CN103290297B - Zirconium-molybdenum-magnesium-containing alloy and preparation technique thereof - Google Patents
Zirconium-molybdenum-magnesium-containing alloy and preparation technique thereof Download PDFInfo
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Abstract
The invention discloses a zirconium-molybdenum-magnesium-containing alloy and a preparation technique thereof. The zirconium-molybdenum-magnesium-containing alloy comprises the following ingredients in percentage by weight: 26-38% of Mg, 23-34% of Mo, 4-5% of Nb, 2-4% of Zr, 2-6% of Ca, less than or equal to 0.05% of Fe, less than or equal to 0.05% of C, less than or equal to 0.05% of N, less than or equal to 0.05% of H, less than or equal to 0.06% of O, and the balance of Ni. By controlling the ingredients and machining mode of a material, the zirconium-molybdenum-magnesium-containing alloy not only has a high strength equivalent to that of the aluminum alloy, has good performance stability after being used at room temperature, and the strength of the zirconium-molybdenum-magnesium-containing alloy can also be improved by 1.5-3 times compared with the existing zirconium-molybdenum-magnesium-containing alloy.
Description
Technical field:
The invention belongs to Material Field, relate to a kind of containing zirconium molybdenum magnesium alloy, especially a kind of low impurity content is containing zirconium molybdenum magnesium alloy and cold working thereof and heat treating method
Background technology:
MAGNESIUM METAL is argenteous metal, and matter is hard, slightly ductility.Magnesium is mainly for the manufacture of light metal alloy, containing zirconium molybdenum magnesium alloy, there is the excellent feature such as toughness plasticity, solidity to corrosion, processibility, and low cost of manufacture, simultaneously, alloy-free element adds environmentally compatible, is the structured material being widely used in the fields such as military project national defence, aerospace, medical treatment.But because the intensity containing zirconium molybdenum magnesium alloy is lower, as structured material, range of application is restricted.
At present, in industrial application, improving containing the most ripe, the most effective means of zirconium molybdenum magnesium alloy strength is carry out refined crystalline strengthening.The principle of refined crystalline strengthening can be explained with hall-Petch formula: because the crystal boundary resistance to deformation in polycrystal is larger, and the distortion of each crystal grain will be subject to pining down of surrounding grains, therefore multicrystal room temperature strength always improves along with the refinement (i.e. the increase of the crystal boundary total area) of crystal grain.The available hall-Petch formula of relation between polycrystal yield strength σ s and average grain diameter d describes: σ
s=σ
0+ kd
-1/2.For various grain sizes containing zirconium molybdenum magnesium alloy, when grain-size is 7 ~ 8 grades, intensity is about 400Mpa, and when grain-size reaches 11 ~ 12 grades, intensity can improve 70 ~ 100Mpa.This has absolutely proved that refined crystalline strengthening is effective for the lifting of the strength of materials.
Summary of the invention:
The object of the invention is to the shortcoming overcoming above-mentioned prior art, there is provided a kind of containing zirconium molybdenum magnesium alloy and preparation technology thereof, adopt containing the method for adding the element such as molybdenum, niobium in zirconium molybdenum magnesium alloy containing zirconium molybdenum magnesium alloy, obtained by cold working and heat treatment mode and contain zirconium molybdenum magnesium alloy higher than existing intensity 2 ~ 3 times.
The object of the invention is to solve by the following technical programs:
A kind of containing zirconium molybdenum magnesium alloy, described containing Mg 26-38wt%, Mo23-34wt%, Nb 4-5wt%, Zr 2-4wt%, Ca 2-6wt%, Fe≤0.05wt%, C≤0.05wt%, N≤0.05wt%, H≤0.05wt%, O≤0.06wt% in zirconium molybdenum magnesium alloy, all the other are Ni.
The described preparation technology containing zirconium molybdenum magnesium alloy, comprises the steps:
(1) melting: adopt magnesium powder, molybdenum powder, nickel powder, niobium powder, zirconium powder, calcium powder to be raw material, melting in the tungsten crucible that thermodynamic stability is good, the purity>=99.9wt% of tungsten crucible; Molybdenum powder, nickel powder, niobium powder and zirconium powder are mixed in rear loading tungsten crucible, magnesium powder and calcium powder load hopper, add in the melting later stage; First by pumping high vacuum in body of heater, in stove, vacuum tightness is 1 × 10
-1pa, leak rate < 0.2Pa/min, is filled with argon gas, makes vacuum tightness be 0.1MPa; Energising, the molybdenum powder that melting mixes, nickel powder, niobium powder and zirconium powder, after molybdenum powder, nickel powder, niobium powder and zirconium powder all melt, Turnover bunker, adds magnesium powder and calcium powder, after magnesium powder and calcium powder all melt, leave standstill 5-10 minute, 2050-2150 degree Celsius of casting, obtain containing zirconium molybdenum magnesium alloy.
The granularity of described magnesium powder, molybdenum powder, nickel powder, niobium powder, zirconium powder or calcium powder is as 100-300 order.
(2) cold working: after adopting kicker annealing, the mode of room temperature drawing is processed, and annealing temperature is 750 DEG C, time 1h, must not heat-treat in the middle of each drawing passes; Passage accumulation cold deformation >=70%;
(3) finished products thermal treatment: temperature≤400 DEG C, time≤1h.
The described optimal way containing zirconium molybdenum magnesium alloy preparation technology is:
The described excellent silk material made containing zirconium molybdenum magnesium alloy, the diameter Ф≤12mm of described excellent silk material, the tensile strength >=750Mpa of excellent silk material, unit elongation >=18%.
The present invention is by controlling composition and the processing mode of material, and make not only have containing zirconium molybdenum magnesium alloy the high strength being equivalent to aluminium alloy, at room temperature use and have good stability, its strength ratio is existing high 1.5 ~ 3 times containing zirconium molybdenum magnesium alloy; The plasticity-of zirconium is good, and corrosion-resistant, after with the addition of zirconium, can improve its corrosion resistance in molybdenum magnesium alloy, improves that it is moulding.
Embodiment:
Below the present invention is described in further detail:
The object of the invention is to adopt low impurity content containing zirconium molybdenum magnesium alloy, by suitable processing mode obtain higher than existing intensity 1.5 ~ 3 times containing zirconium molybdenum magnesium alloy.This invention, by controlling composition and the processing mode of material, makes not only have quite high intensity containing zirconium molybdenum magnesium alloy, at room temperature uses and have good stability.
Along with the increase of deflection, a large amount of feather organization and twin-plane boundary are there is containing in zirconium molybdenum magnesium alloy.Twin-plane boundary to the mode of action of material reinforcement and crystal boundary similar, when there is a large amount of twin-plane boundaries in material structure, dislocation will be difficult to be out of shape through twin-plane boundary, interface is caused to fill in long-pending a large amount of dislocations, cause stress concentration, cause work hardening, reach the object promoting the strength of materials.Therefore, the deflection containing zirconium molybdenum magnesium alloy is larger, mechanical twin is more, and twin size is less, and the strength of materials will be higher.
The heat treating regime adopted in the present invention is as follows:
Under the prerequisite of not loss material intensity, in order to improve the plasticity containing zirconium molybdenum magnesium alloy, suitably improving the unit elongation containing zirconium molybdenum magnesium alloy, can low-temperature heat treatment be carried out.Thermal treatment is formulated: temperature≤400 DEG C, time≤1h.
Embodiment 1:
A kind of containing zirconium molybdenum magnesium alloy, described containing Mg 26wt%, Mo 32wt%, Nb 5wt%, Zr 4wt%, Ca 6wt%, Fe≤0.05wt%, C≤0.05wt%, N≤0.05wt%, H≤0.05wt%, O≤0.06wt% in zirconium molybdenum magnesium alloy, all the other are Ni.
Embodiment 2:
A kind of containing zirconium molybdenum magnesium alloy, described containing Mg 38wt%, Mo 34wt%, Nb 4wt%, Zr 2wt%, Ca 2wt%, Fe≤0.05wt%, C≤0.05wt%, N≤0.05wt%, H≤0.05wt%, O≤0.06wt% in zirconium molybdenum magnesium alloy, all the other are Ni.
Embodiment 3:
A kind of containing zirconium molybdenum magnesium alloy, described containing Mg 30wt%, Mo 23wt%, Nb 4.5wt%, Zr 3wt%, Ca 4wt%, Fe≤0.05wt%, C≤0.05wt%, N≤0.05wt%, H≤0.05wt%, O≤0.06wt% in zirconium molybdenum magnesium alloy, all the other are Ni.
Embodiment 4:
A kind of containing zirconium molybdenum magnesium alloy, described containing Mg 32wt%, Mo 30wt%, Nb 4wt%, Zr 2wt%, Ca 5wt%, Fe≤0.05wt%, C≤0.05wt%, N≤0.05wt%, H≤0.05wt%, O≤0.06wt% in zirconium molybdenum magnesium alloy, all the other are Ni.
Embodiment 5:
A kind of containing zirconium molybdenum magnesium alloy, described containing Mg 33wt%, Mo 32wt%, Nb 5wt%, Zr 2wt%, Ca 4wt%, Fe≤0.05wt%, C≤0.05wt%, N≤0.05wt%, H≤0.05wt%, O≤0.06wt% in zirconium molybdenum magnesium alloy, all the other are Ni.
Embodiment 6:
A kind of containing zirconium molybdenum magnesium alloy, described containing Mg 28wt%, Mo 24wt%, Nb 5wt%, Zr4wt%, Ca 6wt%, Fe≤0.05wt%, C≤0.05wt%, N≤0.05wt%, H≤0.05wt%, O≤0.06wt% in zirconium molybdenum magnesium alloy, all the other are Ni.
The described preparation technology containing zirconium molybdenum magnesium alloy, comprises the steps:
(1) melting: adopt magnesium powder, molybdenum powder, nickel powder, niobium powder, zirconium powder, calcium powder to be raw material, melting in the tungsten crucible that thermodynamic stability is good, the purity>=99.9wt% of tungsten crucible; Molybdenum powder, nickel powder, niobium powder and zirconium powder are mixed in rear loading tungsten crucible, magnesium powder and calcium powder load hopper, add in the melting later stage; First by pumping high vacuum in body of heater, in stove, vacuum tightness is 1 × 10
-1pa, leak rate < 0.2Pa/min, is filled with argon gas, makes vacuum tightness be 0.1MPa; Energising, the molybdenum powder that melting mixes, nickel powder, niobium powder and zirconium powder, after molybdenum powder, nickel powder, niobium powder and zirconium powder all melt, Turnover bunker, adds magnesium powder and calcium powder, after magnesium powder and calcium powder all melt, leave standstill 5-10 minute, 2050-2150 degree Celsius of casting, obtain containing zirconium molybdenum magnesium alloy.
The granularity of described magnesium powder, molybdenum powder, nickel powder, niobium powder, zirconium powder or calcium powder is as 100-300 order.
(2) cold working: after adopting kicker annealing, the mode of room temperature drawing is processed, and annealing temperature is 750 DEG C, time 1h, must not heat-treat in the middle of each drawing passes; Passage accumulation cold deformation >=70%;
(3) finished products thermal treatment: temperature≤400 DEG C, time≤1h.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, although the present invention discloses as above with preferred embodiment, but and be not used to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, when the method and technology contents that can utilize above-mentioned announcement are made a little change or be modified to the Equivalent embodiments of equivalent variations, in every case be the content not departing from technical solution of the present invention, according to any simple modification that technical spirit of the present invention is done above embodiment, equivalent variations and modification, still belong in the scope of technical solution of the present invention.
Claims (6)
1. one kind contains zirconium molybdenum magnesium alloy, it is characterized in that: described containing in zirconium molybdenum magnesium alloy contains Mg 26-38wt%, Mo 23-34wt%, Nb 4-5wt%, Zr 2-4wt%, Ca 2-6wt%, Fe≤0.05wt%, C≤0.05wt%, N≤0.05wt%, H≤0.05wt%, O≤0.06wt%, and all the other are Ni.
2. as claimed in claim 1 containing zirconium molybdenum magnesium alloy, it is characterized in that: described containing Mg 26wt%, Mo 32wt%, Nb 5wt%, Zr 4wt%, Ca 6wt%, Fe≤0.05wt%, C≤0.05wt%, N≤0.05wt%, H≤0.05wt%, O≤0.06wt% in zirconium molybdenum magnesium alloy, all the other are Ni.
3. as claimed in claim 1 containing zirconium molybdenum magnesium alloy, it is characterized in that: described containing Mg 38wt%, Mo 34wt%, Nb 4wt%, Zr 2wt%, Ca 2wt%, Fe≤0.05wt%, C≤0.05wt%, N≤0.05wt%, H≤0.05wt%, O≤0.06wt% in zirconium molybdenum magnesium alloy, all the other are Ni.
4., as claimed in claim 1 containing zirconium molybdenum magnesium alloy preparation technology, it is characterized in that, comprise the steps:
(1) melting: adopt magnesium powder, molybdenum powder, nickel powder, niobium powder, zirconium powder, calcium powder to be raw material, melting in the tungsten crucible that thermodynamic stability is good, the purity>=99.9wt% of tungsten crucible; Molybdenum powder, nickel powder, niobium powder and zirconium powder are mixed in rear loading tungsten crucible, magnesium powder and calcium powder load hopper, add in the melting later stage; First by pumping high vacuum in body of heater, in stove, vacuum tightness is 1 × 10
-1pa, leak rate < 0.2Pa/min, is filled with argon gas, makes vacuum tightness be 0.1MPa; Energising, the molybdenum powder that melting mixes, nickel powder, niobium powder and zirconium powder, after molybdenum powder, nickel powder, niobium powder and zirconium powder all melt, Turnover bunker, adds magnesium powder and calcium powder, after magnesium powder and calcium powder all melt, leave standstill 5-10 minute, 2050-2150 degree Celsius of casting, obtain containing zirconium molybdenum magnesium alloy;
(2) cold working: after adopting kicker annealing, the mode of room temperature drawing is processed, and annealing temperature is 750 DEG C, time 1h, must not heat-treat in the middle of each drawing passes; Passage accumulation cold deformation >=70%;
(3) finished products thermal treatment: temperature≤400 DEG C, time≤1h.
5. as claimed in claim 4 containing zirconium molybdenum magnesium alloy preparation technology, it is characterized in that: the described excellent silk material made containing zirconium molybdenum magnesium alloy, the diameter Ф≤12mm of described excellent silk material, the tensile strength >=750MPa of excellent silk material, unit elongation >=18%.
6., as claimed in claim 4 containing zirconium molybdenum magnesium alloy preparation technology, it is characterized in that: the granularity of described magnesium powder, molybdenum powder, nickel powder, niobium powder, zirconium powder or calcium powder is 100-300 order.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09272934A (en) * | 1996-02-05 | 1997-10-21 | Mitsubishi Materials Corp | Heat transfer tube for refuse incinerating waste heat boiler excellent in high temperature corrosion resistance |
| JPH10204563A (en) * | 1997-01-22 | 1998-08-04 | Mitsubishi Materials Corp | Composite heat exchanger tube for waste heat boiler using exhaust gas of refuse incinerator excellent in high temperature corrosion resistance |
| CN101600814A (en) * | 2006-12-29 | 2009-12-09 | 阿海珐核能公司 | To nickel-base alloy, in particular for fuel assembly for nuclear reactor and be used for heat treating method that the auxiliary cracking of environment of the nickel-base alloy of nuclear reactor desensitizes and with the parts of the alloy manufacturing of so handling |
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- 2013-06-06 CN CN201310224307.5A patent/CN103290297B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09272934A (en) * | 1996-02-05 | 1997-10-21 | Mitsubishi Materials Corp | Heat transfer tube for refuse incinerating waste heat boiler excellent in high temperature corrosion resistance |
| JPH10204563A (en) * | 1997-01-22 | 1998-08-04 | Mitsubishi Materials Corp | Composite heat exchanger tube for waste heat boiler using exhaust gas of refuse incinerator excellent in high temperature corrosion resistance |
| CN101600814A (en) * | 2006-12-29 | 2009-12-09 | 阿海珐核能公司 | To nickel-base alloy, in particular for fuel assembly for nuclear reactor and be used for heat treating method that the auxiliary cracking of environment of the nickel-base alloy of nuclear reactor desensitizes and with the parts of the alloy manufacturing of so handling |
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