 浙江大学 High-plasticity ZrCuAgAlBe bulk metal glass and preparation method thereof
CN103773977B (en) * 2014-01-26 2016-07-27 浙江大学 A kind of big plasticity ZrCuAgAlBe system bulk metallic glass and preparation method thereof
CN106756647A (en) * 2016-12-12 2017-05-31 北京科技大学 A kind of high-ductility zirconium-based bulk amorphous alloy without nickel and preparation method thereof without beryllium
CN107841692A (en) * 2017-11-13 2018-03-27 东莞宜安科技股份有限公司 A kind of method that β type amorphous situ composite materials are prepared using iteration thought
CN107841692B (en) * 2017-11-13 2019-06-07 东莞宜安科技股份有限公司 A method of β type amorphous situ composite material is prepared using iteration thought

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