CN103668010B - A series of Zr Al Ni Cu block amorphous alloys with born of the same parents' shape microstructure - Google Patents

A series of Zr Al Ni Cu block amorphous alloys with born of the same parents' shape microstructure Download PDF

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CN103668010B
CN103668010B CN201310640750.0A CN201310640750A CN103668010B CN 103668010 B CN103668010 B CN 103668010B CN 201310640750 A CN201310640750 A CN 201310640750A CN 103668010 B CN103668010 B CN 103668010B
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born
same parents
melting
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vacuum chamber
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CN103668010A (en
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蔡安辉
熊翔
刘咏
安伟科
周果君
罗云
李铁林
李小松
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Hunan Institute of Science and Technology
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Abstract

The invention belongs to field of new materials, discloses a series of Zr Al Ni Cu block amorphous alloys with born of the same parents' shape microstructure.Zr Al Ni Cu block amorphous alloys are by Zr(99.99wt%)、Al(99.99wt%)、Ni(99.99wt%)And Cu(99.99wt%)Melting is carried out by vacuum melting method, a diameter of 3mm non-crystaline amorphous metal sample is then prepared by vacuum suction casting technique.The serial Zr Al Ni Cu block amorphous alloys have the microstructure of born of the same parents' shape, are the preferable presomas for preparing Zr Al Ni Cu bulk amorphous alloy foamed materials.

Description

A series of Zr-Al-Ni-Cu block amorphous alloys with born of the same parents' shape microstructure
Technical field
The present invention relates to a series of Zr-Al-Ni-Cu block amorphous alloys with born of the same parents' shape microstructure.
Background technology
Zirconium-based bulk amorphous alloy has that amorphous formation ability is good, elastic strain is big, resistance to corrosion is high, compression strength Height, the temperature-room type plasticity and biocompatibility that particularly some zirconium-base amorphous alloys have been shown, these features cause it in structure With there is great application prospect in technical field of biological material.At present, using high power transmission electron microscope it is observed that amorphous closes There is the presence of the cluster structure of atom or nanoscale in gold, but do not prepare also with the non-of micro-meter scale microstructure Peritectic alloy.And the temperature-room type plasticity of non-crystaline amorphous metal and its internal microstructure are closely bound up, therefore prepare with special micron The zirconium-based bulk amorphous alloy of yardstick microstructure has very important significance.
The content of the invention
It is an object of the invention to provide a series of Zr-Al-Ni-Cu block amorphous alloys with born of the same parents' shape microstructure.
The purpose of the present invention is achieved through the following technical solutions:A series of Zr-Al- with born of the same parents' shape microstructure Ni-Cu block amorphous alloys, it is characterised in that:Comprise the following steps:By purity be 99.99wt% block Cu, Zr, Al and Ni presses Zr-Al-Ni-Cu alloying component proportion ingredients;The material prepared is put into the crucible of electric arc furnaces, it is evacuated down to 1 × 10-3Purity is re-filled with after Pa>99.99wt% argon gas makes the pressure of vacuum chamber reach 0.45 atmospheric pressure, and then melting Ti is inhaled Gas;Molten alloy 5 times, foundry alloy is taken out after vacuum chamber cooling, crucible is cleaned up and crushes foundry alloy; The part foundry alloy crushed is put into the crucible of electric arc furnaces, and installs a diameter of 3mm of die cavity water cooled copper mould;Take out true It is empty to 1 × 10-3Purity is re-filled with after Pa>99.99wt% argon gas makes the pressure of vacuum chamber reach 0.2 atmospheric pressure, then melting Ti Air-breathing is carried out, and melting is carried out to foundry alloy and carries out suction casting, you can obtains a diameter of 3mm non-crystaline amorphous metal.
The alloying component is respectively Zr65Al8.7Cu14.4Ni11.9、Zr64Al10.1Cu11.7Ni14.2、 Zr63.5Al10.7Cu10.7Ni15.1、Zr62Al10Cu15Ni13、Zr61.5Al10.7Cu13.65Ni14.15、Zr60.5Al12.1Cu10.95Ni16.45 (at%), a diameter of 3mm amorphous sample can be formed, its inside has microstructure of born of the same parents' shape.
Product uses X-ray diffractometer respectively made of the present invention(XRD)And differential scanning calorimeter(DTA)Detect material Amorphous structure, burn into is carried out to the cross section of non-crystaline amorphous metal sample with the mixed liquor of hydrofluoric acid and nitric acid shown with scanning electron Micro mirror(SEM)The microstructure on cross section that analysis sample corroded, it is all complete non-to find product made of the present invention Crystalline substance simultaneously includes born of the same parents' shape microstructure that size is 3~20 microns.
Embodiment
Below according to specific embodiment, the invention will be further described:
Embodiment 1
According to Zr65Al8.7Cu14.4Ni11.9(at%)Alloying component, with assay balance weigh 15.2474 ± 0.0001g of zirconium, 1.7959 ± 0.0001g of 0.6036 ± 0.0001g of aluminium, 2.3530 ± 0.0001g of copper and nickel, it is put into the copper crucible of vacuum arc furnace ignition In, it is evacuated to 1 × 10-3Pa, being filled with argon gas makes the pressure of vacuum chamber up to 0.45 atmospheric pressure, after melting Ti carries out air-breathing, so Molten alloy 5 times afterwards, foundry alloy is taken out after vacuum chamber cooling, crucible is cleaned up and crushes foundry alloy, will be broken Good part foundry alloy is put into the crucible of electric arc furnaces, and installs a diameter of 3mm of die cavity water cooled copper mould, it is evacuated down to 1 × 10-3Purity is re-filled with after Pa>99.99wt% argon gas makes the pressure of vacuum chamber reach 0.2 atmospheric pressure, and then melting Ti is inhaled Gas, and melting is carried out to foundry alloy and inhale casting and obtain a diameter of 3mm sample.Then with water cooling diamond custting machine at a slow speed The sample that length is 2mm is removed among sample, its cross section is polished, polished and is carried out with the mixed liquor of hydrofluoric acid and nitric acid Corrosion.Find that the product is complete amorphous state by XRD and DTA technology for detection, the cross section hair after corroding by sem analysis Now there is clear born of the same parents' shape microstructure that size is 20 microns.
Embodiment 2
According to Zr61.5Al10.7Cu13.65Ni14.15(at%)Alloying component, with assay balance weigh zirconium 14.7700 ± 0.0001g, 2.1863 ± 0.0001g of 0.7601 ± 0.0001g of aluminium, 2.2836 ± 0.0001g of copper and nickel, are put into vacuum arc furnace ignition Copper crucible in, be evacuated to 1 × 10-3Pa, being filled with argon gas makes the pressure of vacuum chamber be inhaled up to 0.45 atmospheric pressure, melting Ti After gas, then molten alloy 5 time, foundry alloy is taken out after vacuum chamber cooling, crucible is cleaned up and crushes foundry alloy, The part foundry alloy crushed is put into the crucible of electric arc furnaces, and installs a diameter of 3mm of die cavity water cooled copper mould, is vacuumized To 1 × 10-3Purity is re-filled with after Pa>99.99wt% argon gas makes the pressure of vacuum chamber reach 0.2 atmospheric pressure, and then melting Ti enters Row air-breathing, and melting is carried out to foundry alloy and inhale casting and obtain a diameter of 3mm sample.Then with water cooling diamond cutting at a slow speed Cutting mill removes the sample that length is 2mm among sample, and its cross section is polished, polished and with hydrofluoric acid and the mixed liquor of nitric acid Corroded.Find that the product is complete amorphous state by XRD and DTA technology for detection, it is transversal after being corroded by sem analysis Face is found with clear born of the same parents' shape microstructure that size is 8 microns.
Embodiment 3
According to Zr60.5Al12.1Cu10.95Ni16.45(at%)Alloying component, with assay balance weigh zirconium 14.7041 ± 0.0001g, 2.5722 ± 0.0001g of 0.8698 ± 0.0001g of aluminium, 1.8539 ± 0.0001g of copper and nickel, are put into vacuum arc furnace ignition Copper crucible in, be evacuated to 1 × 10-3Pa, being filled with argon gas makes the pressure of vacuum chamber be inhaled up to 0.45 atmospheric pressure, melting Ti After gas, then molten alloy 5 time, foundry alloy is taken out after vacuum chamber cooling, crucible is cleaned up and crushes foundry alloy, The part foundry alloy crushed is put into the crucible of electric arc furnaces, and installs a diameter of 3mm of die cavity water cooled copper mould, is vacuumized To 1 × 10-3Purity is re-filled with after Pa>99.99wt% argon gas makes the pressure of vacuum chamber reach 0.2 atmospheric pressure, and then melting Ti enters Row air-breathing, and melting is carried out to foundry alloy and inhale casting and obtain a diameter of 3mm sample.Then with water cooling diamond cutting at a slow speed Cutting mill removes the sample that length is 2mm among sample, and its cross section is polished, polished and with hydrofluoric acid and the mixed liquor of nitric acid Corroded.Find that the product is complete amorphous state by XRD and DTA technology for detection, it is transversal after being corroded by sem analysis Face is found with clear born of the same parents' shape microstructure that size is 12 microns.
Embodiment 4
According to Zr63.5Al10.7Cu10.7Ni15.1(at%)Alloying component, with assay balance weigh zirconium 15.1492 ± 0.0001g, 2.3176 ± 0.0001g of 0.7550 ± 0.0001g of aluminium, 1.7782 ± 0.0001g of copper and nickel, are put into vacuum arc furnace ignition Copper crucible in, be evacuated to 1 × 10-3Pa, being filled with argon gas makes the pressure of vacuum chamber be inhaled up to 0.45 atmospheric pressure, melting Ti After gas, then molten alloy 5 time, foundry alloy is taken out after vacuum chamber cooling, crucible is cleaned up and crushes foundry alloy, The part foundry alloy crushed is put into the crucible of electric arc furnaces, and installs a diameter of 3mm of die cavity water cooled copper mould, is vacuumized To 1 × 10-3Purity is re-filled with after Pa>99.99wt% argon gas makes the pressure of vacuum chamber reach 0.2 atmospheric pressure, and then melting Ti enters Row air-breathing, and melting is carried out to foundry alloy and inhale casting and obtain a diameter of 3mm sample.Then with water cooling diamond cutting at a slow speed Cutting mill removes the sample that length is 2mm among sample, and its cross section is polished, polished and with hydrofluoric acid and the mixed liquor of nitric acid Corroded.Find that the product is complete amorphous state by XRD and DTA technology for detection, it is transversal after being corroded by sem analysis Face is found with clear born of the same parents' shape microstructure that size is 3 microns.

Claims (1)

  1. A series of 1. Zr-Al-Ni-Cu block amorphous alloys with born of the same parents' shape microstructure, it is characterised in that:Described alloy into It is respectively Zr65Al8.7Cu14.4Ni11.9、Zr64Al10.1Cu11.7Ni14.2、Zr63.5Al10.7Cu10.7Ni15.1、 Zr62Al10Cu15Ni13、Zr61.5Al10.7Cu13.65Ni14.15、Zr60.5Al12.1Cu10.95Ni16.45(at%), alloying component institute shape Into a diameter of 3mm sample be amorphous state, it is internal to include born of the same parents' shape microstructure;The preparation technology of the non-crystaline amorphous metal includes Following steps:
    Block Cu, Zr, Al and Ni that purity is 99.99wt% are pressed into Zr-Al-Ni-Cu alloying component proportion ingredients;
    The material prepared is put into the crucible of electric arc furnaces, is evacuated down to 1 × 10-3Purity is re-filled with after Pa>99.99wt% argon Gas makes the pressure of vacuum chamber reach 0.45 atmospheric pressure, and then melting Ti carries out air-breathing;
    Molten alloy 5 times, foundry alloy is taken out after vacuum chamber cooling, crucible is cleaned up and crushes foundry alloy;
    The part foundry alloy crushed is put into the crucible of electric arc furnaces, and installs the water cooled copper mould that diameter of bore is 3mm;
    It is evacuated down to 1 × 10-3Purity is re-filled with after Pa>99.99wt% argon gas makes the pressure of vacuum chamber reach 0.2 atmospheric pressure, Then melting Ti carries out air-breathing, and carries out melting to foundry alloy and carry out suction casting, you can obtains a diameter of 3mm non-crystaline amorphous metal.
CN201310640750.0A 2013-12-04 2013-12-04 A series of Zr Al Ni Cu block amorphous alloys with born of the same parents' shape microstructure Expired - Fee Related CN103668010B (en)

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CN104762497B (en) * 2015-05-05 2017-01-25 湖南理工学院 Zr-Al-Ni-Cu bulk amorphous alloy series with indoor temperature compressive plasticity and high strength
CN104775082A (en) * 2015-05-05 2015-07-15 湖南理工学院 Zr-Al-Ni-Cu bulk metallic glass achieving room temperature compression superplasticity
CN107829049B (en) * 2017-11-08 2022-01-18 湖南理工学院 Titanium-containing zirconium-based block amorphous alloy and preparation process thereof
CN108070801B (en) * 2017-12-19 2019-12-31 哈尔滨工业大学 Method for preparing low-cost centimeter-level zirconium-based amorphous alloy by adopting industrial-level sponge zirconium

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CN1609243A (en) * 2004-09-16 2005-04-27 上海交通大学 Control method of bulk amorphous alloy micro-structure
CN101225501A (en) * 2007-01-16 2008-07-23 中国科学院物理研究所 Zirconium-based block metal glass and preparation method thereof
CN103008614A (en) * 2012-12-18 2013-04-03 广东工业大学 Copper mould for preparing bulk amorphous alloy and manufacture method of copper mould

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EP1513637B1 (en) * 2002-05-20 2008-03-12 Liquidmetal Technologies Foamed structures of bulk-solidifying amorphous alloys

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Publication number Priority date Publication date Assignee Title
CN1609243A (en) * 2004-09-16 2005-04-27 上海交通大学 Control method of bulk amorphous alloy micro-structure
CN101225501A (en) * 2007-01-16 2008-07-23 中国科学院物理研究所 Zirconium-based block metal glass and preparation method thereof
CN103008614A (en) * 2012-12-18 2013-04-03 广东工业大学 Copper mould for preparing bulk amorphous alloy and manufacture method of copper mould

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