CN106521240B - A kind of high tough zircaloy and preparation method thereof - Google Patents

A kind of high tough zircaloy and preparation method thereof Download PDF

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Publication number
CN106521240B
CN106521240B CN201610928741.5A CN201610928741A CN106521240B CN 106521240 B CN106521240 B CN 106521240B CN 201610928741 A CN201610928741 A CN 201610928741A CN 106521240 B CN106521240 B CN 106521240B
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zircaloy
alloy
tough
smelting furnace
vacuum
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CN106521240A (en
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花能斌
陈文哲
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Fujian University of Technology
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Fujian University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C16/00—Alloys based on zirconium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous alloys by melting using master alloys

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Abstract

The present invention provides a kind of high tough zircaloy, and the chemical molecular formula of the height is tough zircaloy is ZraAlbCocMd, in formula：A, b, c, d are atomic percentage；Wherein 45≤a≤50,8≤b≤10,35≤c≤40,2≤d≤5, and a+b+c+d=100；M is at least one of Ti, Nb, Ta, Fe, Ni, Cu；Also disclose the preparation method of the tough zircaloy of the height；Zircaloy of the present invention not only has high intensity and high tenacity, but also with good compressive plastic deformation ability and excellent corrosion resistance；Whole preparation process is simply easily operated, and manufacturing cost is low；Therefore, the present invention has widened the selection of material for fields such as structural material, aerospace, medical instruments.

Description

A kind of high tough zircaloy and preparation method thereof
【Technical field】
The invention belongs to structural material field, and in particular to a kind of high tough zircaloy and preparation method thereof.
【Background technology】
Zirconium is a kind of rare metal, has excellent corrosion resistance and high fusing point (more than 1800 DEG C)；Zirconium has Allomorph changes, and the crystal structure under high temperature is body-centered cubic, is close-packed hexagonal under low temperature；The plasticity of zirconium is good, can pass through modeling Property be processed into tubing, plate, bar and silk material, its weldability might as well, be used for welding processing；But the room temperature of pure zirconium Tensile strength is very low, less than 400MPa, it is difficult to meet the requirement to mechanical property of structural material, therefore, industrial application with Based on zircaloy.
Zircaloy is the non-ferrous alloy formed using zirconium as matrix addition other elements, and main alloy element has tin, niobium, iron Deng.Zircaloy has good corrosion resisting property, moderate mechanical property, relatively low in 300~400 DEG C of high-temperature high pressure water and steam Atom thermal neutron absorption cross section, have good compatibility to nuclear fuel, the core structural materials for being used as water cooled nuclear reactor more. Zirconium has excellent corrosion stability to a variety of acid, alkali and salt, has strong affinity with gases such as oxygen, nitrogen, therefore zircaloy is also used for Corrosion-resistant member and pharmaceutical machine component are manufactured, is widely used as non-evaporable getter in electrovacuum and lamp industry.In addition, Zirconium has relatively low elasticity modulus, excellent corrosion resisting property and biocompatibility.Therefore zircaloy is in aerospace, military project, core Reaction, atomic energy and biomedical materials field are with a wide range of applications.
The zircaloy of commercial scale has two class of zirconium tin system and zirconium niobium system, the former alloy designations have Zr-2, Zr-4, the latter Typical Representative be Zr-2.5Nb.After the elements such as a small amount of tin of the alloying in pure zirconium, niobium, the intensity of zircaloy can improve To 900MPa, but it is also relatively low as intensity for structural material, it is therefore desirable to develop the zircaloy of high intensity.Block amorphous alloy It is a kind of new metallic material, different from crystal alloy, its atomic arrangement has the design feature of longrange disorder shortrange order, because And show a series of characteristics better than crystal alloy.In recent years, zirconium-base amorphous alloy due to high intensity (~ 1600MPa), high rigidity (~450Hv), low elastic modulus (~80GPa), high-fracture toughness (~60MPa m1/2) and high fatigue The excellent performance such as resistance and receive much concern；However, the plastic deformation of zirconium-base amorphous alloy relies primarily on height region at room temperature The shear band of change carries out, so that the features such as showing significant brittleness at room temperature and strain softening, limits it as structural material Application.Therefore, exploitation at the same time the zircaloy with high intensity and high tenacity for its structural material field application with Important meaning.
【The content of the invention】
The technical problems to be solved by the invention are to provide a kind of high tough zircaloy and preparation method thereof, the conjunction of gained zirconium Gold utensil has the characteristics of high intensity and high tenacity, and preparation method is simply easily operated.
The present invention is to solve above-mentioned technical problem by the following technical programs：The chemical molecular formula of the height is tough zircaloy For ZraAlbCocMd, in formula：A, b, c, d are atomic percentage；Wherein 45≤a≤50,8≤b≤10,35≤c≤40,2≤d≤ 5, and a+b+c+d=100；M is at least one of Ti, Nb, Ta, Fe, Ni, Cu.
Further, each component of the tough zircaloy of the height mass percent purity >=99.0%.
Further, the compression yield strength of the tough zircaloy of the height is 1100~1400MPa, and compressed rupture strength is 1350~1710MPa.
Further, corrosion rate of the tough zircaloy of the height in the HCl that concentration is 1mol/L is less than 1 μm/year.
At the same time, the preparation method of the above-mentioned tough zircaloy of height is disclosed, which includes following concrete operations Step：
Step 1: dispensing：Zr is weighed by atomic percentaAlbCocMdEach component, and the quality of each component Percent purity is not less than 99.0%, obtains melting raw material after mixing, spare；
Step 2: melting ZraAlbCocMdFoundry alloy：
Melting raw material obtained by step 1 is put into vacuum smelting furnace, adjusts the vacuum of the vacuum chamber of vacuum smelting furnace To 1 × 10-3~5 × 10-3Pa, and carry out melting, melting under the high-purity argon gas protection of mass percent purity >=99.999% 2500~2800 DEG C of temperature；Melt back 4 times or more than 4 times, obtains ZraAlbCocMdFoundry alloy；
Step 3: ZraAlbCocMdAlloy cast ingot cools down：
By the foundry alloy that step 2 obtains under the high-purity argon gas protection of mass percent purity >=99.999%, using true The water jacketed copper crucible of empty smelting furnace cools down the foundry alloy, until foundry alloy by liquid cooled to solid-state, then proceedes to protect Hold the copper crucible water cooling state of vacuum smelting furnace, taken out after foundry alloy is continued cool to room temperature in vacuum smelting furnace, then The Zr of even tissueaAlbCocMdAlloy cast ingot, that is, tough the zircaloy of the height.
Further, which further includes Step 4: ZraAlbCocMdAlloy sample is processed：
By Zr made from step 3aAlbCocMdAlloy cast ingot wire cutting method requires to intercept according to required size Intermediate portion, after being ground polishing to cutting rear surface, that is, obtains ZraAlbCocMdAlloy sample.
The beneficial effects of the present invention are：
For current most of zircaloy plasticity preferably but intensity is relatively low, zirconium-base amorphous alloy intensity is higher but plasticity The problem of deformation energy force difference, the present invention provides a kind of zircaloy with high intensity and high tenacity, and have good compression Plastic deformation ability and excellent corrosion resistance；The preparation method of the tough zircaloy of the height is also disclosed, was entirely prepared Journey is simply easily operated, and manufacturing cost is low；Therefore, the present invention widens for fields such as structural material, aerospace, medical instruments The selection of material.
【Embodiment】
The chemical molecular formula of high tough zircaloy of the invention is ZraAlbCocMd, in formula：A, b, c, d are atomic percentage； Wherein 45≤a≤50,8≤b≤10,35≤c≤40,2≤d≤5, and a+b+c+d=100；M is Ti, Nb, Ta, Fe, Ni, Cu At least one of.
Wherein, the mass percent purity of each component of high tough zircaloy is >=99.0%；The height is tough, and zirconium closes The compression yield strength of gold is 1100~1400MPa, and compressed rupture strength is 1350~1710MPa, it is 1mol/L in concentration HCl in corrosion rate be less than 1 μm/year.
The preparation method of the above-mentioned tough zircaloy of height includes following concrete operation step：
Step 1: dispensing：Zr is weighed by atomic percentaAlbCocMdEach component, and the quality of each component Percent purity is not less than 99.0%, obtains melting raw material after mixing, spare；
Step 2: melting ZraAlbCocMdFoundry alloy：
Melting raw material obtained by step 1 is put into vacuum smelting furnace, adjusts the vacuum of the vacuum chamber of vacuum smelting furnace To 1 × 10-3~5 × 10-3Pa, and carry out melting, melting under the high-purity argon gas protection of mass percent purity >=99.999% 2500~2800 DEG C of temperature；Melt back 4 times or more than 4 times, obtains ZraAlbCocMdFoundry alloy；
Step 3: ZraAlbCocMdAlloy cast ingot cools down：
The foundry alloy that step 2 obtains is allowed under the high-purity argon gas protection of mass percent purity >=99.999%, using true The water jacketed copper crucible of empty smelting furnace cools down the foundry alloy, until the foundry alloy is (cold by liquid by liquid cooled to solid-state But be generally 20-60 seconds to the cooling time needed for solid-state), then proceed to keep vacuum smelting furnace copper crucible water cooling state, Taken out after foundry alloy is continued cool to room temperature in vacuum smelting furnace, then obtain the Zr of even tissueaAlbCocMdAlloy cast ingot is The tough zircaloy of height.
In addition, in order to enable Zr of the present inventionaAlbCocMdAlloy cast ingot can generally incite somebody to action easy to market demands such as later stage sale It is processed into sample, i.e. the present invention may also include Step 4: ZraAlbCocMdAlloy sample is processed, specifically, by made from ZraAlbCocMdAlloy cast ingot wire cutting method requires interception intermediate portion according to required size, to cutting rear surface After being ground polishing, that is, obtain ZraAlbCocMdAlloy sample.
In order to be preferably described to the present invention, applicant illustrates following examples.
Embodiment 1
It is Zr to prepare chemical molecular formula50Al10Co35Ni5High tough zircaloy, specifically operate it is as follows：
By atomic percent Zr50Al10Co35Ni5Zr, Al, Co, Ni pure element are weighed, and the mass percent of each element is pure Degree is not less than 99.0%, obtains melting raw material after mixing, spare；The melting raw material of gained is put into vacuum smelting furnace, The vacuum of the vacuum chamber of vacuum smelting furnace is adjusted to 3 × 10-3Pa, and in the high-purity argon of mass percent purity >=99.999% Melting, 2600 DEG C of smelting temperature are carried out under gas shielded；Melt back 5 times, obtains Zr50Al10Co35Ni5Foundry alloy；Allow obtain Foundry alloy still mass percent purity >=99.999% high-purity argon gas protection under, utilize the water-cooled copper of vacuum smelting furnace Crucible cools down the foundry alloy, which is 30 seconds by liquid to solid cooling time, then proceedes to keep vacuum The copper crucible water cooling state of smelting furnace, takes out after foundry alloy is continued cool to room temperature in vacuum smelting furnace, then must organize Even Zr50Al10Co35Ni5Alloy cast ingot, that is, tough the zircaloy of the height.
By Zr made from the present embodiment50Al10Co35Ni5Alloy cast ingot is disconnected with wire cutting method interception intermediate portion Face, after being ground polishing, is tested using X-ray diffraction and determines crystalline phase, the results showed that the crystalline phase of alloy for ZrCo phases and ZrAlCo eutectic phases；Scanning electron microscope tissues observed pattern, the distribution of ZrAlCo eutectic phase crystal grain even dispersion are used at the same time Around ZrCo phase crystal grain；Interception specification is the alloy cast ingot sample of 2mm × 2mm × 4mm, tests its Compressive Mechanical Properties, Then know the yield strength 1100MPa, fracture strength 1710MPa, amount of plastic deformation 18% of the alloy cast ingot；Using 1mol/L's HCl immersion test beta alloy ingot castings, it is 0.96 μm/year to learn its corrosion rate.
Embodiment 2
It is Zr to prepare chemical molecular formula50Al10Co35Fe5High tough zircaloy, specifically operate it is as follows：
By atomic percent Zr50Al10Co35Fe5Weighing Zr, Al, Co, Fe pure element, and the mass percent of each element Purity is not less than 99.0%, obtains melting raw material after mixing, spare；The melting raw material of gained is put into vacuum smelting furnace In, the vacuum of vacuum chamber of vacuum smelting furnace is adjusted to 1 × 10-3Pa, and in the height of mass percent purity >=99.999% Melting, 2500 DEG C of smelting temperature are carried out under straight argon gas shielded；Melt back 4 times, obtains Zr50Al10Co35Fe5Foundry alloy；Allow Obtained foundry alloy still under the high-purity argon gas protection of mass percent purity >=99.999%, utilizes the water of vacuum smelting furnace Cold copper crucible cools down the foundry alloy, which is 30 seconds by liquid to solid cooling time, then proceedes to keep The copper crucible water cooling state of vacuum smelting furnace, takes out after foundry alloy is continued cool to room temperature in vacuum smelting furnace, then obtains group Knit uniform Zr50Al10Co35Fe5Alloy cast ingot, that is, tough the zircaloy of the height.
By Zr made from the present embodiment50Al10Co35Fe5Alloy cast ingot is disconnected with wire cutting method interception intermediate portion Face, after being ground polishing, is tested using X-ray diffraction and determines crystalline phase, the results showed that the crystalline phase of alloy for ZrCo phases and ZrAlCo eutectic phases；Scanning electron microscope tissues observed pattern, the distribution of ZrAlCo eutectic phase crystal grain even dispersion are used at the same time Around ZrCo phase crystal grain；Interception specification is the alloy cast ingot sample of 2mm × 2mm × 4mm, tests its Compressive Mechanical Properties, Then know the yield strength 1110MPa, fracture strength 1350MPa, amount of plastic deformation 8% of the alloy cast ingot；Using the HCl of 1mol/L Immersion test beta alloy ingot casting, it is 0.54 μm/year to learn its corrosion rate.
Embodiment 3
It is Zr to prepare chemical molecular formula50Al10Co35Cu5High tough zircaloy, specifically operate it is as follows：
By atomic percent Zr50Al10Co35Cu5Weighing Zr, Al, Co, Cu pure element, and the mass percent of each element Purity is not less than 99.0%, obtains melting raw material after mixing, spare；The melting raw material of gained is put into vacuum smelting furnace In, the vacuum of vacuum chamber of vacuum smelting furnace is adjusted to 2 × 10-3Pa, and in the height of mass percent purity >=99.999% Melting, 2500 DEG C of smelting temperature are carried out under straight argon gas shielded；Melt back 6 times, obtains Zr50Al10Co35Cu5Foundry alloy；Allow Obtained foundry alloy still under the high-purity argon gas protection of mass percent purity >=99.999%, utilizes the water of vacuum smelting furnace Cold copper crucible cools down the foundry alloy, which is 25 seconds by liquid to solid cooling time, then proceedes to keep The copper crucible water cooling state of vacuum smelting furnace, takes out after foundry alloy is continued cool to room temperature in vacuum smelting furnace, then obtains group Knit uniform Zr50Al10Co35Cu5Alloy cast ingot, that is, tough the zircaloy of the height.
By Zr made from the present embodiment50Al10Co35Cu5Alloy cast ingot is disconnected with wire cutting method interception intermediate portion Face, after being ground polishing, is tested using X-ray diffraction and determines crystalline phase, the results showed that the crystalline phase of alloy for ZrCo phases and ZrAlCo eutectic phases；Scanning electron microscope tissues observed pattern, the distribution of ZrAlCo eutectic phase crystal grain even dispersion are used at the same time Around ZrCo phase crystal grain；Interception specification is the alloy cast ingot sample of 2mm × 2mm × 4mm, tests its Compressive Mechanical Properties, Then know the yield strength 1360MPa, fracture strength 1690MPa, amount of plastic deformation 9% of the alloy cast ingot；Using the HCl of 1mol/L Immersion test beta alloy ingot casting, it is 0.79 μm/year to learn its corrosion rate.
Embodiment 4
It is Zr to prepare chemical molecular formula48Al8Co38Ni3Fe3High tough zircaloy, specifically operate it is as follows：
By atomic percent Zr48Al8Co38Ni3Fe3Weighing Zr, Al, Co, Ni, Fe pure element, and the quality of each element Percent purity is not less than 99.0%, obtains melting raw material after mixing, spare；The melting raw material of gained is put into vacuum smelting In furnace, the vacuum of vacuum chamber of vacuum smelting furnace is adjusted to 3 × 10-3Pa, and in mass percent purity >=99.999% High-purity argon gas protection lower carry out melting, 2600 DEG C of smelting temperature；Melt back 4 times, obtains Zr48Al8Co38Ni3Fe3Female conjunction Gold；The foundry alloy allowed still under the high-purity argon gas protection of mass percent purity >=99.999%, utilizes vacuum metling The water jacketed copper crucible of stove cools down the foundry alloy, which is 32 seconds by liquid to solid cooling time, Ran Houji The copper crucible water cooling state of vacuum smelting furnace is held in continuation of insurance, is taken out after foundry alloy is continued cool to room temperature in vacuum smelting furnace, Then obtain the Zr of even tissue48Al8Co38Ni3Fe3Alloy cast ingot, that is, tough the zircaloy of the height.
By Zr made from the present embodiment48Al8Co38Ni3Fe3Alloy cast ingot is disconnected with wire cutting method interception intermediate portion Face, after being ground polishing, is tested using X-ray diffraction and determines crystalline phase, the results showed that the crystalline phase of alloy for ZrCo phases and ZrAlCo eutectic phases；Scanning electron microscope tissues observed pattern, the distribution of ZrAlCo eutectic phase crystal grain even dispersion are used at the same time Around ZrCo phase crystal grain；Interception specification is the alloy cast ingot sample of 2mm × 2mm × 4mm, tests its Compressive Mechanical Properties, Then know the yield strength 1100MPa, fracture strength 1650MPa, amount of plastic deformation 14% of the alloy cast ingot；Using 1mol/L's HCl immersion test beta alloy ingot castings, it is 0.78 μm/year to learn its corrosion rate.
Embodiment 5
It is Zr to prepare chemical molecular formula48Al8Co38Ni3Cu3High tough zircaloy, specifically operate it is as follows：
By atomic percent Zr48Al8Co38Ni3Cu3Weighing Zr, Al, Co, Ni, Cu pure element, and the quality of each element Percent purity is not less than 99.0%, obtains melting raw material after mixing, spare；The melting raw material of gained is put into vacuum smelting In furnace, the vacuum of vacuum chamber of vacuum smelting furnace is adjusted to 1 × 10-3Pa, and in mass percent purity >=99.999% High-purity argon gas protection lower carry out melting, 2550 DEG C of smelting temperature；Melt back 6 times, obtains Zr48Al8Co38Ni3Cu3Female conjunction Gold；The foundry alloy allowed still under the high-purity argon gas protection of mass percent purity >=99.999%, utilizes vacuum metling The water jacketed copper crucible of stove cools down the foundry alloy, which is 50 seconds by liquid to solid cooling time, Ran Houji The copper crucible water cooling state of vacuum smelting furnace is held in continuation of insurance, is taken out after foundry alloy is continued cool to room temperature in vacuum smelting furnace, Then obtain the Zr of even tissue48Al8Co38Ni3Cu3Alloy cast ingot, that is, tough the zircaloy of the height.
By Zr made from the present embodiment48Al8Co38Ni3Cu3Alloy cast ingot is disconnected with wire cutting method interception intermediate portion Face, after being ground polishing, is tested using X-ray diffraction and determines crystalline phase, the results showed that the crystalline phase of alloy for ZrCo phases and ZrAlCo eutectic phases；Scanning electron microscope tissues observed pattern, the distribution of ZrAlCo eutectic phase crystal grain even dispersion are used at the same time Around ZrCo phase crystal grain；Interception specification is the alloy cast ingot sample of 2mm × 2mm × 4mm, tests its Compressive Mechanical Properties, Then know the yield strength 1210MPa, fracture strength 1680MPa, amount of plastic deformation 15% of the alloy cast ingot；Using 1mol/L's HCl immersion test beta alloy ingot castings, it is 0.86 μm/year to learn its corrosion rate.
Embodiment 6
It is Zr to prepare chemical molecular formula48Al8Co38Cu3Fe3High tough zircaloy, specifically operate it is as follows：
By atomic percent Zr48Al8Co38Cu3Fe3Weighing Zr, Al, Co, Cu, Fe pure element, and the quality of each element Percent purity is not less than 99.0%, obtains melting raw material after mixing, spare；The melting raw material of gained is put into vacuum smelting In furnace, the vacuum of vacuum chamber of vacuum smelting furnace is adjusted to 4.5 × 10-3Pa, and mass percent purity >= 99.999% high-purity argon gas protection is lower to carry out melting, 2600 DEG C of smelting temperature；Melt back 5 times, obtains Zr48Al8Co38Ni3Cu3Foundry alloy；The foundry alloy allowed is still in the high-purity argon of mass percent purity >=99.999% Under gas shielded, the foundry alloy is cooled down using the water jacketed copper crucible of vacuum smelting furnace, the foundry alloy is by liquid to solid Cooling time is 45 seconds, then proceedes to keep the copper crucible water cooling state of vacuum smelting furnace, by foundry alloy in vacuum smelting furnace Taken out after continuing cool to room temperature, then obtain the Zr of even tissue48Al8Co38Cu3Fe3Alloy cast ingot, that is, tough the zircaloy of the height.
By Zr made from the present embodiment48Al8Co38Cu3Fe3Alloy cast ingot is disconnected with wire cutting method interception intermediate portion Face, after being ground polishing, is tested using X-ray diffraction and determines crystalline phase, the results showed that the crystalline phase of alloy for ZrCo phases and ZrAlCo eutectic phases；Scanning electron microscope tissues observed pattern, the distribution of ZrAlCo eutectic phase crystal grain even dispersion are used at the same time Around ZrCo phase crystal grain；Interception specification is the alloy cast ingot sample of 2mm × 2mm × 4mm, tests its Compressive Mechanical Properties, Then know the yield strength 1180MPa, fracture strength 1570MPa, amount of plastic deformation 10% of the alloy cast ingot；Using 1mol/L's HCl immersion test beta alloy ingot castings, it is 0.62 μm/year to learn its corrosion rate.
Embodiment 7
It is Zr to prepare chemical molecular formula48Al8Co38Ni2Fe2Cu2High tough zircaloy, specifically operate it is as follows：
By atomic percent Zr48Al8Co38Ni2Fe2Cu2Weighing Zr, Al, Co, Ni, Fe, Cu pure element, and each element Mass percent purity is not less than 99.0%, obtains melting raw material after mixing, spare；The melting raw material of gained is put into very In empty smelting furnace, the vacuum of vacuum chamber of vacuum smelting furnace is adjusted to 4 × 10-3Pa, and mass percent purity >= 99.999% high-purity argon gas protection is lower to carry out melting, 2500 DEG C of smelting temperature；Melt back 5 times, obtains Zr48Al8Co38Ni2Fe2Cu2Foundry alloy；The foundry alloy allowed is still in the high-purity of mass percent purity >=99.999% Under argon gas protection, the foundry alloy is cooled down using the water jacketed copper crucible of vacuum smelting furnace, the foundry alloy is by liquid to solid-state Cooling time be 20 seconds, then proceed to keep vacuum smelting furnace copper crucible water cooling state, by foundry alloy in vacuum smelting furnace Taken out after inside continuing cool to room temperature, then obtain the Zr of even tissue48Al8Co38Ni2Fe2Cu2Alloy cast ingot, that is, tough the zirconium of the height Alloy.
By Zr made from the present embodiment48Al8Co38Ni2Fe2Cu2Alloy cast ingot wire cutting method interception intermediate portion Section, after being ground polishing, is tested using X-ray diffraction and determines crystalline phase, the results showed that the crystalline phase of alloy for ZrCo phases and ZrAlCo eutectic phases；Scanning electron microscope tissues observed pattern, the distribution of ZrAlCo eutectic phase crystal grain even dispersion are used at the same time Around ZrCo phase crystal grain；Interception specification is the alloy cast ingot sample of 2mm × 2mm × 4mm, tests its Compressive Mechanical Properties, Then know the yield strength 1150MPa, fracture strength 1610MPa, amount of plastic deformation 13% of the alloy cast ingot；Using 1mol/L's HCl immersion test beta alloy ingot castings, it is 0.74 μm/year to learn its corrosion rate.
Embodiment 8
It is Zr to prepare chemical molecular formula45Ti5Al10Co40High tough zircaloy, specifically operate it is as follows：
By atomic percent Zr45Ti5Al10Co40Weighing Zr, Ti, Al, Co pure element, and the mass percent of each element Purity is not less than 99.0%, obtains melting raw material after mixing, spare；The melting raw material of gained is put into vacuum smelting furnace In, the vacuum of vacuum chamber of vacuum smelting furnace is adjusted to 1 × 10-3Pa, and in the height of mass percent purity >=99.999% Melting, 2600 DEG C of smelting temperature are carried out under straight argon gas shielded；Melt back 5 times, obtains Zr45Ti5Al10Co40Foundry alloy；Allow Obtained foundry alloy still under the high-purity argon gas protection of mass percent purity >=99.999%, utilizes the water of vacuum smelting furnace Cold copper crucible cools down the foundry alloy, which is 40 seconds by liquid to solid cooling time, then proceedes to keep The copper crucible water cooling state of vacuum smelting furnace, takes out after foundry alloy is continued cool to room temperature in vacuum smelting furnace, then obtains group Knit uniform Zr45Ti5Al10Co40Alloy cast ingot, that is, tough the zircaloy of the height.
By Zr made from the present embodiment45Ti5Al10Co40Alloy cast ingot is disconnected with wire cutting method interception intermediate portion Face, after being ground polishing, is tested using X-ray diffraction and determines crystalline phase, the results showed that the crystalline phase of alloy for ZrCo phases and ZrAlCo eutectic phases；Scanning electron microscope tissues observed pattern, the distribution of ZrAlCo eutectic phase crystal grain even dispersion are used at the same time Around ZrCo phase crystal grain；Interception specification is the alloy cast ingot sample of 2mm × 2mm × 4mm, tests its Compressive Mechanical Properties, Then know the yield strength 1350MPa, fracture strength 1480MPa, amount of plastic deformation 2% of the alloy cast ingot；Using the HCl of 1mol/L Immersion test beta alloy ingot casting, it is 0.33 μm/year to learn its corrosion rate.
Embodiment 9
It is Zr to prepare chemical molecular formula45Nb5Al10Co40High tough zircaloy, specifically operate it is as follows：
By atomic percent Zr45Ti5Al10Co40Weighing Zr, Nb, Al, Co pure element, and the mass percent of each element Purity is not less than 99.0%, obtains melting raw material after mixing, spare；The melting raw material of gained is put into vacuum smelting furnace In, the vacuum of vacuum chamber of vacuum smelting furnace is adjusted to 2 × 10-3Pa, and in the height of mass percent purity >=99.999% Melting, 2800 DEG C of smelting temperature are carried out under straight argon gas shielded；Melt back 4 times, obtains Zr45Nb5Al10Co40Foundry alloy；Allow Obtained foundry alloy still under the high-purity argon gas protection of mass percent purity >=99.999%, utilizes the water of vacuum smelting furnace Cold copper crucible cools down the foundry alloy, which is 50 seconds by liquid to solid cooling time, then proceedes to keep The copper crucible water cooling state of vacuum smelting furnace, takes out after foundry alloy is continued cool to room temperature in vacuum smelting furnace, then obtains group Knit uniform Zr45Nb5Al10Co40Alloy cast ingot, that is, tough the zircaloy of the height.
By Zr made from the present embodiment45Nb5Al10Co40Alloy cast ingot is disconnected with wire cutting method interception intermediate portion Face, after being ground polishing, is tested using X-ray diffraction and determines crystalline phase, the results showed that the crystalline phase of alloy for ZrCo phases and ZrAlCo eutectic phases；Scanning electron microscope tissues observed pattern, the distribution of ZrAlCo eutectic phase crystal grain even dispersion are used at the same time Around ZrCo phase crystal grain；Interception specification is the alloy cast ingot sample of 2mm × 2mm × 4mm, tests its Compressive Mechanical Properties, Then know the yield strength 1360MPa, fracture strength 1700MPa, amount of plastic deformation 14% of the alloy cast ingot；Using 1mol/L's HCl immersion test beta alloy ingot castings, it is 0.19 μm/year to learn its corrosion rate.
Embodiment 10
It is Zr to prepare chemical molecular formula45Ta5Al10Co40High tough zircaloy, specifically operate it is as follows：
By atomic percent Zr45Ta5Al10Co40Weighing Zr, Ta, Al, Co pure element, and the mass percent of each element Purity is not less than 99.0%, obtains melting raw material after mixing, spare；The melting raw material of gained is put into vacuum smelting furnace In, the vacuum of vacuum chamber of vacuum smelting furnace is adjusted to 2 × 10-3Pa, and in the height of mass percent purity >=99.999% Melting, 2800 DEG C of smelting temperature are carried out under straight argon gas shielded；Melt back 6 times, obtains Zr45Ta5Al10Co40Foundry alloy；Allow Obtained foundry alloy still under the high-purity argon gas protection of mass percent purity >=99.999%, utilizes the water of vacuum smelting furnace Cold copper crucible cools down the foundry alloy, which is 60 seconds by liquid to solid cooling time, then proceedes to keep The copper crucible water cooling state of vacuum smelting furnace, takes out after foundry alloy is continued cool to room temperature in vacuum smelting furnace, then obtains group Knit uniform Zr45Ta5Al10Co40Alloy cast ingot, that is, tough the zircaloy of the height.
By Zr made from the present embodiment45Ta5Al10Co40Alloy cast ingot is disconnected with wire cutting method interception intermediate portion Face, after being ground polishing, is tested using X-ray diffraction and determines crystalline phase, the results showed that the crystalline phase of alloy for ZrCo phases and ZrAlCo eutectic phases；Scanning electron microscope tissues observed pattern, the distribution of ZrAlCo eutectic phase crystal grain even dispersion are used at the same time Around ZrCo phase crystal grain；Interception specification is the alloy cast ingot sample of 2mm × 2mm × 4mm, tests its Compressive Mechanical Properties, Then know the yield strength 1400MPa, fracture strength 1500MPa, amount of plastic deformation 2% of the alloy cast ingot；Using the HCl of 1mol/L Immersion test beta alloy ingot casting, it is 0.09 μm/year to learn its corrosion rate.
Embodiment 11
It is Zr to prepare chemical molecular formula45Ti3Nb3Al9Co40High tough zircaloy, specifically operate it is as follows：
By atomic percent Zr45Ti3Nb3Al9Co40Weighing Zr, Ti, Nb, Al, Co pure element, and the quality of each element Percent purity is not less than 99.0%, obtains melting raw material after mixing, spare；The melting raw material of gained is put into vacuum smelting In furnace, the vacuum of vacuum chamber of vacuum smelting furnace is adjusted to 5 × 10-3Pa, and in mass percent purity >=99.999% High-purity argon gas protection lower carry out melting, 2500 DEG C of smelting temperature；Melt back 4 times, obtains Zr45Ti3Nb3Al9Co40Female conjunction Gold；The foundry alloy allowed still under the high-purity argon gas protection of mass percent purity >=99.999%, utilizes vacuum metling The water jacketed copper crucible of stove cools down the foundry alloy, which is 50 seconds by liquid to solid cooling time, Ran Houji The copper crucible water cooling state of vacuum smelting furnace is held in continuation of insurance, is taken out after foundry alloy is continued cool to room temperature in vacuum smelting furnace, Then obtain the Zr of even tissue45Ti3Nb3Al9Co40Alloy cast ingot, that is, tough the zircaloy of the height.
By Zr made from the present embodiment45Ti3Nb3Al9Co40Alloy cast ingot is disconnected with wire cutting method interception intermediate portion Face, after being ground polishing, is tested using X-ray diffraction and determines crystalline phase, the results showed that the crystalline phase of alloy for ZrCo phases and ZrAlCo eutectic phases；Scanning electron microscope tissues observed pattern, the distribution of ZrAlCo eutectic phase crystal grain even dispersion are used at the same time Around ZrCo phase crystal grain；Interception specification is the alloy cast ingot sample of 2mm × 2mm × 4mm, tests its Compressive Mechanical Properties, Then know the yield strength 1340MPa, fracture strength 1650MPa, amount of plastic deformation 10% of the alloy cast ingot；Using 1mol/L's HCl immersion test beta alloy ingot castings, it is 0.21 μm/year to learn its corrosion rate.
Embodiment 12
It is Zr to prepare chemical molecular formula45Ti3Ta3Al9Co40High tough zircaloy, specifically operate it is as follows：
By atomic percent Zr45Ti3Nb3Al9Co40Weighing Zr, Ti, Ta, Al, Co pure element, and the quality of each element Percent purity is not less than 99.0%, obtains melting raw material after mixing, spare；The melting raw material of gained is put into vacuum smelting In furnace, the vacuum of vacuum chamber of vacuum smelting furnace is adjusted to 2.5 × 10-3Pa, and mass percent purity >= 99.999% high-purity argon gas protection is lower to carry out melting, 2650 DEG C of smelting temperature；Melt back 6 times, obtains Zr45Ti3Ta3Al9Co40Foundry alloy；The foundry alloy allowed is still in the high-purity argon of mass percent purity >=99.999% Under gas shielded, the foundry alloy is cooled down using the water jacketed copper crucible of vacuum smelting furnace, the foundry alloy is by liquid to solid Cooling time is 39 seconds, then proceedes to keep the copper crucible water cooling state of vacuum smelting furnace, by foundry alloy in vacuum smelting furnace Taken out after continuing cool to room temperature, then obtain the Zr of even tissue45Ti3Ta3Al9Co40Alloy cast ingot, that is, tough the zircaloy of the height.
By Zr made from the present embodiment45Ti3Ta3Al9Co40Alloy cast ingot is disconnected with wire cutting method interception intermediate portion Face, after being ground polishing, is tested using X-ray diffraction and determines crystalline phase, the results showed that the crystalline phase of alloy for ZrCo phases and ZrAlCo eutectic phases；Scanning electron microscope tissues observed pattern, the distribution of ZrAlCo eutectic phase crystal grain even dispersion are used at the same time Around ZrCo phase crystal grain；Interception specification is the alloy cast ingot sample of 2mm × 2mm × 4mm, tests its Compressive Mechanical Properties, Then know the yield strength 1370MPa, fracture strength 1490MPa, amount of plastic deformation 2% of the alloy cast ingot；Using the HCl of 1mol/L Immersion test beta alloy ingot casting, it is 0.17 μm/year to learn its corrosion rate.
Embodiment 13
It is Zr to prepare chemical molecular formula45Nb3Ta3Al9Co40High tough zircaloy, specifically operate it is as follows：
By atomic percent Zr45Nb3Ta3Al9Co40Weighing Zr, Nb, Ta, Al, Co pure element, and the quality of each element Percent purity is not less than 99.0%, obtains melting raw material after mixing, spare；The melting raw material of gained is put into vacuum smelting In furnace, the vacuum of vacuum chamber of vacuum smelting furnace is adjusted to 5 × 10-3Pa, and in mass percent purity >=99.999% High-purity argon gas protection lower carry out melting, 2600 DEG C of smelting temperature；Melt back 4 times, obtains Zr45Nb3Ta3Al9Co40Female conjunction Gold；The foundry alloy allowed still under the high-purity argon gas protection of mass percent purity >=99.999%, utilizes vacuum metling The water jacketed copper crucible of stove cools down the foundry alloy, which is 45 seconds by liquid to solid cooling time, Ran Houji The copper crucible water cooling state of vacuum smelting furnace is held in continuation of insurance, is taken out after foundry alloy is continued cool to room temperature in vacuum smelting furnace, Then obtain the Zr of even tissue45Nb3Ta3Al9Co40Alloy cast ingot, that is, tough the zircaloy of the height.
By Zr made from the present embodiment45Nb3Ta3Al9Co40Alloy cast ingot is disconnected with wire cutting method interception intermediate portion Face, after being ground polishing, is tested using X-ray diffraction and determines crystalline phase, the results showed that the crystalline phase of alloy for ZrCo phases and ZrAlCo eutectic phases；Scanning electron microscope tissues observed pattern, the distribution of ZrAlCo eutectic phase crystal grain even dispersion are used at the same time Around ZrCo phase crystal grain；Interception specification is the alloy cast ingot sample of 2mm × 2mm × 4mm, tests its Compressive Mechanical Properties, Then know the yield strength 1380MPa, fracture strength 1610MPa, amount of plastic deformation 7% of the alloy cast ingot；Using the HCl of 1mol/L Immersion test beta alloy ingot casting, it is 0.12 μm/year to learn its corrosion rate.
Embodiment 14
It is Zr to prepare chemical molecular formula45Ti2Nb2Ta2Al9Co40High tough zircaloy, specifically operate it is as follows：
By atomic percent Zr45Ti2Nb2Ta2Al9Co40Weighing Zr, Ti, Nb, Ta, Al, Co pure element, and each element Mass percent purity is not less than 99.0%, obtains melting raw material after mixing, spare；The melting raw material of gained is put into very In empty smelting furnace, the vacuum of vacuum chamber of vacuum smelting furnace is adjusted to 1 × 10-3Pa, and mass percent purity >= 99.999% high-purity argon gas protection is lower to carry out melting, 2700 DEG C of smelting temperature；Melt back 5 times, obtains Zr45Ti2Nb2Ta2Al9Co40Foundry alloy；The foundry alloy allowed is still in the high-purity of mass percent purity >=99.999% Under argon gas protection, the foundry alloy is cooled down using the water jacketed copper crucible of vacuum smelting furnace, the foundry alloy is by liquid to solid-state Cooling time be 30 seconds, then proceed to keep vacuum smelting furnace copper crucible water cooling state, by foundry alloy in vacuum smelting furnace Taken out after inside continuing cool to room temperature, then obtain the Zr of even tissue45Ti2Nb2Ta2Al9Co40Alloy cast ingot, that is, tough the zirconium of the height Alloy.
By Zr made from the present embodiment45Ti2Nb2Ta2Al9Co40Alloy cast ingot wire cutting method interception intermediate portion Section, after being ground polishing, is tested using X-ray diffraction and determines crystalline phase, the results showed that the crystalline phase of alloy for ZrCo phases and ZrAlCo eutectic phases；Scanning electron microscope tissues observed pattern, the distribution of ZrAlCo eutectic phase crystal grain even dispersion are used at the same time Around ZrCo phase crystal grain；Interception specification is the alloy cast ingot sample of 2mm × 2mm × 4mm, tests its Compressive Mechanical Properties, Then know the yield strength 1340MPa, fracture strength 1600MPa, amount of plastic deformation 6% of the alloy cast ingot；Using the HCl of 1mol/L Immersion test beta alloy ingot casting, it is 0.20 μm/year to learn its corrosion rate.
Embodiment 15
It is Zr to prepare chemical molecular formula45Ti2Nb2Ta2Al8Co35Fe2Cu2Ni2High tough zircaloy, specifically operate such as Under：
By atomic percent Zr45Ti2Nb2Ta2Al8Co35Fe2Cu2Ni2Weighing Zr, Ti, Nb, Ta, Al, Co, Fe, Cu, Ni Pure element, and the mass percent purity of each element is not less than 99.0%, obtains melting raw material after mixing, it is spare；By institute Melting raw material be put into vacuum smelting furnace, adjust the vacuum of vacuum chamber of vacuum smelting furnace to 2 × 10-3Pa, and in matter Measure the lower progress melting of high-purity argon gas protection of percent purity >=99.999%, 2600 DEG C of smelting temperature；Melt back 4 times, obtains To Zr45Ti2Nb2Ta2Al8Co35Fe2Cu2Ni2Foundry alloy；The foundry alloy allowed still mass percent purity >= Under 99.999% high-purity argon gas protection, the foundry alloy is cooled down using the water jacketed copper crucible of vacuum smelting furnace, which closes Gold is 50 seconds by liquid to solid cooling time, then proceedes to keep the copper crucible water cooling state of vacuum smelting furnace, mother is closed Gold takes out after room temperature is continued cool in vacuum smelting furnace, then obtains the Zr of even tissue45Ti2Nb2Ta2Al8Co35Fe2Cu2Ni2 Alloy cast ingot, that is, tough the zircaloy of the height.
By Zr made from the present embodiment45Ti2Nb2Ta2Al8Co35Fe2Cu2Ni2Alloy cast ingot is intercepted wherein with wire cutting method Between part section, after being ground polishing, tested using X-ray diffraction and determine crystalline phase, the results showed that the crystalline phase of alloy is ZrCo phases and ZrAlCo eutectic phases；Scanning electron microscope tissues observed pattern is used at the same time, ZrAlCo eutectic phase crystal grain is uniform Dispersed precipitate is around ZrCo phase crystal grain；Interception specification is the alloy cast ingot sample of 2mm × 2mm × 4mm, tests its compression stress Performance is learned, then knows the yield strength 1330MPa, fracture strength 1640MPa, amount of plastic deformation 10% of the alloy cast ingot；Using The HCl immersion test beta alloy ingot castings of 1mol/L, it is 0.57 μm/year to learn its corrosion rate.
To sum up, the mechanical property of high tough zircaloy and the model parameter of corrosion resistance that various embodiments of the present invention obtain It is as shown in table 1 below afterwards：
The performance parameter of the high tough zircaloy of table 1
And by the various embodiments described above, the present invention can obtain the Zr-Al-Co alloys containing ZrCo phases, and pass through At least one of alloying Ti, Nb, Ta, Fe, Ni, Cu in Zr-Al-Co alloys, to improve intensity and the modeling of alloy at the same time Property deformability；Present invention selection Zr50Al10Co40Component based on alloy, the alloy are to be total to ZrCo phases and ZrAlCo The composite diphase material of crystalline phase, since ZrCo phases are B2 phase structures, can occur martensitic traoformation in deformation process, have excellent modeling Property deformability, ZrAlCo intermetallic compounds have higher hardness, and even dispersion is distributed in around ZrCo phases, can be played The effect of dispersion-strengtherning；Ti, Nb, Ta, Fe, Ni, Cu element are further added on the basis of the alloy and carries out solution strengthening, and is led to Control alloying element content is crossed to control institutional framework, plays the role of regulating and controlling alloy mechanical property and corrosion resistance.
Therefore, the tough zircaloy of height produced by the present invention has high compression yield strength (1100~1400MPa) and pressure Contracting fracture strength is (1350~1710MPa), while has good compressive plastic deformation performance and excellent corrosion resistance； The preparation method of the tough zircaloy of the height is also disclosed, whole preparation process is simply easily operated, it is only necessary in vacuum metling Directly cooled down after stove melting using the water of its copper crucible flows, avoid the forging in existing zircaloy production, roll The manufacturing procedures such as system, heat treatment, greatly reduce production cost；Therefore, the excellent performance of the comprehensive high-strength tough zircaloy of the present invention, It is set to have widened the selection of material for fields such as structural material, aerospace, medical instruments, i.e., with good application prospect.

Claims (6)

  1. A kind of 1. high tough zircaloy, it is characterised in that：The chemical molecular formula of the height is tough zircaloy is ZraAlbCocMd, in formula：
    A, b, c, d are atomic percentage；Wherein 45≤a≤50,8≤b≤10,35≤c≤40,2≤d≤5, and a+b+c+d= 100；M is at least one of Ti, Nb, Ta, Fe, Ni, Cu.
  2. A kind of 2. high tough zircaloy according to claim 1, it is characterised in that：The height is tough, and each of zircaloy forms member The mass percent purity of element is >=99.0%.
  3. A kind of 3. high tough zircaloy according to claim 1, it is characterised in that：The compression yield of the height is tough zircaloy Intensity is 1100~1400MPa, and compressed rupture strength is 1350~1710MPa.
  4. A kind of 4. high tough zircaloy according to claim 1, it is characterised in that：The height is tough, and zircaloy is in concentration Corrosion rate in the HCl of 1mol/L is less than 1 μm/year.
  5. A kind of 5. preparation method of high tough zircaloy as claimed in claim 1, it is characterised in that：The preparation method is included such as Lower concrete operation step：
    Step 1: dispensing：Zr is weighed by atomic percentaAlbCocMdEach component, and the quality percentage of each component It is not less than 99.0% than purity, obtains melting raw material after mixing, it is spare；
    Step 2: melting ZraAlbCocMdFoundry alloy：
    Melting raw material obtained by step 1 is put into vacuum smelting furnace, adjusts the vacuum of vacuum chamber of vacuum smelting furnace to 1 ×10-3~5 × 10-3Pa, and carry out melting, melting temperature under the high-purity argon gas protection of mass percent purity >=99.999% 2500~2800 DEG C of degree；Melt back more than 4 times, obtains ZraAlbCocMdFoundry alloy；
    Step 3: ZraAlbCocMdAlloy cast ingot cools down：
    By the foundry alloy that step 2 obtains under the high-purity argon gas protection of mass percent purity >=99.999%, vacuum smelting is utilized The water jacketed copper crucible of furnace cools down the foundry alloy, until foundry alloy is then proceeded to keep true by liquid cooled to solid-state The copper crucible water cooling state of empty smelting furnace, takes out after foundry alloy is continued cool to room temperature in vacuum smelting furnace, then must organize Uniform ZraAlbCocMdAlloy cast ingot, that is, tough the zircaloy of the height.
  6. 6. the preparation method of the tough zircaloy of height according to claim 5, it is characterised in that：The preparation method further includes step Rapid four, ZraAlbCocMdAlloy sample is processed：
    By Zr made from step 3aAlbCocMdAlloy cast ingot wire cutting method requires interception in-between according to required size Part, after being ground polishing to cutting rear surface, that is, obtains ZraAlbCocMdAlloy sample.
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