CN101928895A - Gd-Co-Al massive metal glass with favorable amorphous forming ability and preparation method thereof - Google Patents
Gd-Co-Al massive metal glass with favorable amorphous forming ability and preparation method thereof Download PDFInfo
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- CN101928895A CN101928895A CN2009103041110A CN200910304111A CN101928895A CN 101928895 A CN101928895 A CN 101928895A CN 2009103041110 A CN2009103041110 A CN 2009103041110A CN 200910304111 A CN200910304111 A CN 200910304111A CN 101928895 A CN101928895 A CN 101928895A
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Abstract
The invention provides a rare-earth gadolinium-base massive metal glass with favorable amorphous forming ability and a preparation method thereof, belonging to the field of metal material science and technology. The gadolinium-base massive metal glass comprises the following components by atom percent: 52.5-53.8% of gadolinium, 16.5-20.5% of cobalt and 25.7-31.0% of aluminum. The invention also provides the preparation method of the gadolinium-base massive metal glass, which comprises the following steps: mixing gadolinium, cobalt and aluminum according to the atom percent, arc-melting until the alloy is evenly molten to obtain Gd-Co-Al mother alloy cast ingots, carrying out copper mold suction casting to obtain massive metal glass of which the maximum diameter is 4 millimeters. The gadolinium-base massive metal glass has favorable amorphous forming ability and high thermal stability, and has wide application prospects in the fields of magnetic refrigeration functional materials and structural materials.
Description
Technical field
The present invention relates to bulk-metallic glass, particularly is bulk-metallic glass of matrix and preparation method thereof with the rare earth.
Background technology
Bulk-metallic glass typically refers to three-dimensional dimension all greater than the block amorphous alloy of 1mm, is different to adopt fast quenching to get rid of the amorphous thin ribbon of band method preparation.Bulk-metallic glass has excellent mechanical property, all has than corresponding crystal alloy at aspects such as intensity, hardness, anti-corrosion, wear resisting propertys better to show.As Zr
41.2Ti
13.8Cu
12.5Ni
10Be
22.5(commercial trade mark Vit-1) alloy tensile strength at room temperature is up to 1.9GPa, and the recoverable deformation before the fracture reaches 2%.
Rare earth element has physicalies such as abundant magnetic, heat, sound, light, electricity, thereby makes the rare earth based alloy have abundant application prospect.Studies show that in recent years, the rare earth based bulk-metallic glass is as Gd
53Al
24Co
20Zr
3, Ho
30Y
26Al
24Co
20, Er
50Al
24Co
20Y
6Deng, have big magnetic entropy to become and relative refrigerating duty, be suitable as very much magnetic refrigerating working medium and use.To further promote of the application of rare earth based bulk-metallic glass, also must continue to improve the amorphous formation ability of alloy, prepare larger sized non-crystaline amorphous metal at the magnetic refrigerating field.Literature search shows, DingChen etc. are at " Materials Science andEngineering A " (" Materials Science and Engineering A ", 2008 457 the volume 226～230 pages) on delivered the article that is entitled as Gd-Co-Al and Gd-Ni-Al bulk metallic glasses with high glass forming ability andgood mechanical properties (Gd-Co-Al and Gd-Ni-Al bulk-metallic glass) with high glass forming ability and good mechanical properties, propose to adopt the method (injection casting) of spray up n., composition is Gd
60Co
25Al
15Alloy to form large block amorphous greatest circle column diameter be 5mm.Yet this breadboard studies show that of applicant place is adopted suction casting method (suck casting), Gd
60Co
25Al
15The maximum critical diameter that alloy forms bulk-metallic glass has only 2mm.Therefore, seeking the alloying constituent with better amorphous formation ability in the Gd-Co-Al system has very important significance.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of Gd-Co-Al (gadolinium-cobalt-aluminium) Alloy And Preparation Method with better amorphous formation ability and thermostability is provided, make it be more suitable for using as magnetic refrigerating working medium.
The objective of the invention is to be achieved through the following technical solutions, be specially: the method by arc melting is even until alloy melting, obtain the mother alloy ingot of Gd-Co-Al, adopting copper mold casting to obtain maximum diameter then is 4 millimeters bulk-metallic glass.
Gd-Co-Al bulk-metallic glass with good amorphous formation ability of the present invention, it comprises component and atomic percent is: 52.5～53.8%Gd, 16.5～20.5%Co, 25.7～31.0%Al.
Gd-Co-Al bulk-metallic glass of the present invention, it comprises component and atomic percent is preferably: 53.8%Gd, 17.3%Co, 28.9%Al.
Gd-Co-Al bulk-metallic glass of the present invention, it comprises component and atomic percent also can be: 52.5%Gd, 16.5%Co, 31%Al.
Gd-Co-Al bulk-metallic glass of the present invention, its maximum diameter are 4 millimeters, and maximum supercooling liquid phase region width is 79K.
The preparation method of Gd-Co-Al bulk-metallic glass of the present invention, it comprises following steps:
(1) presses Gd
52.5～53.8Co
16.5～20.5Al
25.7～31.0The chemical formula weighing; Wherein Gd, Co, Al purity of raw materials are more than 99.5% (mass percent);
(2) will be set by step (1) raw material of preparing put into non-consumable arc furnace, be evacuated to 3 * 10
-5More than the torr; After high-purity argon gas purging method cleaning 1～2 time, the melting 4～6 times of overturning repeatedly under 1 atmospheric high-purity argon gas protection is till smelting temperature melts with raw material;
(3) will be set by step (2) melted mother alloy put into vacuum arc fumace and inhale the cast copper crucible, cast cylindric sample with inhaling behind the alloy melting.
The invention has the advantages that: Gd-Co-Al bulk-metallic glass provided by the present invention, i.e. Gd
52.5～53.8, Co
16.5～ 20.5Al
25.7～31.0Alloy, can form maximum critical diameter in this alloy system is the single non-crystal structure of 4mm, and has higher thermostability, the supercooling liquid phase region width is up to 79K.This is that the through engineering approaches of alloy is used and to be laid a good foundation for this.
The preparation method of Gd-Co-Al bulk amorphous alloys provided by the invention has that preparation technology is simple, the material microstructure structure is advantages such as single non-crystal structure.
Description of drawings
Fig. 1 is the Gd of the embodiment of the invention 1,2,3,4,5 preparations
53.8Co
20.5Al
25.7, Gd
53.8Co
17.3Al
28.9, Gd
53.5Co
18.0Al
28.5, Gd
53.0Co
20.0Al
27.0, Gd
52.5Co
16.5Al
31.0The X-ray diffraction spectrum of bulk-metallic glass;
Fig. 2 is the Gd of the embodiment of the invention 2 preparations
53.8Co
17.3Al
28.9The high resolution transmission electron microscopy photo of bulk-metallic glass;
Fig. 3 is the Gd of the embodiment of the invention 1,2,3,4,5 preparations
53.8Co
17.3Al
28.9, Gd
53.5Co
18.0Al
28.5, Gd
53.0Co
20.0Al
27.0, Gd
52.5Co
16.5Al
31.0The differential thermal analysis curve of bulk-metallic glass;
Fig. 4 is the Gd of the embodiment of the invention 5 preparations
52.5Co
16.5Al
31.0Alloy magnetic entropy change under 0～5 tesla's changes of magnetic field varies with temperature curve;
Embodiment
Embodiment 1Gd
53.8Co
20.5Al
25.7The preparation of bulk-metallic glass and thermostability
Purity is pressed Gd greater than gadolinium, cobalt, the aluminum feedstock of 99.5% (massfraction)
53.8Co
20.5Al
25.7The chemical formula weighing is put into non-consumable arc furnace with the raw material for preparing, and is evacuated to 3 * 10
-5More than the torr; After high-purity argon gas purging method cleaning 1～2 time, the melting of overturning repeatedly under 1 atmospheric high-purity argon gas protection is made mother alloy 4～6 times; To put into vacuum arc fumace by the melted mother alloy of above-mentioned steps and inhale the cast copper crucible, to cast diameter be 3 millimeters cylindrical sample with inhaling behind the alloy melting.X-ray diffraction analysis shows does not find any crystalline diffraction peak in the alloy diffraction spectra, illustrate that alloy is made up of amorphous phase.Differential scanning calorimetry shows the second-order transition temperature (T of alloy
g) be 334 degrees centigrade, the initial crystallization temperature (T of alloy
x) be 399 degrees centigrade, supercooling liquid phase region width (the Δ T=T of alloy
x-T
g) be 65 degrees centigrade.
Embodiment 2Gd
53.8Co
17.3Al
28.9The preparation of bulk-metallic glass and thermostability
Purity is pressed Gd greater than gadolinium, cobalt, the aluminum feedstock of 99.5% (massfraction)
53.8Co
17.3Al
28.9The chemical formula weighing is put into non-consumable arc furnace with the raw material for preparing, and is evacuated to 3 * 10
-5More than the torr; After high-purity argon gas purging method cleaning 1～2 time, the melting of overturning repeatedly under 1 atmospheric high-purity argon gas protection is made mother alloy 4～6 times; To put into vacuum arc fumace by the melted mother alloy of above-mentioned steps and inhale the cast copper crucible, to cast diameter be 4 millimeters cylindrical sample with inhaling behind the alloy melting.X-ray diffraction analysis shows does not find any crystalline diffraction peak in the alloy diffraction spectra, illustrate that alloy is made up of amorphous phase.The high-resolution-ration transmission electric-lens analysis revealed, atom is random arrangement in the alloy, does not find any crystal mutually and ordered structure, confirms that further alloy is made up of amorphous phase.Differential scanning calorimetry shows the second-order transition temperature (T of alloy
g) be 332 degrees centigrade, the initial crystallization temperature (T of alloy
x) be 411 degrees centigrade, supercooling liquid phase region width (the Δ T=T of alloy
x-T
g) be 79 degrees centigrade.
Embodiment 3Gd
53.5Co
18.0Al
28.5The preparation of bulk-metallic glass and thermostability
Purity is pressed Gd greater than gadolinium, cobalt, the aluminum feedstock of 99.5% (massfraction)
53.5Co
18.0Al
28.5The chemical formula weighing is put into non-consumable arc furnace with the raw material for preparing, and is evacuated to 3 * 10
-5More than the torr; After high-purity argon gas purging method cleaning 1～2 time, the melting of overturning repeatedly under 1 atmospheric high-purity argon gas protection is made mother alloy 4～6 times; To put into vacuum arc fumace by the melted mother alloy of above-mentioned steps and inhale the cast copper crucible, to cast diameter be 3 millimeters cylindrical sample with inhaling behind the alloy melting.X-ray diffraction analysis shows does not find any crystalline diffraction peak in the alloy diffraction spectra, illustrate that alloy is made up of amorphous phase.Differential scanning calorimetry shows the second-order transition temperature (T of alloy
g) be 332 degrees centigrade, the initial crystallization temperature (T of alloy
x) be 407 degrees centigrade, supercooling liquid phase region width (the Δ T=T of alloy
x-T
g) be 75 degrees centigrade.
Embodiment 4Gd
53.0Co
20.0Al
27.0The preparation of bulk-metallic glass and thermostability
Purity is pressed Gd greater than gadolinium, cobalt, the aluminum feedstock of 99.5% (massfraction)
53.0Co
20.0Al
27.0The chemical formula weighing is put into non-consumable arc furnace with the raw material for preparing, and is evacuated to 3 * 10
-5More than the torr; After high-purity argon gas purging method cleaning 1～2 time, the melting of overturning repeatedly under 1 atmospheric high-purity argon gas protection is made mother alloy 4～6 times; To put into vacuum arc fumace by the melted mother alloy of above-mentioned steps and inhale the cast copper crucible, to cast diameter be 3 millimeters cylindrical sample with inhaling behind the alloy melting.X-ray diffraction analysis shows does not find any crystalline diffraction peak in the alloy diffraction spectra, illustrate that alloy is made up of amorphous phase.Differential scanning calorimetry shows the second-order transition temperature (T of alloy
g) be 328 degrees centigrade, the initial crystallization temperature (T of alloy
x) be 400 degrees centigrade, supercooling liquid phase region width (the Δ T=T of alloy
x-T
g) be 72 degrees centigrade.
Embodiment 5Gd
52.5Co
16.5Al
31.0The preparation of bulk-metallic glass and thermostability
Purity is pressed Gd greater than gadolinium, cobalt, the aluminum feedstock of 99.5% (massfraction)
52.5Co
16.5Al
31.0The chemical formula weighing is put into non-consumable arc furnace with the raw material for preparing, and is evacuated to 3 * 10
-5More than the torr; After high-purity argon gas purging method cleaning 1～2 time, the melting of overturning repeatedly under 1 atmospheric high-purity argon gas protection is made mother alloy 4～6 times; To put into vacuum arc fumace by the melted mother alloy of above-mentioned steps and inhale the cast copper crucible, to cast diameter be 4 millimeters cylindrical sample with inhaling behind the alloy melting.X-ray diffraction analysis shows does not find any crystalline diffraction peak in the alloy diffraction spectra, illustrate that alloy is made up of amorphous phase.Differential scanning calorimetry shows the second-order transition temperature (T of alloy
g) be 328 degrees centigrade, the initial crystallization temperature (T of alloy
x) be 398 degrees centigrade, supercooling liquid phase region width (the Δ T=T of alloy
x-T
g) be 70 degrees centigrade.Magnetic Measurement shows, Gd
52.5Co
16.5Al
31.0The Curie temperature of bulk-metallic glass is 95K, and the maximum magnetic entropy variable of alloy under 0～5 tesla's changes of magnetic field is 9.8Jkg
-1K
-1, the relative refrigerating duty of alloy is 9.1? 0
2J/kg.Being highly suitable near the 95K the most, magnetic refrigerating working medium uses.
The present invention has prepared a series of Gd-Co-Al bulk-metallic glass, and its associated hot thing parameter is listed in table 1.
The hot thing parameter of table 1 Gd-Co-Al bulk-metallic glass
| The embodiment numbering | Critical diameter (mm) | Second-order transition temperature (℃) | Initial crystallization temperature (℃) | The supercooling liquid phase region width (℃) |
| 1 | 3 | 334 | 399 | 65 |
| 2 | 4 | 332 | 411 | 79 |
| 3 | 3 | 332 | 407 | 75 |
| 4 | 3 | 328 | 400 | 72 |
| 5 | 4 | 328 | 398 | 70 |
| Comparative example (Gd 55Co 15Al 30) | 2 | 278 | 308 | 30 |
Claims (5)
1. Gd-Co-Al bulk-metallic glass with good amorphous formation ability is characterized in that comprising component and atomic percent thereof and is: 52.5～53.8%Gd, 16.5～20.5%Co, 25.7～31.0%Al.
2. Gd-Co-Al bulk-metallic glass according to claim 1 is characterized in that comprising component and atomic percent thereof and is: 53.8%Gd, 17.3%Co, 28.9%Al.
3. Gd-Co-Al bulk-metallic glass according to claim 1 is characterized in that comprising component and atomic percent thereof and is: 52.5%Gd, 16.5%Co, 31%Al.
4. by the arbitrary described Gd-Co-Al bulk-metallic glass of claim 1 to 3, it is characterized in that described bulk-metallic glass maximum diameter is 4 millimeters, maximum supercooling liquid phase region width is 79K.
5. according to the preparation method of the described Gd-Co-Al bulk-metallic glass of claim 1, it is characterized in that comprising following steps:
(1) presses Gd52.5～53.8Co16.5～20.5Al25.7～31.0 chemical formula weighings; Wherein Gd, Co, Al purity of raw materials are more than 99.5% (mass percent);
(2) will be set by step (1) raw material of preparing put into non-consumable arc furnace, be evacuated to more than 3 * 10-5 torr; After high-purity argon gas purging method cleaning 1～2 time, the melting 4～6 times of overturning repeatedly under 1 atmospheric high-purity argon gas protection is till smelting temperature melts with raw material;
(3) will be set by step (2) melted mother alloy put into vacuum arc fumace and inhale the cast copper crucible, cast cylindric sample with inhaling behind the alloy melting.
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102328902A (en) * | 2011-08-26 | 2012-01-25 | 华中科技大学 | Method for preparing surface microstructure of super-hydrophobic amorphous alloy |
| CN103031478A (en) * | 2012-12-12 | 2013-04-10 | 电子科技大学 | In-situ complex-phase gadolinium-based magnetic refrigeration material having magnetic entropy change platform and preparation method thereof |
| CN112342475A (en) * | 2020-10-13 | 2021-02-09 | 东南大学 | Microalloyed heavy rare earth based amorphous alloy and preparation method and application thereof |
-
2009
- 2009-07-08 CN CN2009103041110A patent/CN101928895A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102328902A (en) * | 2011-08-26 | 2012-01-25 | 华中科技大学 | Method for preparing surface microstructure of super-hydrophobic amorphous alloy |
| CN102328902B (en) * | 2011-08-26 | 2014-06-18 | 华中科技大学 | Method for preparing surface microstructure of super-hydrophobic amorphous alloy |
| CN103031478A (en) * | 2012-12-12 | 2013-04-10 | 电子科技大学 | In-situ complex-phase gadolinium-based magnetic refrigeration material having magnetic entropy change platform and preparation method thereof |
| CN112342475A (en) * | 2020-10-13 | 2021-02-09 | 东南大学 | Microalloyed heavy rare earth based amorphous alloy and preparation method and application thereof |
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Open date: 20101229 |