CN103422037B - Technology for separation of recrystallization and precipitated phase precipitation of low scandium Al-Mg alloy - Google Patents
Technology for separation of recrystallization and precipitated phase precipitation of low scandium Al-Mg alloy Download PDFInfo
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- CN103422037B CN103422037B CN201210162715.8A CN201210162715A CN103422037B CN 103422037 B CN103422037 B CN 103422037B CN 201210162715 A CN201210162715 A CN 201210162715A CN 103422037 B CN103422037 B CN 103422037B
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Abstract
The invention relates to a technology for separation of recrystallization and precipitated phase precipitation of low scandium Al-Mg alloy. In the technology, ingot castings are subjected to cold rolling at room temperature and the deformation is no less than 70%. then the alloy after cold rolling treatment is subjected to salt bath anneal for 1s-5min at the temperature interval of 340-525 DEG C, then is taken out and subjected to water quenching rapidly. Finally, the alloy after salt bath anneal is subjected to second anneal for 3h-36h at the temperature of 275-325 DEG C. The average crystal grain size of the alloy is less than 10 micrometers through the technology, and the average size of Al3(Sc, Zr) precipitation strengthening phase is below 10 nanometers.
Description
Technical field
The invention belongs to Novel aluminum alloy material field, be specifically related to a kind of technique being separated low scandium Al-Mg alloy recrystallization and precipitated phase and separating out.
Background technology
Mo-bearing granitoid because intensity is high, plasticity and toughness are good, corrosion resisting property and welding property excellent, come into one's own in scientific research and engineer applied field.In conventional commercial Al-Mg-Sc alloy, scandium content is generally 0.15 ~ 0.3wt.%, and its effect mainly contains following 2 points: one is in process of setting, form nascent Al
3original as-cast grain is refined to 40 ~ 60 microns by (Sc, Zr); Two is the nano level Al by separating out in subsequent thermal processing and thermal treatment
3(Sc, Zr) carrys out reinforced alloys mutually.But because the price of scandium is high, the application of such material is limited by very large, is only confined to some special dimensions such as Aeronautics and Astronautics.In Al-Mg-Sc alloy, if replaced with nascent Al by other mode
3(Sc, Zr) phase crystal grain thinning, this development and utilization for alloy will have great significance.
Due to nascent Al
3(Sc, Zr) is the most effective alterant in the Al alloy found up to now mutually, therefore wants that the method by adding alterant in fusion process reaches nascent Al
3the effect possibility of (Sc, Zr) phase crystal grain thinning is little.And for general wrought aluminium alloy, the grain-size of refining alloy can be carried out by the thermal treatment generation recrystallize after hot-work or cold deformation.But for Al-Mg-Sc alloy, the recrystallization temperature of alloy is very high, this is mainly subject to the impact containing the precipitated phase of scandium in alloy.Alloy through the process of a homogenizing annealing, can separate out the nano level Al of a large amount of disperse in this process after casting
3(Sc, Zr) phase, their strong pinning crystal boundaries, hinder the carrying out of recrystallize.And alloy is after cold deformation, even if annealing temperature be raised to close near alloy melting point, recrystallize also can not fully carry out.Therefore think having disperse nanometer Al
3more tiny crystal grain is obtained by recrystallize very difficult in the alloy that (Sc, Zr) separates out mutually.
Recently, with waiting channel pressings technology (ECAP), Al-Mg-Sc alloy is carried out large viscous deformation at a certain temperature, make its occurrence dynamics recrystallize and the research work of crystal grain thinning has obtained and carries out fully, and the grain-size of alloy can be refine to several micron even level of submicron, but this technology has an obvious defect, namely while crystal grain thinning, the nanometer Al in alloy
3(Sc, Zr) also there occurs alligatoring mutually, and this can reduce the strengthening effect of precipitated phase greatly.
Summary of the invention
The object of this invention is to provide the low scandium Al-Mg alloy of a kind of separation (without nascent Al in process of setting
3(Sc, Zr) separates out crystal grain thinning mutually) technique that recrystallize and precipitated phase are separated out, this technique makes it that recrystallize occur and obtains the crystal grain less than the common Al-Mg-Sc alloy having primary phase to separate out, thus avoids with nascent Al
3(Sc, Zr) carrys out the consumption of scandium in the alloy that crystal grain thinning causes mutually, the intensity increase simultaneously brought because of grain refining can also make up in a part of low scandium Al-Mg alloy because of dispersion-strengthened phase amount reduce caused by the loss of intensity.For avoiding the strengthening effect of the high temperature annealing in recrystallization process to precipitated phase to impact, recrystallization process is at nano level Al
3complete before the precipitation of (Sc, Zr) phase.Through the low-temperature annealing of subordinate phase, the nano level Al of disperse
3(Sc, Zr) separates out mutually, and reinforced alloys.
The invention provides a kind of technique being separated low scandium Al-Mg alloy recrystallization and precipitated phase and separating out, the method step is as follows: 1) carry out cold rolling in room temperature to ingot casting, deflection is not less than 70%; 2) alloy through step 1) process is carried out to the liquid annealing of 1 second ~ 5 minutes in 340 ~ 525 DEG C of temperature ranges, and take out shrend rapidly; 3) 275 ~ 325 DEG C time, second annealing in 3 hours ~ 36 hours is carried out to the alloy through liquid annealing.
The technique that separation provided by the invention low scandium Al-Mg alloy recrystallization and precipitated phase are separated out, in described step 1), ingot casting is low scandium Al-Mg alloy, and by element mass percent, the chemical composition of this alloy is as follows: magnesium: 4.5-6.0%; Manganese: 0.30-0.60%; Scandium: 0.05-0.12%; Zirconium: 0.05-0.15%; Surplus is aluminium and inevitable impurity.
The technique that separation provided by the invention low scandium Al-Mg alloy recrystallization and precipitated phase are separated out, in described step 1) after cold rolling, rolling direction with roll crystal grain in plane that face normal direction formed and significantly elongated, and the hardness value in this face is not less than 110HV1.
The technique that separation provided by the invention low scandium Al-Mg alloy recrystallization and precipitated phase are separated out, described step 2) in after liquid annealing, alloy generation perfect recrystallization, average grain size is less than 10 microns, without nano level Al in matrix
3(Sc, Zr) precipitation phase is separated out, and hardness value is 78 ~ 90HV1.
The technique that separation provided by the invention low scandium Al-Mg alloy recrystallization and precipitated phase are separated out, in described step 3) after second annealing, Al
3(Sc, Zr) precipitation phase separate out, its mean sizes below 10 nanometers, alloy rigidity value rise 10 ~ 20HV1.
Its principle of work is:
For the magnalium ingot casting of oversaturated low scandium content, when annealing after distortion, recrystallize can be there is and precipitated phase separates out two physical processes in the present invention.When certain deflection, when rate of heating is enough fast, when annealing temperature is enough high, recrystallization process can complete before precipitated phase is separated out, so just recrystallize and precipitated phase can be separated out two processes separately, and controlled the precipitation of precipitated phase by follow-up thermal treatment, thus do not affect again the strengthening effect of precipitated phase while obtaining compared with fine grain size.
(1) the Al-Mg alloy of specific scandium content.It is 0.05-0.12wt.% that specific scandium content refers to scandium content in this alloy.Why being selected within the scope of this by scandium content, is because when scandium too high levels, and alloy can directly separate out nascent Al in process of setting on the one hand
3(Sc, Zr) phase, this consumes valuable scandium element; On the other hand, alloy is in hypersaturated state after solidification, and in matrix, scandium concentration also can be higher, nano level Al when alloy is heated
3the motivating force that (Sc, Zr) separates out mutually is comparatively large, and this precipitated phase is once separate out, will pinning dislocation and grain boundary strongly, is unfavorable for subsequent step 2) generation of middle recrystallize and carrying out.And when scandium content is too low, alloy is at subsequent step 3) the middle nano level Al separated out
3very little, strengthening effect is very weak for (Sc, Zr) phase amount, also just loses the effect adding scandium element.
(2) certain deflection cold rolling under room temperature.It is cold rolling in this link that to refer to rolling temperature identical with envrionment temperature; The rolling of certain deflection refers to the rolling deformation that reduced down in thickness amount is not less than 70%.Why selecting rolling at ambient temperature, is that alloy is easily replied because the stacking fault energy of aluminium alloy is higher.When rolling temperature is too high, alloy returns degree is larger, and deformation energy is little, is unfavorable for subsequent step 2) in the generation of recrystallize.Equally, why will implement the rolling deformation that reduced down in thickness amount is not less than 70%, be also mainly have enough deformation energies in alloy to ensure, increases the Enhancing Nucleation Density of alloy recrystallize in subsequent anneal process.
(3) liquid annealing in specified temp interval.Refer to the liquid annealing in 340 DEG C ~ 525 DEG C temperature ranges, the alloy through step 1) process carried out 1 second ~ 5 minutes, and take out shrend.Alloy through liquid annealing and after shrend, should possess three essential characteristics.First, its average grain size should be less than 10 microns, namely possesses the grain structure feature just completing primary recrystallization.Secondly, without nano level Al in microstructure
3(Sc, Zr) precipitation phase is separated out.3rd, the hardness value of alloy is 78 ~ 90HV1.These three essential characteristics are that alloy is at subsequent step 3) in form disperse educt and reach the precondition of best strengthening effect, very crucial.
(4) second annealing in specified temp interval.Referring to 275 ~ 325 DEG C time through step 2) alloy that processes carries out second annealing in 3 hours ~ 36 hours.In this annealing, super saturated solid solution cognition is decomposed, and forms the nano level Al of disperse
3(Sc, Zr) precipitation phase is separated out, and mean sizes is below 10 nanometers, and what cause alloy rigidity rises to 10 ~ 20HV1.Annealing time is too short, and precipitated phase is separated out insufficient; Annealing time is long, and precipitated phase can alligatoring.
The invention has the advantages that:
1, compared to the common Al-Mg alloy containing scandium with nascent Al
3grain refining to 40 ~ 60 microns, makes grain-size obtain more significant refinement by the method for recrystallize, can reach less than 10 microns by (Sc, Zr) precipitated phase in this alloy.
2, by being separated recrystallize and Precipitation two processes, while crystal grain thinning, the strengthening effect of precipitated phase is not affected.
Accompanying drawing explanation
Fig. 1 is Al-5.5Mg-0.5Mn-0.09Sc-0.09Zr (mass percent) As-cast Microstructure (opticmicroscope 50 ×);
Fig. 2 is the rolling state tissue (opticmicroscope 100 ×) after Al-5.5Mg-0.5Mn-0.09Sc-0.09Zr (mass percent) alloy cold rolling 90%;
Fig. 3 is the recrystallized structure (opticmicroscope 500 ×) of Al-5.5Mg-0.5Mn-0.09Sc-0.09Zr (mass percent) alloy after salt bath 375 DEG C annealing 20s;
Fig. 4 is that Al-5.5Mg-0.5Mn-0.09Sc-0.09Zr (mass percent) alloy is at 300 DEG C of annealing nano level Al after 24 hours
3(Sc, Zr) precipitated phase pattern;
Fig. 5 anneals 20 seconds through 375 DEG C after Al-5.5Mg-0.5Mn-0.09Sc-0.09Zr (mass percent) alloy rolling 90% and the changes in hardness in 36 hours period of annealing at 300 DEG C in salt bath.
Embodiment
Following examples will be further described the present invention, but not thereby limiting the invention.
Embodiment 1:
Step 1:Al-5.5Mg-0.5Mn-0.09Sc-0.07Zr (mass percent, as follows) cast alloy (Fig. 1 is shown in its metallographic structure) in cold rolling at room temperature distortion 90%, after distortion roll to and roll face normal direction metallographic structure planar as shown in Figure 2;
Step 2: 375 DEG C of liquid annealings 20 seconds, the average grain size occurred after recrystallize is 5 microns, and corresponding metallographic structure is as shown in Figure 3;
Step 3: 300 DEG C of annealing 36 hours, Al
3(Sc, Zr) precipitation phase is separated out, and size is less than 10 nanometers, and its transmission photo as shown in Figure 4.
After liquid annealing, hardness is 83HV1, and after second annealing, hardness is 101HV1, and average grain size is 5 microns.The changes in hardness curve of liquid annealing (step 2) and second annealing (step 3) process interalloy as shown in Figure 5.
Embodiment 2:
Step 1:Al-5.5Mg-0.5Mn-0.09Sc-0.07Zr (mass percent, as follows) cast alloy is in cold rolling at room temperature distortion 90%;
Step 2: 340 DEG C of liquid annealings 60 seconds;
Step 3: 300 DEG C of annealing 3 hours.
After liquid annealing, hardness is 84HV1, and after second annealing, hardness is 101HV1, and average grain size is 4.5 microns.
Embodiment 3:
Step 1:Al-5.5Mg-0.5Mn-0.09Sc-0.07Zr (mass percent, as follows) cast alloy is in cold rolling at room temperature distortion 90%;
Step 2: 450 DEG C of liquid annealings 20 seconds;
Step 3: 300 DEG C of annealing 36 hours.
After liquid annealing, hardness is 80HV1, and after second annealing, hardness is 97HV1, and average grain size is 8 microns.
Embodiment 4:
Step 1:Al-5.5Mg-0.5Mn-0.09Sc-0.07Zr (mass percent, as follows) cast alloy is in cold rolling at room temperature distortion 90%;
Step 2: 525 DEG C of liquid annealings 1 second;
Step 3: 300 DEG C of annealing 24 hours.
After liquid annealing, hardness is 78HV1, and after second annealing, hardness is 95HV1, and average grain size is 10 microns.
Embodiment 5:
Step 1:Al-5.5Mg-0.5Mn-0.09Sc-0.09Zr (mass percent, as follows) cast alloy is in cold rolling at room temperature distortion 70%;
Step 2: 350 DEG C of liquid annealings 60 seconds;
Step 3: 300 DEG C of annealing 3 hours.
After liquid annealing, hardness is 88HV1, and after second annealing, hardness is 103HV1, and average grain size is 5 microns.
Embodiment 6:
Step 1:Al-5.5Mg-0.5Mn-0.09Sc-0.09Zr (mass percent, as follows) cast alloy is in cold rolling at room temperature distortion 70%;
Step 2: 400 DEG C of liquid annealings 20 seconds;
Step 3: 300 DEG C of annealing 36 hours.
After liquid annealing, hardness is 80HV1, and after second annealing, hardness is 98HV1, and average grain size is 8 microns.
Embodiment 7:
Step 1:Al-5.5Mg-0.5Mn-0.05Sc-0.06Zr (mass percent, as follows) cast alloy is in cold rolling at room temperature distortion 70%;
Step 2: 450 DEG C of liquid annealings 30 seconds;
Step 3: 300 DEG C of annealing 24 hours.
After liquid annealing, hardness is 78HV1, and after second annealing, hardness is 88HV1, and average grain size is 10 microns.
Claims (4)
1. be separated the technique that low scandium Al-Mg alloy recrystallization and precipitated phase are separated out, it is characterized in that: method steps is as follows:
1) carry out cold rolling in room temperature to ingot casting, deflection is not less than 70%;
2) in 340 ~ 525 DEG C of temperature ranges to through step 1) alloy that processes carries out the liquid annealing of 1 second ~ 5 minutes;
3) 275 ~ 325 DEG C time, second annealing in 3 hours ~ 36 hours is carried out to the alloy through liquid annealing;
Described ingot casting is low scandium Al-Mg alloy, and by element mass percent, the chemical composition of this alloy is as follows: magnesium: 4.5-6.0%; Manganese: 0.30-0.60%; Scandium: 0.05-0.12%; Zirconium: 0.05-0.15%; Surplus is aluminium and inevitable impurity.
2. according to the technique being separated low scandium Al-Mg alloy recrystallization and precipitated phase described in claim 1 and separating out, it is characterized in that: described step 1) in after cold rolling, rolling direction with roll crystal grain in plane that face normal direction formed and significantly elongated, and the hardness value in this face is not less than 110HV1.
3. according to the technique being separated low scandium Al-Mg alloy recrystallization and precipitated phase described in claim 1 and separating out, it is characterized in that: described step 2) in after liquid annealing, alloy generation perfect recrystallization, average grain size is less than 10 microns, without nano level Al in matrix
3(Sc, Zr) precipitation phase is separated out, and hardness value is 78 ~ 90HV1.
4., according to the technique being separated low scandium Al-Mg alloy recrystallization and precipitated phase described in claim 1 and separating out, it is characterized in that: described step 3) in after second annealing, Al
3(Sc, Zr) precipitation phase separate out, its mean sizes below 10 nanometers, alloy rigidity value rise 10 ~ 20HV1.
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| CN101233252A (en) * | 2005-08-16 | 2008-07-30 | 阿勒里斯铝业科布伦茨有限公司 | High strength weldable al-mg alloy |
| CN101353745A (en) * | 2008-09-10 | 2009-01-28 | 中南大学 | Al-Mg-Mn-Sc-Er alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101233252A (en) * | 2005-08-16 | 2008-07-30 | 阿勒里斯铝业科布伦茨有限公司 | High strength weldable al-mg alloy |
| CN101353745A (en) * | 2008-09-10 | 2009-01-28 | 中南大学 | Al-Mg-Mn-Sc-Er alloy |
Non-Patent Citations (2)
| Title |
|---|
| Al-Mg-Sc合金的再结晶;潘青林等;《中国有色金属学报》;19980930;第8卷(第3期);第427-430页 * |
| Sc和Zr复合微合金化在Al-Mg合金中的存在形式和作用;潘青林等;《航空材料学报》;20020331;第22卷(第1期);第6-10页 * |
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