Summary of the invention
At the problem that prior art exists, the invention provides a kind of the have magnesium alloy of warm extrusion pressure characteristic and the preparation method of squeeze wood thereof, purpose is that preparation can be implemented in the magnesium alloy that 160 ~ 240 ℃ of following warm extrusions are pressed, its squeeze wood has 20 ~ 35% high-elongation.
Magnesium alloy of the present invention is Mg-Zn-(Cu or Ni) series magnesium alloy, by mass percentage, contains 3.0% ~ 6.0% Zn, 1.5% ~ 5.0% Cu or Ni, and 0 ~ 1.0% Y, Nd, Gd, Ce or MM, Mg are surplus.
Wherein MM is rich Ce mishmetal, and wherein by mass percentage, Ce content is at least 50%, and surplus is La, Nd and Pr.
Preparing the squeeze wood with high-elongation magnesium alloy of warm extrusion pressure characteristic of the present invention carries out according to following steps:
(1) adopts melting resistance furnace or combustion gas smelting furnace, under the protection of barium fluxing agent or No. five flux, with MAGNESIUM METAL fusing and be heated to ° C fusing of 730 ° of C ~ 740, press the mass percent of magnesium alloy, the Zn of adding 3.0% ~ 6.0%, 1.5% ~ 5.0% Cu or Ni, 0 ~ 1.0% Y, Nd, Gd, Ce or MM, the Mg-Zn-that obtains (Cu or Ni) series magnesium alloy melt adopts hexachloroethane and flux to purify, and melt is cooled to 660 ° of C ~ 680 ° C and casts after stirring;
(2) at SF
6+ CO
2Under mixed gas protected, adopt the cunning semicontinuous casting of low frequency electromagnetic, electromagnetic frequency is 30Hz, a.t. is 6000AT, and the casting specification is the magnesium alloy cast ingot blank of cross-sectional diameter 100 ~ 300mm, and the ingot blank that obtains was annealed 10 hours at 410 ± 10 times, then scale, strip off the skin, standby;
(3) adopt reverse squeezing device under 160 ~ 240 ℃ the condition to scale and the casting of Mg-Zn-(Cu or the Ni) series magnesium alloy after stripping off the skin ingot blank carry out reverse warm extrusion and press, extrusion ratio is 8 ~ 20, extrusion speed is 4.5 ~ 8m/min, obtains Mg-Zn-(Cu or Ni) series magnesium alloy extruded bars;
(4) to obtaining Mg-Zn-(Cu or Ni) series magnesium alloy extruded bars after the extruding, carry out T4 or T6 thermal treatment, namely in 400 ° of C solid solutions 2 hours or in 400 ° of C solid solutions after 2 hours again in 200 ° of C timeliness 15~30 hours.
Described SF
6+ CO
2SF in the mixed gas
6And CO
2Volume ratio is: 1:10.
Described reverse squeezing device comprises the extrusion stem of hollow, extrusion mould, container, extruding pad and extruding base, be equipped with container at the extruding base, the container inner bottom part is the extruding pad, extruding pad top is extrusion mould, the extrusion mould top is the extrusion stem of hollow, wherein extrusion mould is the right cylinder of hollow, right cylinder inside is the modular angle section from top to bottom successively, pre-work zone, sizing work zone and outlet section, modular angle is 30 ~ 45 °, the diameter of outlet section is greater than the diameter of work zone, pre-work zone diameter is greater than sizing work zone diameter, and the ratio of two land lengths is 0.5 ~ 0.8, and the sizing land length is 4 ~ 8mm.
Described reverse squeezing device is smeared the molybdenumdisulphide lithium soap grease at extrusion mould inwall, blank surface and container inwall in extrusion process.
Compared with prior art, the invention has the beneficial effects as follows:
(1) Mg-Zn-of the present invention (Cu or Ni) series magnesium alloy has and can carry out reverse warm extrusion compressive strain characteristics at 160 ~ 240 ℃, and squeeze wood has the high-ductility index.
(2) the reverse squeezing device of the present invention has adopted the little modular angle design of 30 ~ 45 ° of modular angles, adopts the design of two work zones simultaneously, has alleviated the high problem of magnesium alloy moment squeeze peak value, and has guaranteed the great surface quality of squeeze wood.
(3) after T4 or T6 thermal treatment, its unit elongation is 20% ~ 35% to Mg-Zn-of the present invention (Cu or Ni) series magnesium alloy at the 160 ° of reverse warm extrusion pressure bar of C ~ 240 ° C materials.
Embodiment
Reverse squeezing device of the present invention as shown in Figure 1, the extrusion stem 1, container 2, extrusion mould 3, extruding pad 4 and the extruding base 5 that comprise hollow, be equipped with container 2 at extruding base 5, container 2 inner bottom parts are extruding pads 4, extruding pad 4 tops are extrusion moulds 3, and extrusion mould 3 tops are extrusion stems 1 of hollow;
The structure of extrusion mould 3 as shown in Figure 2, extrusion mould 3 is right cylinders of a hollow, its inside is modular angle section 3-1, pre-work zone 3-2, sizing work zone 3-3 and outlet section 3-4 from top to bottom successively, the modular angle of modular angle section is 30 ~ 45 °, the diameter of outlet section 3-4 is greater than the diameter of work zone 3-2, pre-work zone diameter 3-2 is greater than sizing work zone diameter 3-3, and the length ratio of pre-work zone 3-2 and sizing work zone 3-3 is 0.5 ~ 0.8, and the length of sizing work zone 3-3 is 4 ~ 8mm.
Mg in the present embodiment, Zn and Cu adopt one-level magnesium ingot, one-level zinc ingot metal and one-level electrolytic copper to add, and Y, Nd or Gd adopt master alloy to add, and Ce or MM adopt pure metal, and flux is that market is bought.
Embodiment 1
Adopt the melting resistance furnace; under the protection of barium fluxing agent; with MAGNESIUM METAL fusing and be heated to 730 ° of C fusings; press the mass percent of magnesium alloy; the Zn of adding 4% and 3% Cu; the gained magnesium alloy fused mass carries out purifying treatment with hexachloroethane and No. five flux, and melt is cooled to 666 ° of C after stirring, be the SF of 1:10 in volume ratio
6And CO
2That forms is mixed gas protected following, adopt the cunning semicontinuous casting of low frequency electromagnetic to prepare magnesium alloy ingot blank, applying the electromagnetism condition is: electromagnetic frequency 30Hz, a.t. 6000AT, casting speed is 103mm/min, the water yield is 65L/min, obtaining specification is diameter 165mm, high 1800mm, chemical analysis consist of the magnesium alloy ingot blank of Mg-4.26Zn-3.06Cu, and accompanying drawing 4 is its typical cast structure; In 410 ± 10 annealing 10 hours, the cut-off footpath 46mm that strips off the skin after annealing finishes, high 120mm specification sample carries out reverse warm extrusion and presses under the temperature of 160 ° of C ~ 240 ° C.
Adopt reverse squeezing device as shown in Figures 1 and 2, magnesium alloy sample, mould, container and extruding pad all are heated to 160 ° of C ~ 240 ° C, be incubated 2 hours, on 300 tons of oil presses, with the extrusion speed extrusion magnesium alloy sample of 5.0m/min, obtain the magnesium alloy rod of diameter 12mm, its extrusion ratio is 17.4, before extruding, smear the molybdenumdisulphide lithium soap grease at extrusion mould inwall, blank surface and container inwall.To the Mg-4.26Zn-3.06Cu magnesium alloy rod that obtains in 400 ° of C solid solutions after 2 hours again in 200 ° of C timeliness 15 hours.As shown in Figure 3 tension specimen is processed in extruded bars sampling, carries out room temperature tensile at the Instron8032 drawing machine, draw speed is 2mm/min.Its heat treatment state room temperature tensile mechanical property is as shown in table 1, for: R
m=265MPa, yield strength R
P0.2=150 ~ 170MPa, unit elongation A=20 ~ 23%.
The extruded bar from magnesium alloy room temperature tensile mechanical property of table 1 example 1
Embodiment 2
Adopt the melting resistance furnace; under the protection of No. five flux; with MAGNESIUM METAL fusing and be heated to 740 ° of C fusings; press the mass percent of magnesium alloy; the Zn of adding 4%, 3% Cu and 0.4% Y; the gained magnesium alloy fused mass carries out purifying treatment with hexachloroethane and No. five flux, and melt is cooled to 670 ° of C after stirring, be the SF of 1:10 in volume ratio
6And CO
2That forms is mixed gas protected following, adopt the cunning semicontinuous casting of low frequency electromagnetic to prepare magnesium alloy ingot blank, applying the electromagnetism condition is: electromagnetic frequency 30Hz, a.t. 6000AT, casting speed is 80mm/min, and the water yield is 60L/min, and obtaining specification is the high 1800mm of diameter 165mm, chemical analysis consists of the magnesium alloy ingot blank of Mg-3.91Zn-2.78Cu-0.31Y, and accompanying drawing 5 is typical cast structure; In 410 ± 10 ° of C annealing 10 hours; The cut-off footpath 50mm that strips off the skin after annealing finishes, high 120mm specification sample carries out reverse warm extrusion and presses under the temperature of 180 ° of C.
Adopt reverse squeezing device as shown in Figures 1 and 2, magnesium alloy sample, mould, container and extruding pad all are heated to 180 ° of C, be incubated 2 hours, on 300 tons of oil presses, with the extrusion speed extrusion magnesium alloy sample of 5.0m/min, obtain the magnesium alloy rod of diameter 12mm, its extrusion ratio is 17.4, before extruding, smear the molybdenumdisulphide lithium soap grease at extrusion mould inwall, blank surface and container inwall.The Mg-3.91Zn-2.78Cu-0.31Y magnesium alloy rod that obtains is carried out T4 thermal treatment, in 400 ° of C solid solutions 2 hours.As shown in Figure 3 tension specimen is processed in extruded bars sampling, carries out room temperature tensile at the Instron8032 drawing machine, draw speed is 2mm/min.Its T4 heat treatment state room temperature tensile mechanical property is: R
m=207MPa, yield strength R
P0.2=81MPa, unit elongation A=34.8%.
Embodiment 3
Prepare the Mg-3.91Zn-2.78Cu-0.31Y extruded bar from magnesium alloy by example 2 methods, bar is carried out T6 thermal treatment, in 400 ° of C solid solutions after 2 hours, at 200 ℃ of timeliness 30h.As shown in Figure 3 tension specimen is processed in extruded bars sampling, carries out room temperature tensile at the Instron8032 drawing machine, draw speed is 2mm/min.Its T6 heat treatment state room temperature tensile mechanical property is: R
m=279MPa, yield strength R
P0.2=235MPa, unit elongation A=32.3%.
Embodiment 4
Adopt the melting resistance furnace; under the protection of No. five flux; with MAGNESIUM METAL fusing and be heated to 740 ° of C fusings; press the mass percent of magnesium alloy; the Zn of adding 5.5%, 3% Ni and 0.4% Y; the gained magnesium alloy fused mass carries out purifying treatment with hexachloroethane and No. five flux, and melt is cooled to 670 ° of C after stirring, be the SF of 1:10 in volume ratio
6And CO
2That forms is mixed gas protected following, adopt the cunning semicontinuous casting of low frequency electromagnetic to prepare magnesium alloy ingot blank, applying the electromagnetism condition is: electromagnetic frequency 30Hz, a.t. 6000AT, casting speed is 60mm/min, the water yield is 70L/min, obtaining specification is diameter 165mm, high 1600mm, chemical analysis consist of the magnesium alloy ingot blank of Mg-5.1Zn-2.91Ni-0.23Y, and accompanying drawing 6 is typical cast structure; In 410 ± 10 ° of C annealing 10 hours; The cut-off footpath 50mm that strips off the skin after annealing finishes, high 120mm specification sample carries out reverse warm extrusion and presses under the temperature of 180 ° of C.
Adopt reverse squeezing device as shown in Figures 1 and 2, magnesium alloy sample, mould, container and extruding pad all are heated to 180 ° of C, be incubated 2 hours, on 300 tons of oil presses, with the extrusion speed extrusion magnesium alloy sample of 5.0m/min, obtain the magnesium alloy rod of diameter 12mm, its extrusion ratio is 17.4, before extruding, smear the molybdenumdisulphide lithium soap grease at extrusion mould inwall, blank surface and container inwall.The Mg-5.1Zn-2.91Ni-0.23Y magnesium alloy rod that obtains is carried out T6 thermal treatment, in 400 ° of C solid solutions after 2 hours, at 200 ℃ of timeliness 24h.As shown in Figure 3 tension specimen is processed in extruded bars sampling, carries out room temperature tensile at the Instron8032 drawing machine, draw speed is 2mm/min.Its T6 heat treatment state room temperature tensile mechanical property is: R
m=284MPa, yield strength R
P0.2=270MPa, unit elongation A=27%.
Embodiment 5
Adopt the melting resistance furnace; under the protection of No. five flux; with MAGNESIUM METAL fusing and be heated to 740 ° of C fusings; press the mass percent of magnesium alloy; the Zn of adding 5%, 3% Ni and 0.5% Ce; the gained magnesium alloy fused mass carries out purifying treatment with hexachloroethane and No. five flux, and melt is cooled to 670 ° of C after stirring, be the SF of 1:10 in volume ratio
6And CO
2That forms is mixed gas protected following, adopt the cunning semicontinuous casting of low frequency electromagnetic to prepare magnesium alloy ingot blank, applying the electromagnetism condition is: electromagnetic frequency 30Hz, a.t. 6000AT, casting speed is 60mm/min, the water yield is 70L/min, obtaining specification is diameter 165mm, high 1600mm, chemical analysis consist of the magnesium alloy ingot blank of Mg-5.01Zn-2.89Ni-0.42Ce, and accompanying drawing 7 is typical cast structure; In 410 ± 10 ° of C annealing 10 hours; The cut-off footpath 50mm that strips off the skin after annealing finishes, high 120mm specification sample carries out reverse warm extrusion and presses under the temperature of 180 ° of C.
Adopt reverse squeezing device as shown in Figures 1 and 2, magnesium alloy sample, mould, container and extruding pad all are heated to 180 ° of C, be incubated 2 hours, on 300 tons of oil presses, with the extrusion speed extrusion magnesium alloy sample of 6.0m/min, obtain the magnesium alloy rod of diameter 12mm, its extrusion ratio is 17.4, before extruding, smear the molybdenumdisulphide lithium soap grease at extrusion mould inwall, blank surface and container inwall.The Mg-5.01Zn-2.89Ni-0.42Ce magnesium alloy rod that obtains is carried out T6 thermal treatment, in 400 ° of C solid solutions after 2 hours, at 200 ℃ of timeliness 24h.As shown in Figure 3 tension specimen is processed in extruded bars sampling, carries out room temperature tensile at the Instron8032 drawing machine, draw speed is 2mm/min.Its T6 heat treatment state room temperature tensile mechanical property is: R
m=275MPa, yield strength R
P0.2=260MPa, unit elongation A=25%.
Embodiment 6
Adopt the combustion gas smelting furnace; under the protection of No. five flux; with MAGNESIUM METAL fusing and be heated to 740 ° of C fusings; press the mass percent of magnesium alloy; the Zn of adding 5%, 4% Cu and 1.0% Nd; the gained magnesium alloy fused mass carries out purifying treatment with hexachloroethane and No. five flux, and melt is cooled to 660 ° of C after stirring, be the SF of 1:10 in volume ratio
6And CO
2That forms is mixed gas protected following, adopt the cunning semicontinuous casting of low frequency electromagnetic to prepare magnesium alloy ingot blank, applying the electromagnetism condition is: electromagnetic frequency 30Hz, a.t. 6000AT, casting speed is 60mm/min, the water yield is 70L/min, obtaining specification is diameter 165mm, high 1600mm, chemical analysis consist of the magnesium alloy ingot blank of Mg-4.77Zn-3.76Cu-0.82Nd, and accompanying drawing 7 is typical cast structure; In 410 ± 10 ° of C annealing 10 hours; The cut-off footpath 46mm that strips off the skin after annealing finishes, high 120mm specification sample carries out reverse warm extrusion and presses under the temperature of 180 ° of C.
Adopt reverse squeezing device as shown in Figures 1 and 2, magnesium alloy sample, mould, container and extruding pad all are heated to 180 ° of C, be incubated 2 hours, on 300 tons of oil presses, with the extrusion speed extrusion magnesium alloy sample of 4.5m/min, obtain the magnesium alloy rod of diameter 16mm, its extrusion ratio is 8.3, before extruding, smear the molybdenumdisulphide lithium soap grease at extrusion mould inwall, blank surface and container inwall.The Mg-4.77Zn-3.76Cu-0.82Nd magnesium alloy rod that obtains is carried out T6 thermal treatment, in 400 ° of C solid solutions after 2 hours, at 200 ℃ of timeliness 24h.
Embodiment 7
Adopt the combustion gas smelting furnace; under the protection of No. five flux; with MAGNESIUM METAL fusing and be heated to 740 ° of C fusings; press the mass percent of magnesium alloy; the Zn of adding 3%, 5.0% Ni and 1.0% Gd; the gained magnesium alloy fused mass carries out purifying treatment with hexachloroethane and No. five flux, and melt is cooled to 680 ° of C after stirring, be the SF of 1:10 in volume ratio
6And CO
2That forms is mixed gas protected following, adopt the cunning semicontinuous casting of low frequency electromagnetic to prepare magnesium alloy ingot blank, applying the electromagnetism condition is: electromagnetic frequency 30Hz, a.t. 6000AT, casting speed is 60mm/min, the water yield is 70L/min, obtaining specification is diameter 165mm, high 1600mm, chemical analysis consist of the magnesium alloy ingot blank of Mg-2.98Zn-4.89Ni-0.94Gd, and accompanying drawing 7 is typical cast structure; In 410 ± 10 ° of C annealing 10 hours; The cut-off footpath 46mm that strips off the skin after annealing finishes, high 120mm specification sample carries out reverse warm extrusion and presses under the temperature of 220 ° of C.
Adopt reverse squeezing device as shown in Figures 1 and 2, magnesium alloy sample, mould, container and extruding pad all are heated to 220 ° of C, be incubated 2 hours, on 300 tons of oil presses, with the extrusion speed extrusion magnesium alloy sample of 7.0m/min, obtain the magnesium alloy rod of diameter 12mm, its extrusion ratio is 14.6, before extruding, smear the molybdenumdisulphide lithium soap grease at extrusion mould inwall, blank surface and container inwall.The Mg-3.98Zn-4.89Ni-0.94Gd magnesium alloy rod that obtains is carried out T4 thermal treatment, in 400 ° of C solid solutions 2 hours.
Embodiment 8
Adopt the melting resistance furnace; under the protection of No. five flux; with MAGNESIUM METAL fusing and be heated to 740 ° of C fusings; press the mass percent of magnesium alloy; the Zn of adding 6%, 2% Ni and 0.5% MM; the gained magnesium alloy fused mass carries out purifying treatment with hexachloroethane and No. five flux, and melt is cooled to 680 ° of C after stirring, be the SF of 1:10 in volume ratio
6And CO
2That forms is mixed gas protected following, adopt the cunning semicontinuous casting of low frequency electromagnetic to prepare magnesium alloy ingot blank, applying the electromagnetism condition is: electromagnetic frequency 30Hz, a.t. 6000AT, casting speed is 60mm/min, the water yield is 70L/min, obtaining specification is diameter 165mm, high 1600mm, chemical analysis consist of the magnesium alloy ingot blank of Mg-6.0Zn-1.90Ni-0.44MM, and accompanying drawing 7 is typical cast structure; In 410 ± 10 ° of C annealing 10 hours; The cut-off footpath 50mm that strips off the skin after annealing finishes, high 120mm specification sample carries out reverse warm extrusion and presses under the temperature of 200 ° of C.
Adopt reverse squeezing device as shown in Figures 1 and 2, magnesium alloy sample, mould, container and extruding pad all are heated to 200 ° of C, be incubated 2 hours, on 300 tons of oil presses, with the extrusion speed extrusion magnesium alloy sample of 8.0m/min, obtain the magnesium alloy rod of diameter 12mm, its extrusion ratio is 17.4, before extruding, smear the molybdenumdisulphide lithium soap grease at extrusion mould inwall, blank surface and container inwall.The Mg-6.0Zn-1.90Ni-0.44MM magnesium alloy rod that obtains is carried out T4 thermal treatment, in 400 ° of C solid solutions 2 hours.