CN103173699A - Zn-containing Mg-Cu-Gd bulk amorphous alloy and preparation method thereof - Google Patents
Zn-containing Mg-Cu-Gd bulk amorphous alloy and preparation method thereof Download PDFInfo
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- CN103173699A CN103173699A CN2013100949661A CN201310094966A CN103173699A CN 103173699 A CN103173699 A CN 103173699A CN 2013100949661 A CN2013100949661 A CN 2013100949661A CN 201310094966 A CN201310094966 A CN 201310094966A CN 103173699 A CN103173699 A CN 103173699A
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Abstract
The invention provides a Zn-containing Mg-Cu-Gd bulk amorphous alloy and a preparation method thereof. On the basis of an Mg-Cu-Gd amorphous alloy with strong glass forming capability, Mg elements are partially substituted by Zn elements, and the quaternary bulk amorphous alloy with Mg65-xZnxCu25Gd10(x=3, 5, 8at. %) as a component is prepared by using a copper mold spray casting process. A Cu-Gd intermediate alloy is prepared in advance by using a vacuum conduction melting furnace, a Mg-Zn-Cu-Gd mother alloy is then prepared, the mother alloy is remelted finally, and the molten mother alloy is sprayed into a copper mold cavity to obtain the Mg-Zn-Cu-Gd bulk amorphous alloy. The preparation method provided by the invention is simple in process and low in cost, and the mechanical property of the amorphous alloy can be remarkably improved while the stronger glass forming capability of the amorphous alloy is kept.
Description
Technical field
What the present invention relates to is a kind of block amorphous alloy, and that the present invention also relates to is a kind of preparation method of block amorphous alloy.
Background technology
Enter 21 century, along with industrial expansions such as China's aerospace, electronics, machineries, alloy material light to quality, excellent combination property has proposed requirements at the higher level.Under this background, high performance light-duty alloy there is active demand, therefore, the research and development that strengthens the light weight high strength structure material is imperative.Magnesium base amorphous alloy is light due to its quality, intensity is high, glass forming ability is strong, and the many advantages such as its raw material and low price, is the ideal candidates person as the light weight high strength structure material, has very wide application prospect.
In early days, mainly to concentrate on the stronger Mg-Cu-(Y, Gd) of glass forming ability be the ternary non-crystaline amorphous metal in the research of magnesium base amorphous alloy.Afterwards, along with the development of non-crystaline amorphous metal, people developed by the method for adjusting alloying constituent and adding other elements (as Al, Ag, Li, Pd, Ni and Zn etc.) on this basis a series ofly have the quaternary of larger glass forming ability and excellent mechanical property, magnesium base amorphous alloy more than five yuan and five yuan.The development light weight high strength structure material that appears as of magnesium base amorphous alloy opens up a new way, and the development of this class magnesium base amorphous alloy material all is devoted in countries in the world at present.Recently, (the G.Y.Yuan such as Yuan, T.Zhang and A.Inoue, Mater.Trans.JIM, 2003,44:2271) and (Z.G.Li such as Li, X.Hui, C.M.Zhang and G.L.Chen, J.Alloys Compd., 2008,454:168) prepare respectively on Mg-Cu-Y ternary non-crystaline amorphous metal basis and studied the Mg-Cu-Zn-Y Al-La-Y-Ni.Result all finds, the Zn element add the mechanical property that Mg-Cu-Y ternary non-crystaline amorphous metal is significantly carried in membership, wherein composition is Mg
58Cu
25Zn
7Y
10The compressed rupture strength of non-crystaline amorphous metal has reached 1090MPa, be far above Mg
65Cu
25Y
10The 823MPa of non-crystaline amorphous metal.Yet however, also do not add Zn in Mg-Cu-Gd ternary non-crystaline amorphous metal at present, the relevant report of research and preparation Mg-Zn-Cu-Gd Al-La-Y-Ni.
Summary of the invention
The object of the present invention is to provide a kind of Mg-Cu-Gd block amorphous alloy that contains Zn with high compression breaking tenacity and microhardness.The present invention also aims to provide a kind of loss on ignition that can reduce the low melting point metals such as Mg, the preparation method of the Mg-Cu-Gd block amorphous alloy that contains Zn of the accuracy of assurance alloying constituent.
The nominal composition of the Mg-Cu-Gd block amorphous alloy of the Zn of containing of the present invention is Mg
65-xZn
xCu
25Gd
10, x=3 wherein, 5,8at. ﹪.
The preparation method of the Mg-Cu-Gd block amorphous alloy of the Zn of containing of the present invention is:
1, the preparation of mother alloy: be that 99.9% MAG block, purity are that 99.9% spelter, purity are that 99.8% copper ingot and purity are that 99.99% gadolinium piece is by nominal composition Mg with purity
65-xZn
xCu
25Gd
10Batching, x=3 wherein, 5,8at. ﹪; At first copper ingot and gadolinium piece raw material are put into quartz test tube, be placed in induction melting furnace ruhmkorff coil center, close fire door, then be evacuated to 10
-4Pa is filled with 10
-2The argon gas of Pa carries out the melting of Cu-Gd master alloy with the method for vacuum induction melting under argon shield; Then with Cu-Gd master alloy sanding and polishing, mix with MAG block and spelter after pulverizing, use the melting method identical with the melting of Cu-Gd master alloy to prepare the Mg-Zn-Cu-Gd mother alloy;
2, non-crystaline amorphous metal sample preparation: with the Mg-Zn-Cu-Gd mother alloy sanding and polishing that makes, with ultrasonic oscillator, it is cleaned, in the quartz test tube of packing into after pulverizing, be placed in the ruhmkorff coil center of induction melting furnace, closing fire door, is P toward the interior charged pressure of quartz test tube upper end gas-holder
1High-purity argon gas, P
1=5 * 10
-2Pa is filled with 5 * 10 after pumping high vacuum repeatedly with furnace chamber
-2The argon shield gas of Pa forms P
2Negative pressure, remelting mother alloy in the intermediate frequency vacuum induction melting furnace of argon gas atmosphere, with the molten state Mg-Zn-Cu-Gd mother alloy that obtains at pressure difference P=P
1+ P
2Effect under spray in the copper mold die cavity, obtain the Mg-Zn-Cu-Gd block amorphous alloy.
After the present invention partly substituted Mg element in the Mg-Cu-Gd alloy with the Zn element, the alloy constituent element had been increased to quaternary by ternary, and the chemical complicacy of alloy increases thereupon, is beneficial to the decrystallized of alloy, meets " confusion " principle that non-crystaline amorphous metal forms design.In addition, owing to larger atomic radius being arranged than (Mg/Zn=1.20 between Zn element and Mg and Gd element; Gd/Zn=1.34) and negative mixture heat (Mg-Zn:-4kJ/mol; Gd-Zn:-31kJ/mol), so the alloy designs in the present invention meets three empirical laws of the formation block amorphous alloy of Inoue proposition fully.Therefore, the Mg element that partly substitutes in the Mg-Cu-Gd alloy with the Zn element is beneficial to the Mg-Zn-Cu-Gd Al-La-Y-Ni that formation has larger glass forming ability and good mechanical properties.In view of the performance of magnesium base block amorphous alloy excellence and wide application prospect, the Mg-Zn-Cu-Gd block amorphous alloy of developing the stronger glass forming ability of a kind of tool and good mechanical property has important scientific research and engineering using value.
The advantage that contains the Mg-Cu-Gd block amorphous alloy of Zn in the present invention is:
1, with the Mg element in Zn element Partial Replacement Mg-Cu-Gd, increase thus alloy constituent element number and chemical complicacy, improved the non-crystaline amorphous metal glass forming ability;
2, alloy melting adopts merological approach, by melting refractory metal in advance, and melting low melting point metal then, the remarkable like this loss on ignition that reduces the low melting point metals such as Mg has guaranteed the accuracy of alloying constituent;
3, gained Mg-Zn-Cu-Gd non-crystaline amorphous metal has high compressed rupture strength and microhardness, is 2～3 times of traditional crystalline state magnesium alloy strength.
Description of drawings
Fig. 1 is the prepared XRD figure spectrum that contains the Mg-Cu-Gd block amorphous alloy of Zn of the present invention.
Fig. 2 is the prepared DSC curve that contains the Mg-Cu-Gd block amorphous alloy of Zn of the present invention.
Fig. 3 is the prepared compressive stress strain curve that contains the Mg-Cu-Gd block amorphous alloy of Zn of the present invention.
Fig. 4 is the prepared microhardness histogram that contains the Mg-Cu-Gd block amorphous alloy of Zn of the present invention.
Embodiment
The below is for a more detailed description to the present invention for example.
Case of comparative examples
Prepared composition is Mg
65Cu
25Gd
10Ternary block amorphous alloy, sample diameter is 2mm.
Step 1: the preparation of mother alloy: be that 99.9% high-purity MAG block, purity are that high-purity copper ingot of 99.8% and purity are that high-purity gadolinium piece of 99.99% is by composition proportion Mg with purity
65Cu
25Gd
10Take raw material; At first alloy raw material Cu and Gd are put into quartz test tube, be placed on the ruhmkorff coil center of induction melting furnace, avoid contacting with coil, close fire door, then be evacuated to 10
-4Pa is filled with 10
-2The argon gas of Pa, repeatedly after three times under argon shield molten alloy, even for making alloying constituent, with alloy melt back 3～5 times, make the Cu-Gd master alloy.Then with Cu-Gd master alloy sanding and polishing, pulverizing heel purity is 99.9% MAG block mixing, makes the Mg-Cu-Gd mother alloy with identical melting method at last.
Step 2: non-crystaline amorphous metal sample preparation: the Mg-Cu-Gd mother alloy sanding and polishing that step 1 is made, to remove the oxide skin on mother alloy surface, with ultrasonic oscillator, it is cleaned, in the quartz test tube of packing into after the mother alloy pulverizing, be placed on the ruhmkorff coil center of induction melting furnace, avoid contacting with coil; Closing fire door, is P toward the interior charged pressure of quartz test tube upper end gas-holder
1(5 * 10
-2Pa) high-purity argon gas is filled with 5 * 10 after pumping high vacuum repeatedly with furnace chamber
-2The argon shield gas of Pa forms P
2Negative pressure, the above-mentioned mother alloy of remelting in the intermediate frequency vacuum induction melting furnace of argon gas atmosphere, with the molten state Mg-Cu-Gd mother alloy that obtains at pressure difference P=P
1+ P
2Effect under spray in the copper mold die cavity, obtain the Mg of diameter 2mm
65Cu
25Gd
10The block amorphous alloy sample.
Adopt the weave construction of X-ray diffraction method sign gained sample, as shown in Figure 1.By " the steamed bun peak " of the general demonstration of XRD figure of this sample as can be known, the typical non-crystal structure feature of the internal structure tool of gained sample illustrates that this alloy sample is non-crystaline amorphous metal.
Adopt the amorphous formation ability of DSC curve sign gained sample, as shown in Figure 2.By the DSC curve as can be known, the glass transformation temperature T of gained sample
g, initial crystallization temperature T
xWith supercooling liquid phase region Δ T
x(Δ T
x=T
x-T
g) value be respectively 437K, 505K, 68K.
Utilize the compressed rupture strength of Instron4505 type electronic universal tester test non-crystaline amorphous metal sample to characterize its mechanical property, compressive strain speed is 2 * 10
-4s
-1, as shown in Figure 3.As seen from the figure, the compressed rupture strength of gained sample is 648MPa.
Utilize the hardness value of HXS-1000Z type hardness tester instrumentation amount sample, as shown in Figure 4.Result shows that the microhardness of gained non-crystaline amorphous metal sample is 257Hv.
Select preparation x=3, be divided into Mg
62Zn
3Cu
25Gd
10Block amorphous alloy, sample diameter is 2mm.
Step 1: the preparation of mother alloy: be that 99.9% high-purity MAG block, purity are that 99.9% spelter, purity are that high-purity copper ingot of 99.8% and purity are that high-purity gadolinium piece of 99.99% is by composition proportion Mg with purity
62Zn
3Cu
25Gd
10Take raw material; At first alloy raw material Cu and Gd are put into quartz test tube, be placed on the ruhmkorff coil center of induction melting furnace, avoid contacting with coil, close fire door, then be evacuated to 10
-4Pa is filled with 10
-2The argon gas of Pa, repeatedly after three times under argon shield molten alloy, even for making alloying constituent, with alloy melt back 3～5 times, make the Cu-Gd master alloy.Then with Cu-Gd master alloy sanding and polishing, pulverize heel purity and be 99.9% MAG block and purity and be 99.9% spelter and mix, make the Mg-Zn-Cu-Gd mother alloy with identical melting method at last.
Step 2: non-crystaline amorphous metal sample preparation: the Mg-Zn-Cu-Gd mother alloy sanding and polishing that step 1 is made, to remove the oxide skin on mother alloy surface, with ultrasonic oscillator, it is cleaned, in the quartz test tube of packing into after the mother alloy pulverizing, be placed on the ruhmkorff coil center of induction melting furnace, avoid contacting with coil; Closing fire door, is P toward the interior charged pressure of quartz test tube upper end gas-holder
1(5 * 10
-2Pa) high-purity argon gas is filled with 5 * 10 after pumping high vacuum repeatedly with furnace chamber
-2The argon shield gas of Pa forms P
2Negative pressure, the above-mentioned mother alloy of remelting in the intermediate frequency vacuum induction melting furnace of argon gas atmosphere, with the molten state Mg-Zn-Cu-Gd mother alloy that obtains at pressure difference P=P
1+ P
2Effect under spray in the copper mold die cavity, obtain the Mg of diameter 2mm
62Zn
3Cu
25Gd
10The block amorphous alloy sample.
Adopt the weave construction of X-ray diffraction method sign gained sample, as shown in Figure 1.By " the steamed bun peak " of the general demonstration of XRD figure of this sample as can be known, the typical non-crystal structure feature of the internal structure tool of gained sample illustrates that this alloy sample is non-crystaline amorphous metal.
Adopt the amorphous formation ability of DSC curve sign gained sample, as shown in Figure 2.By its DSC curve as can be known, the glass transformation temperature T of gained sample
g, initial crystallization temperature T
xWith supercooling liquid phase region Δ T
x(Δ T
x=T
x-T
g) value be respectively 439K, 501K, 62K illustrates that the gained sample has strong amorphous formation ability.
Utilize the compressed rupture strength of Instron4505 type electronic universal tester test non-crystaline amorphous metal sample to characterize its mechanical property, compressive strain speed is 2 * 10
-4s
-1, as shown in Figure 3.As seen from the figure, the final compressed rupture strength of gained sample is 698MPa, higher than Mg
65Cu
25Gd
10The 648MPa of ternary block amorphous alloy sample.
Utilize the hardness value of HXS-1000Z type hardness tester instrumentation amount sample, as shown in Figure 4.Result shows that the microhardness of gained non-crystaline amorphous metal sample has reached 255Hv, with Mg
65Cu
25Gd
10The 257Hv of ternary block amorphous alloy sample is suitable.
Select preparation x=5, be divided into Mg
60Zn
5Cu
25Gd
10Block amorphous alloy, sample diameter is 2mm.
Step 1: the preparation of mother alloy: be that 99.9% high-purity MAG block, purity are that 99.9% spelter, purity are that high-purity copper ingot of 99.8% and purity are that high-purity gadolinium piece of 99.99% is by composition proportion Mg with purity
60Zn
5Cu
25Gd
10Take raw material; At first alloy raw material Cu and Gd are put into quartz test tube, be placed on the ruhmkorff coil center of induction melting furnace, avoid contacting with coil, close fire door, then be evacuated to 10
-4Pa is filled with 10
-2The argon gas of Pa, repeatedly after three times under argon shield molten alloy, even for making alloying constituent, with alloy melt back 3～5 times, make the Cu-Gd master alloy.Then with Cu-Gd master alloy sanding and polishing, pulverize heel purity and be 99.9% MAG block and purity and be 99.9% spelter and mix, make the Mg-Zn-Cu-Gd mother alloy with identical melting method at last.
Step 2: non-crystaline amorphous metal sample preparation: the Mg-Zn-Cu-Gd mother alloy sanding and polishing that step 1 is made, to remove the oxide skin on mother alloy surface, with ultrasonic oscillator, it is cleaned, in the quartz test tube of packing into after the mother alloy pulverizing, be placed on the ruhmkorff coil center of induction melting furnace, avoid contacting with coil; Closing fire door, is P toward the interior charged pressure of quartz test tube upper end gas-holder
1(5 * 10
-2Pa) high-purity argon gas is filled with 5 * 10 after pumping high vacuum repeatedly with furnace chamber
-2The argon shield gas of Pa forms P
2Negative pressure, the above-mentioned mother alloy of remelting in the intermediate frequency vacuum induction melting furnace of argon gas atmosphere, with the molten state Mg-Zn-Cu-Gd mother alloy that obtains at pressure difference P=P
1+ P
2Effect under spray in the copper mold die cavity, obtain the Mg of diameter 2mm
60Zn
5Cu
25Gd
10The block amorphous alloy sample.
Adopt the weave construction of X-ray diffraction method sign gained sample, as shown in Figure 1.By " the steamed bun peak " of the general demonstration of XRD figure of this sample as can be known, the typical non-crystal structure feature of the internal structure tool of gained sample illustrates that this alloy sample is non-crystaline amorphous metal.
Adopt the amorphous formation ability of DSC curve sign gained sample, as shown in Figure 2.By its DSC curve as can be known, the glass transformation temperature T of gained sample
g, initial crystallization temperature T
xWith supercooling liquid phase region Δ T
x(Δ T
x=T
x-T
g) value be respectively 445K, 499K, 54K illustrates that the gained sample has strong amorphous formation ability.
Utilize the compressed rupture strength of Instron4505 type electronic universal tester test non-crystaline amorphous metal sample to characterize its mechanical property, compressive strain speed is 2 * 10
-4s
-1, as shown in Figure 3.As seen from the figure, the final compressed rupture strength of gained sample is 754MPa, far above Mg
65Cu
25Gd
10The 648MPa of ternary block amorphous alloy sample.。
Utilize the hardness value of HXS-1000Z type hardness tester instrumentation amount sample, as shown in Figure 4.Result shows that the microhardness of gained non-crystaline amorphous metal sample has reached 286Hv, apparently higher than Mg
65Cu
25Gd
10The 257Hv of ternary block amorphous alloy sample.
Claims (2)
1. Mg-Cu-Gd block amorphous alloy that contains Zn, it is characterized in that: nominal composition is Mg
65-xZn
xCu
25Gd
10, x=3 wherein, 5,8at. ﹪.
2. preparation method who contains the Mg-Cu-Gd block amorphous alloy of Zn is characterized in that:
(1), the preparation of mother alloy: be that 99.9% MAG block, purity are that 99.9% spelter, purity are that 99.8% copper ingot and purity are that 99.99% gadolinium piece is by nominal composition Mg with purity
65-xZn
xCu
25Gd
10Batching, x=3 wherein, 5,8at. ﹪; At first copper ingot and gadolinium piece raw material are put into quartz test tube, be placed in induction melting furnace ruhmkorff coil center, close fire door, then be evacuated to 10
-4Pa is filled with 10
-2The argon gas of Pa carries out the melting of Cu-Gd master alloy with the method for vacuum induction melting under argon shield; Then with Cu-Gd master alloy sanding and polishing, mix with MAG block and spelter after pulverizing, use the melting method identical with the melting of Cu-Gd master alloy to prepare the Mg-Zn-Cu-Gd mother alloy;
(2), non-crystaline amorphous metal sample preparation: with the Mg-Zn-Cu-Gd mother alloy sanding and polishing that makes, with ultrasonic oscillator, it is cleaned, in the quartz test tube of packing into after pulverizing, be placed in the ruhmkorff coil center of induction melting furnace, closing fire door, is P toward the interior charged pressure of quartz test tube upper end gas-holder
1High-purity argon gas, P
1=5 * 10
-2Pa is filled with 5 * 10 after pumping high vacuum repeatedly with furnace chamber
-2The argon shield gas of Pa forms P
2Negative pressure, remelting mother alloy in the intermediate frequency vacuum induction melting furnace of argon gas atmosphere, with the molten state Mg-Zn-Cu-Gd mother alloy that obtains at pressure difference P=P
1+ P
2Effect under spray in the copper mold die cavity, obtain the Mg-Zn-Cu-Gd block amorphous alloy.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105382224A (en) * | 2015-11-27 | 2016-03-09 | 济南大学 | Method for manufacturing amorphous alloy thin strip through Mg-Zn-Gd quasi-crystal alloy |
| CN111321358A (en) * | 2020-04-17 | 2020-06-23 | 中国科学院物理研究所 | Amorphous alloy with spontaneous color change on surface, and preparation method and application thereof |
| CN111748752A (en) * | 2020-06-10 | 2020-10-09 | 中国航发北京航空材料研究院 | Magnesium-based amorphous alloy for fracturing ball and preparation method of fracturing ball |
| CN112466409A (en) * | 2020-11-19 | 2021-03-09 | 江苏科技大学 | Five-element high-entropy amorphous alloy component design method based on combination of two quaternary amorphous alloy elements |
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| CN1403617A (en) * | 2001-09-13 | 2003-03-19 | 中国科学院金属研究所 | Multicomponent magnesium-base amorphous alloy containing zinc element |
| CN101880840A (en) * | 2010-07-02 | 2010-11-10 | 哈尔滨工程大学 | Preparation method of Mg-Li matrix Mg-Li-Cu-Ni-Y series bulk amorphous alloy |
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2013
- 2013-03-22 CN CN2013100949661A patent/CN103173699A/en active Pending
Patent Citations (2)
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| CN1403617A (en) * | 2001-09-13 | 2003-03-19 | 中国科学院金属研究所 | Multicomponent magnesium-base amorphous alloy containing zinc element |
| CN101880840A (en) * | 2010-07-02 | 2010-11-10 | 哈尔滨工程大学 | Preparation method of Mg-Li matrix Mg-Li-Cu-Ni-Y series bulk amorphous alloy |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105382224A (en) * | 2015-11-27 | 2016-03-09 | 济南大学 | Method for manufacturing amorphous alloy thin strip through Mg-Zn-Gd quasi-crystal alloy |
| CN111321358A (en) * | 2020-04-17 | 2020-06-23 | 中国科学院物理研究所 | Amorphous alloy with spontaneous color change on surface, and preparation method and application thereof |
| CN111748752A (en) * | 2020-06-10 | 2020-10-09 | 中国航发北京航空材料研究院 | Magnesium-based amorphous alloy for fracturing ball and preparation method of fracturing ball |
| CN111748752B (en) * | 2020-06-10 | 2021-12-03 | 中国航发北京航空材料研究院 | Magnesium-based amorphous alloy for fracturing ball and preparation method of fracturing ball |
| CN112466409A (en) * | 2020-11-19 | 2021-03-09 | 江苏科技大学 | Five-element high-entropy amorphous alloy component design method based on combination of two quaternary amorphous alloy elements |
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Application publication date: 20130626 |