CN102808139A - Method for preparing magnesium-base amorphous alloy strip - Google Patents
Method for preparing magnesium-base amorphous alloy strip Download PDFInfo
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- CN102808139A CN102808139A CN2012102106656A CN201210210665A CN102808139A CN 102808139 A CN102808139 A CN 102808139A CN 2012102106656 A CN2012102106656 A CN 2012102106656A CN 201210210665 A CN201210210665 A CN 201210210665A CN 102808139 A CN102808139 A CN 102808139A
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Abstract
The invention relates to a method for preparing a magnesium-base amorphous alloy strip, and belongs to the technical field of magnesium-base amorphous alloy strips. The method is characterized by comprising the following steps of: preparing Cu-Al-Y intermediate alloy on a vacuum magnetic control tungsten electrode electric-arc furnace according to the atomic percentage of (25-x) percent of Cu, x (x is equal to 1, 3 and 5) percent of Al and 10 percent of Y (the purity is over 99.95 percent); smelting master alloy by using a resistance furnace, namely adding magnesium (the purity is over 99.95 percent) according to the atomic percentage of 65 percent, and putting the magnesium and the molten Cu-Al-Y intermediate alloy into the resistance furnace, keeping temperature of 760 DEG C for 2 hours, and pouring the magnesium and the molten Cu-Al-Y intermediate alloy in a wedge-shaped copper die of which the thickness is 0 to 7 millimeters and the width is 60 millimeters respectively to prepare Mg-Cu-Al-Y master alloy with three ingredients; and preparing the amorphous thin strip by using a high vacuum single-roller rotary quenching and electric arc melting vacuum suction casting system, putting the Mg-Cu-Al-Y master alloy into a quartz glass tube of which the lower end is provided with a spray nozzle, adjusting distance between the spray nozzle and a copper roller, closing a cabin door, vacuumizing to 1.0*10<-3>Pa, and preparing a strip sample by using a single-roller rotary quenching method.
Description
Technical field
The invention belongs to magnesium base band non-crystaline amorphous metal preparing technical field, refer in particular to a kind of preparation method of magnesium base band non-crystaline amorphous metal.
Background technology
Amorphous alloy at home and abroad has been subjected to more and more widely and has paid attention to as a kind of novel material.Since obtaining amorphous alloy for the first time, it is attracting different field ground scientific research personnel such as physics, metallurgy and materialogy ground all angles from basic science to the applied science that it is carried out comprehensive research always.It constantly develops with innovation is not only to have great scientific meaning owing to disclose non-crystalline solids ground physical essence; More importantly still be because amorphous alloy has very excellent ground physics, chemistry, mechanical property, and these performances often are that existing metallic substance is not available.In addition, the preparation technology of amorphous alloy is relatively simple, it with short production cycle, equipment is not huge, therefore, sees from industrial angle, above-mentioned advantage also is that it can develop the favorable factor of serving economic construction rapidly.
The exploitation of magnesium-base amorphous alloy is on the basis of Mg-Cu-Y ternary system, to grow up, and has developed the magnesium-base amorphous alloy system of multiple quaternary and five yuan through 10 years of development people.Though over past ten years people research has obtained breakthrough progress to magnesium-base amorphous alloy, nobody research Mg-Cu-Al-Y amorphous alloy also at present.The present invention adds a spot of Al element on the basis of Mg-Cu-Y ternary system, utilize single roller to get rid of the band method and prepare Mg
65Cu
21Al
1Y
10, Mg
65Cu
22Al
3Y
10And Mg
65Cu
20Al
5Y
10Three kinds of composition amorphous ribbons improve the mechanical property of non-crystaline amorphous metal and reduce its fragility with it; And adopt X-ray diffraction analysis method (XRD) and combine differential thermal analysis (DSC) that three kinds of amorphous ribbons are analyzed.
Summary of the invention
The present invention develops a kind of preparation method of magnesium base band non-crystaline amorphous metal; It is characterized by: at first prepare the Cu-Al-Y master alloy; According to Cu, Al, Y (purity is more than 99.95%) atomic percent is Cu (25-x) %, Al x% (x=1,3 and 5), and Y10% is formulated.The melting of Cu-Al-Y master alloy is on the vacuum magnetic control tungsten electrode arc furnace, to carry out.The Cu-Y-Al master alloy for preparing is placed in the stove, be evacuated to and be lower than 3.0 * 10
-3Pa charges into the shielding gas argon gas to 0.06MPa, melting 50~90s under 400~500A current condition, each intermediate alloy ingot (about 25g) melt back 4~5 times.Melted master alloy is used sharpening machine ground surface zone of oxidation, then each intermediate alloy ingot is smashed into fritter, and use straight alcohol to clean.Pure Mg piece is sawn into fritter by hand, cleans up in the cleaned by ultrasonic vibration machine with acetone, and weighing is accurate then.
The resistance furnace melting is adopted in the mother alloy melting, does not react in order to ensure crucible and starting material, and crucible material uses soft steel.Isolated in order to ensure starting material and air, crucible cover (can conveniently promote) leaves argon gas ventpipe and escape pipe, and the crucible seal inside is good.The preceding crucible inside and outside wall evenly is coated with of melting brushes foundry facing, and places 200 ℃ of bakers to dry.The mother alloy smelting temperature is 760 ℃, and in crucible bottom, Mg is 65% adding by atomic percent with the MAG block of handling well (purity is more than 99.95%) tiling one deck; The Cu-Y-Al master alloy evenly is tiled on the Mg piece; To remain MAG block again and be tiled on the Cu-Y-Al master alloy, form Mg-alloy-Mg lamination, can guarantee the alloy thorough mixing like this; Prevent that master alloy from burning mistake, obtains the uniform mother alloy of composition.Crucible is fed argon gas to 0.06MP, about 760 ℃ of meltings of temperature half hours that the flat gently rolling of crucible is several down, make molten metal evenly mixed, water after 2 hours 760 ℃ of temperature insulations then and cast from the copper mold.3 kinds of composition alloys, i.e. Mg have been prepared
65Cu
24Al
1Y
10, Mg
65Cu
22Al
3Y
10, Mg
65Cu
20Al
5Y
10, be cast in respectively in the wedge shape copper mold of thickness 0~7mm, wide 60mm, prepare mother alloy.
The single roller of amorphous thin ribbon preparation employing high vacuum revolves to be quenched and arc melting suction pouring system; The Mg-Cu-Al-Y mother alloy is polished off surface oxide layer and knock fritter; Use straight alcohol to clean clean oven dry, place the lower end that the quartz glass tube of being with nozzle is arranged then, the distance between adjustment nozzle and copper roller; The sealing hatch door is evacuated to 1.0 * 10
-3Pa revolves the legal system of quenching with single roller and gets the bar carry sample.Selected preferable processing parameter is after repeatedly manufacturing experimently: the silica tube nozzle bore is 3mm * 0.3mm.0.04MPa, copper roller rotating speed 30m/s are pressed in the argon gas spray.
Prepare Mg
65Cu
24Al
1Y
10, Mg
65Cu
22Al
3Y
10, Mg
65Cu
20Al
5Y
10Three kinds of composition alloy strips, prepared beam thickness are 70~80 μ m.Sample is long and continuously, it is bright and clean to paste roll surface, complete copy the surface characteristic of copper roller, free surface is than copper-surfaced roller surface-brightening, it is as shown in Figure 1 that band has certain toughness.
Fig. 2 is Mg
65Cu
21Al
1Y
10, Mg
65Cu
22Al
3Y
10, Mg
65Cu
20Al
55Y
10Three kinds of composition alloy strip X-ray diffraction patterns.When the electronic action in all atoms in X scattering and the crystal, can all directions produce scattering in the space under certain condition.Because atom is periodic arrangement in the space, thereby these are scattered in some space stack and enhancing is interfered in generation, form diffraction peak.For amorphous, the atom spatial disposition is random, so there is not characteristic diffraction peak.But, can form non-crystalline state diffraction maize, i.e. the steamed bun peak because the existence of short range order makes in the range of diffraction of low angle, still to have property according to qualifications.Visible by Fig. 2, near 2 θ=37 °, three kinds of compositions all show as the typical diffuse diffraction of amorphous phase peak, do not have tangible crystalline state peak and occur, and this alloy thin band that shows three kinds of compositions has all formed complete amorphous phase.
Fig. 3. middle (a) and (b) with (c) be respectively Mg
65Cu
21Al
1Y
10, Mg
65Cu
22Al
3Y
10And Mg
65Cu
20Al
5Y
10The DSC detection curve of three kinds of composition amorphous ribbons.Can know Mg by figure
65Cu
24Al
1Y
10The glass transformation temperature Tg of non-crystaline amorphous metal, crystallization temperature Tp1, solidus temperature Tm, temperature of fusion is respectively 142.1 ℃, 204.3 ℃, 457 ℃ and 465.4 ℃; Mg
65Cu
22Al
3Y
10The Tg of non-crystaline amorphous metal, Tp1, Tm, temperature of fusion is respectively 138.7 ℃, 185.6 ℃, 431.0 ℃ and 452.4 ℃; Mg
65Cu
20Al
5Y
10The Tg of non-crystaline amorphous metal, Tp1, Tm, temperature of fusion is respectively 141.5 ℃, 194.4 ℃, 422 ℃ and 445.3 ℃.
Description of drawings
The amorphous ribbon of Fig. 1 preparation (on: the free surface; Down: paste and roll roll surface)
Fig. 2 band Mg
65Cu
24Al
1Y
10, Mg
65Cu
22Al
3Y
10, Mg
65Cu
20Al
5Y
10The X-ray diffraction spectrum of alloy
Fig. 3 band Mg
65Cu
24Al
1Y
10, Mg
65Cu
22Al
3Y
10, Mg
65Cu
20Al
5Y
10The DSC of alloy detects
Embodiment
Embodiment 1
At first preparing the Cu-Al-Y master alloy, is Cu24% according to Cu, Al, Y atomic percent, Al1%, and Y10% is formulated.The melting of Cu-Al-Y master alloy is on the vacuum magnetic control tungsten electrode arc furnace, to carry out.The Cu-Y-Al master alloy for preparing is placed in the stove, be evacuated to and be lower than 3.0 * 10
-3Pa charges into the shielding gas argon gas to 0.06MPa, melting 50~90s under 400~500A current condition, each intermediate alloy ingot (about 25g) melt back 4~5 times.Melted master alloy is used sharpening machine ground surface zone of oxidation, then each intermediate alloy ingot is smashed into fritter, and use straight alcohol to clean.Pure Mg piece is sawn into fritter by hand, cleans up in the cleaned by ultrasonic vibration machine with acetone, and weighing is accurate then.
The resistance furnace melting is adopted in the mother alloy melting, does not react in order to ensure crucible and starting material, and crucible material uses soft steel.Isolated in order to ensure starting material and air, crucible cover (can conveniently promote) leaves argon gas ventpipe and escape pipe, and the crucible seal inside is good.The preceding crucible inside and outside wall evenly is coated with of melting brushes foundry facing, and places 200 ℃ of bakers to dry.The mother alloy smelting temperature is 760 ℃, and in crucible bottom, magnesium is 65% adding by atomic percent with Mg piece tiling one deck of handling well; The Cu-Y-Al master alloy evenly is tiled on the Mg piece; To remain the Mg piece again and be tiled on the Cu-Y-Al master alloy, form Mg-alloy-Mg lamination, can guarantee the alloy thorough mixing like this; Prevent that master alloy from burning mistake, obtains the uniform mother alloy of composition.Crucible is fed argon gas to 0.06MP, about 760 ℃ of meltings of temperature half hours that the flat gently rolling of crucible is several down, make molten metal evenly mixed, water after 2 hours 760 ℃ of temperature insulations then and cast from the copper mold.Prepared Mg
65Cu
24Al
1Y
10, be cast in respectively in the wedge shape copper mold of thickness 0~7mm, wide 60mm, prepare mother alloy.
The single roller of amorphous thin ribbon preparation employing high vacuum revolves to be quenched and arc melting suction pouring system, with Mg
65Cu
24Al
1Y
10Mother alloy polishes off surface oxide layer and knock fritter, uses straight alcohol to clean clean oven dry, places the lower end that the quartz glass tube of being with nozzle is arranged then, the distance between adjustment nozzle and copper roller, and the sealing hatch door is evacuated to 1.0 * 10
-3Pa revolves the legal system of quenching with single roller and gets the bar carry sample.Selected preferable processing parameter is after repeatedly manufacturing experimently: the silica tube nozzle bore is that 0.04MPa, copper roller rotating speed 30m/s are pressed in 3mm * 0.3mm, argon gas spray.
Embodiment 2
According to Cu, Al, Y atomic percent is Cu22%, Al3%, and Y10% is formulated.All process methodes are pressed embodiment 1.
According to Cu, Al, Y atomic percent is Cu20%, A15%, and Y10% is formulated.All process methodes are pressed embodiment 1.
Claims (2)
1. the preparation method of a magnesium base band non-crystaline amorphous metal; It is characterized by: at first prepare the Cu-Al-Y master alloy; According to Cu, Al, Y atomic percent is Cu (25-x) %, Al x% (x=1,3 and 5), Y10% preparation; All material purity is more than 99.95%, the Cu-Y-Al master alloy for preparing placed on the vacuum magnetic control tungsten electrode arc furnace carry out; The resistance furnace melting is adopted in the mother alloy melting; Magnesium is 65% adding by atomic percent; Cu-Y-Al master alloy with melting is put into resistance furnace; Be cast in respectively in the wedge shape copper mold of thickness 0~7mm, wide 60mm after 2 hours 760 ℃ of temperature insulations, prepare 3 kinds of composition Mg-Cu-Al-Y mother alloys; The single roller of amorphous thin ribbon preparation employing high vacuum revolves to be quenched and arc melting suction pouring system, places the lower end that the quartz glass tube of band nozzle is arranged the Mg-Cu-Al-Y mother alloy, adjusts the distance between nozzle and copper roller, and the sealing hatch door is evacuated to 1.0 * 10
-3Pa revolves the legal system of quenching with single roller and gets the bar carry sample.
2. according to the preparation method of the said a kind of magnesium base band non-crystaline amorphous metal of claim 1, optimum process parameters is: the silica tube nozzle bore is that 0.04MPa, copper roller rotating speed 30m/s are pressed in 3mm * 0.3mm, argon gas spray.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103253713A (en) * | 2013-05-14 | 2013-08-21 | 上海大学 | Method for preparing regular octahedral Fe3O4 particles |
CN103952649A (en) * | 2014-05-16 | 2014-07-30 | 辽宁石化职业技术学院 | Magnesium-based amorphous solid and preparation method thereof |
CN103966532A (en) * | 2014-05-16 | 2014-08-06 | 辽宁石化职业技术学院 | Mg-Cu-Dy amorphous body composite material and preparation method thereof |
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 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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US20050279427A1 (en) * | 2004-06-14 | 2005-12-22 | Park Eun S | Magnesium based amorphous alloy having improved glass forming ability and ductility |
CN102312177A (en) * | 2011-09-21 | 2012-01-11 | 镇江忆诺唯记忆合金有限公司 | Bulk magnesium-based amorphous alloy composite material |
-
2012
- 2012-06-25 CN CN2012102106656A patent/CN102808139A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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US20050279427A1 (en) * | 2004-06-14 | 2005-12-22 | Park Eun S | Magnesium based amorphous alloy having improved glass forming ability and ductility |
CN102312177A (en) * | 2011-09-21 | 2012-01-11 | 镇江忆诺唯记忆合金有限公司 | Bulk magnesium-based amorphous alloy composite material |
Non-Patent Citations (1)
Title |
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白高鹏: "镁基条带非晶的制备及其在铝合金中焊接应用的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》, 15 September 2008 (2008-09-15), pages 022 - 298 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103253713A (en) * | 2013-05-14 | 2013-08-21 | 上海大学 | Method for preparing regular octahedral Fe3O4 particles |
CN103952649A (en) * | 2014-05-16 | 2014-07-30 | 辽宁石化职业技术学院 | Magnesium-based amorphous solid and preparation method thereof |
CN103966532A (en) * | 2014-05-16 | 2014-08-06 | 辽宁石化职业技术学院 | Mg-Cu-Dy amorphous body composite material and preparation method thereof |
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 |
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Application publication date: 20121205 |