CN114150193A - Cr-modified heat-resistant aluminum-based alloy composite material and preparation method thereof - Google Patents
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/12—Alloys based on aluminium with copper as the next major constituent
-
- 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
- C22C1/026—Alloys based on aluminium
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- 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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- 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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
- C22F1/057—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with copper as the next major constituent
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Abstract
The invention discloses a Cr modified heat-resistant aluminum-based alloy composite material, which comprises the following elements in percentage by mass: cu 6-10%, Mn 0.2-0.6%, V0.2-0.6%, Cr0.4-0.8%, and the balance of Al, and in a preferred scheme, 4-8% of Al can be added3Zr. The invention also discloses a preparation method of the material. The heat-resistant aluminum-based alloy composite material provided by the invention has very good high-temperature mechanical properties, has higher tensile strength at a high temperature of 350 ℃ compared with the existing heat-resistant aluminum alloy material, and is very suitable for the requirements of heat-resistant parts in the fields of automobiles, weapons, aviation, aerospace, ships and the like. The preparation process of the aluminum-based composite material is simple, and the preparation process time is shortThe process is reliable, the production cost is greatly saved, and the large-scale industrial production is easy to realize.
Description
Technical Field
The invention relates to a preparation method of an aluminum alloy composite material, in particular to a Cr modified heat-resistant aluminum-based alloy composite material and a preparation method thereof.
Background
The heat-resistant aluminum-based alloy composite material is an aluminum-based composite material which is compounded by taking aluminum alloy as a matrix and other high-thermal-stability ceramic particles or intermetallic compounds as reinforcements through various processes and can effectively bear high-temperature load for a long time. The high-temperature heat-resistant steel material has the performance characteristics of small density, high-temperature specific strength, good thermal fatigue resistance and wear resistance, lower thermal expansion coefficient, good thermal conductivity, simple and convenient processing, low price and the like, can partially replace heavy steel materials and expensive titanium alloys, and is applied to the fields of automobile engines, aerospace engines, tank armored car engines, ships and the like as high-performance light-weight heat-resistant components.
At present, the high-temperature strength, the thermal fatigue resistance and the like of the traditional casting heat-resistant aluminum alloy are close to the extreme state, and the high-efficiency development requirement of a novel high-power engine, such as a high-power armored car engine, can not be met. The main reason is that the strengthening phase in the aluminum alloy has insufficient high-temperature thermal stability and is easy to coarsen or dissolve at high temperature to lose the strengthening effect. The service temperature of the Al-Si series heat-resistant aluminum alloy is generally not more than 230 ℃. Adding Mg into Al-Si alloy, aging and precipitating Mg2Si phase, although improving the room temperature strength of the material, due to Mg2The thermal stability temperature of the Si phase is about 180 ℃, so that the cast Al-Mg-Si alloy has low heat resistance and the working temperature is generally lower than 185 ℃. Al-Cu system or Al-Si system alloy with Cu added can precipitate theta' -Al by solid solution-aging2A Cu phase having a thermal stability temperature of about 225 deg.C, andthe high-temperature strength of the material is improved, but the overall high-temperature strength level of the Al-Cu or Al-Si-Cu series cast aluminum alloy is not high due to the limitation of the thermal stability of the strengthening phase, and generally, the material can only work below 225 ℃. However, a piston, which is one of the key components in the combustion chamber of an engine, needs to be in contact with high-temperature gas of 350-400 ℃ (even higher) for a long time and bear the thermo-mechanical fatigue effect of 25-300 ℃, so that the traditional cast heat-resistant aluminum alloy cannot meet the temperature bearing requirement of the engine component under the high-temperature condition of 300-400 ℃. The development of high-performance heat-resistant aluminum alloy with high strength and better high-temperature creep resistance at high temperature to meet the heat-resistant requirement of a novel high-efficiency engine, and the partial replacement of expensive titanium alloy is an important subject in the research field of novel aluminum alloy at home and abroad in about 20-30 years.
Al-Cu alloy is the most excellent in all cast aluminum alloy matrixes due to high-temperature mechanical properties and is a hot spot of matrix research at present, however, the Al-Cu alloy also has the problems of high density, poor casting performance, poor thermal cracking resistance and the like to be improved. The introduction of fine dispersion strengthening phase with high strength, high thermal stability, high volume fraction and good combination with the aluminum matrix into the aluminum matrix is a fundamental way to improve the high-temperature mechanical property of the heat-resistant aluminum-based alloy composite material. Theta' -Al is often used as a heat-stable strengthening phase of novel heat-resistant alloys2Cu phase, but theta' -Al at temperatures above 250 DEG C2The Cu phase often coarsens seriously and loses the strengthening effect. To increase theta' -Al2The high-temperature thermal stability and the high-temperature strengthening effect of the Cu phase are realized by adding a plurality of micro alloying elements to theta' -Al2The thermal stability modification of the Cu phase has become a focus of recent studies, and for example, Mn, V, Ti, Zr, etc. have been studied. However, Cr element is added to theta' -Al in Al-Cu alloy2The thermal stability modification of the Cu phase has not been reported. In addition, Al3The Zr phase has high melting point (1580 ℃) and high elastic modulus (196GPa) and balances the tetragonal crystal structure D023-Al3Zr and an aluminum matrix form a semi-coherent interface, have lower interface energy and lower lattice mismatching degree, and are considered to have thermal stability of 300-500 ℃. And D0 is introduced into the Al-Cu alloy by in-situ reaction by adding potassium fluozirconate23-Al3Zr strengtheningPhase, discussion of potassium fluorozirconate to theta' -Al2The influence of the high temperature thermal stability of the Cu phase has not been reported. In short, the amount of Cr element added and Al are present3The rule and mechanism of the influence of Zr strengthening phase content and heat treatment process on the room temperature and high temperature mechanical properties of the Al-Cu alloy are not clear, and no relevant report exists.
Disclosure of Invention
Aiming at the technical problems, the invention provides a Cr modified heat-resistant aluminum-based alloy composite material and a preparation method thereof, which meet the use requirement of engine parts on high-temperature-resistant aluminum alloy materials.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a Cr modified heat-resistant aluminum-based alloy composite material comprises the following elements in percentage by mass: 6-10% of Cu, 0.2-0.6% of Mn, 0.2-0.6% of V, 0.4-0.8% of Cr and the balance of Al; preferably, the content of each element is as follows by mass percent: cu 8%, Mn 0.4%, V0.4%, Cr 0.6%, and the balance Al.
The method for preparing the Cr modified heat-resistant aluminum-based alloy composite material comprises the following steps:
step S1, weighing the raw materials according to the element proportion, wherein Cu adopts Al-50Cu intermediate alloy, Mn adopts Al-10Mn intermediate alloy, V adopts Al-10V intermediate alloy, Cr adopts Al-10Cr intermediate alloy, and the rest Al adopts pure aluminum blocks;
step S2, heating the pure aluminum block to be molten, and slagging off;
step S3, keeping the temperature at 760-780 ℃, adding an Al-10V intermediate alloy, an Al-10Mn intermediate alloy and an Al-10Cr intermediate alloy to the middle lower part of the melt, adding a covering agent on the surface of the melt, standing and preserving heat for 8-12 min, and slagging off;
step S4, keeping the temperature at 750-760 ℃, adding an Al-50Cu intermediate alloy to the middle lower part of the melt, standing and preserving heat for 4-8 min, and slagging off;
step S5, keeping the temperature at 750-760 ℃, continuously stirring for 3-5 min, then reducing the temperature to 730-750 ℃, adding hexachloroethane into the melt for degassing, controlling the temperature of the melt to 750 ℃, casting the melt into a preheated mold, solidifying and cooling, and demolding;
and S6, carrying out solid solution treatment on the material obtained in the step S5 at the solid solution temperature of 520-560 ℃ for 10-14 h, then carrying out water quenching at room temperature on the material, carrying out artificial aging treatment on the material at the artificial aging temperature of 165-185 ℃ for 7-9 h, and finally carrying out air cooling.
Preferably, the purity of the pure aluminum block in step S1 is 99.9%.
Preferably, the covering agent in step S3 is a mixture of KCl and NaCl, and the mass ratio of the KCl to the NaCl is 1: 1.
Preferably, in step S5, the addition amount of hexachloroethane is 1% of the total mass of the melt, the addition method is to press hexachloroethane into the melt 2 times, the interval of 2 times is 2min, and after each press-in, the mixture is stirred for 1min at a rotation speed of 150 r/min; the preheating temperature of the die is 200 ℃.
Preferably, the solid solution temperature in the step S6 is 540 ℃, the solid solution time is 12h, the water temperature of room temperature water quenching is 25 ℃, the artificial aging temperature is 175 ℃, and the artificial aging time is 8 h.
The Cr modified heat-resistant aluminum-based alloy composite material has the advantages that the high-temperature mechanical property is improved through the following aspects:
(1) the dissolution of Cr increases the theta' -Al after aging heat treatment2The precipitation amount of Cu phase is reduced, and theta' -Al is refined2The Cu phase improves the high-temperature mechanical property of the aluminum alloy material to a certain extent; in addition, the addition of Cr reduces the interface energy and lattice mismatching degree through segregation at the phase interface, and improves the theta' -Al2The thermal stability of the Cu phase can better play the role of high-temperature reinforcement. The addition of Cr also promotes Al20Cu2Mn3Phase, Al20Cu3Mn2Formation of phase, promoting Al11V phase, Al12Formation, growth and sharpening of (Cr, Mn) phase; wherein, Al20Cu2Mn3Phase, Al20Cu3Mn2The phase also plays a certain role in strengthening at high temperature, and Al12The (Cr, Mn) phase has a high melting point and a high melting pointThe temperature stability assists in improving the high-temperature mechanical property of the aluminum alloy.
(2) The heat-resistant aluminum-based alloy composite material mainly contains an alpha-Al matrix and Al2Cu phase, Al20Cu2Mn3Phase, Al20Cu3Mn2Phase, Al11V phase, Al12A (Cr, Mn) phase; theta' -Al2Cu has better thermal stability, and Mn and V are segregated in Al/Al2Cu interface, inhibiting Al2The coarsening of Cu at the high temperature of 350 ℃ improves the high-temperature mechanical property of the aluminum alloy material;
(3) the alloy material is also added with V element, after the V element is added, all strengthening phases obtain V solid solution strengthening, and the strengthening effect of strengthening the relative matrix is improved.
The invention also provides another Cr modified heat-resistant aluminum-based alloy composite material, which is added with Al on the basis of the material3Zr comprises the following elements in percentage by mass: 6-10% of Cu, 0.2-0.6% of Mn, 0.2-0.6% of V, 0.4-0.8% of Cr, and Al34-8% of Zr and the balance of Al; preferably, the content of each element is as follows by mass percent: cu 8%, Mn 0.4%, V0.4%, Cr 0.4%, Al 36% of Zr and the balance of Al.
The method for preparing the Cr modified heat-resistant aluminum-based alloy composite material comprises the following steps:
step S1, weighing the raw materials according to the element proportion, wherein Cu adopts Al-50Cu intermediate alloy, Mn adopts Al-10Mn intermediate alloy, V adopts Al-10V intermediate alloy, Cr adopts Al-10Cr intermediate alloy, and Zr adopts K2ZrF, and pure aluminum blocks are adopted as the rest Al;
step S2, heating the pure aluminum block to be molten, and slagging off;
step S3, keeping the temperature at 760-780 ℃, adding an Al-10V intermediate alloy, an Al-10Mn intermediate alloy and an Al-10Cr intermediate alloy to the middle lower part of the melt, adding a covering agent on the surface of the melt, standing and preserving heat for 8-12 min, and slagging off;
step S4, keeping the temperature at 750-760 ℃, adding an Al-50Cu intermediate alloy to the middle lower part of the melt, standing and preserving heat for 4-8 min, and slagging off;
step S5, keeping the temperature at 760-780 ℃, mechanically stirring the melt, and adding K while stirring2ZrF6Continuously stirring the metal salt for 4-5 min, standing for 1-3 min, and slagging off;
and step S6, keeping the temperature at 750-760 ℃, continuously stirring for 3-5 min, then reducing the temperature to 730-750 ℃, and adding hexachloroethane into the melt for degassing. Controlling the temperature of the melt to 750 ℃, casting the melt into a preheated mold, and demolding after solidification and cooling;
and S7, carrying out solid solution treatment on the material obtained in the step S6 at the solid solution temperature of 520-560 ℃ for 10-14 h, then carrying out water quenching at room temperature on the material, carrying out artificial aging treatment on the material at the artificial aging temperature of 165-185 ℃ for 7-9 h, and finally carrying out air cooling.
Preferably, the purity of the pure aluminum block in step S1 is 99.9%.
Preferably, the covering agent in step S3 is a mixture of KCl and NaCl, and the mass ratio of the KCl to the NaCl is 1: 1.
Preferably, K is the same as step S52ZrF6The metal salt is in powder form, and K is added2ZrF6The method of the metal salt comprises the following steps: stirring the melt at 600r/min to generate vortex for the liquid metal, and spraying powder K with a powder sprayer2ZrF6The metal salt is slowly sprayed into the vortex generated by stirring to be involved in the melt.
Preferably, in step S6, the addition amount of hexachloroethane is 1% of the total mass of the melt, the addition method is to press hexachloroethane into the melt 2 times, the 2 times interval is 2min, stirring is performed at a rotation speed of 150r/min for 1min after each press, and the mold preheating temperature is 200 ℃.
Preferably, the solid solution temperature in the step S7 is 540 ℃, the solid solution time is 12h, the water temperature of room temperature water quenching is 25 ℃, the artificial aging temperature is 175 ℃, and the artificial aging time is 8 h.
Al in the heat-resistant aluminum-based alloy composite material3Zr phase is formed by adding K2ZrF6The alloy is generated by in-situ reaction in an Al-8Cu-0.4Mn-0.4V-0.4Cr alloy melt, and the chemical equation of the reaction is as follows: 3K2ZrF6+13Al→3Al3Zr+4AlF3+6KF, AlF as a by-product of the reaction3And KF floats slightly above the melt in density and is removed by skimming.
The Cr modified heat-resistant aluminum-based alloy composite material is continuously added with Al on the basis of adding Cr3Zr，Al3Zr has the following effects on the high-temperature mechanical properties of the composite material:
(1) the aluminum-based alloy material mainly contains an alpha-Al matrix and Al3Zr phase, Al2Cu phase, Al85Mn15Phase, Al2.5Cu0.5Zr phase, Al introduced using in situ reaction3The Zr phase has small size, is more uniformly distributed in the matrix and has better mechanical property; fine Al3Zr can effectively pin dislocation and promote theta' -Al2The Cu phase is separated out and refined, so that the high-temperature strengthening effect is improved;
(2) after solution heat treatment, there is a portion of Al3Conversion of Zr-phase particles to Al2.5Cu0.5Zr phase, which is also a high-strength and high-hardness phase, having a higher Al content than Al3The Zr phase has higher thermal stability and is in an elliptical shape, so that the stress concentration of an interface can be reduced, and the high-temperature strengthening effect is further improved;
(3) softening of matrix at high temperature, Al, in the present aluminum-based alloy composite3Introduction of Zr phase, theta' -Al2Refinement of Cu phase, segregation of Mn, Zr, V in Al/Al2The Cu interface inhibits Al2Coarsening of Cu phase, Al3Zr phase and Al2Cu phase and Al2.5Cu0.5The Zr phase plays a role in synergistic reinforcement, so that the high-temperature mechanical property is further improved.
Compared with the prior art, the invention has the following beneficial effects:
the Cr modified heat-resistant aluminum-based alloy composite material provided by the invention has very good high-temperature strengthening performance, has better tensile strength at a high temperature of 350 ℃ compared with the existing heat-resistant aluminum alloy material, and is very suitable for the fields of ships, weapons, aviation, aerospace, automobiles and the like. The preparation method of the heat-resistant aluminum-based alloy composite material is simple in process, short in preparation process time and reliable in process, greatly saves the production cost, and is easy for large-scale industrial production.
Drawings
FIG. 1 is an XRD pattern of a heat-resistant aluminum-based alloy composite material according to examples 1 to 5 of the present invention.
FIG. 2 is an SEM analysis of a heat resistant aluminum-based alloy composite material according to examples 1 to 5 of the present invention.
FIG. 3 is a graph showing the tensile properties at room temperature of the heat-resistant aluminum-based alloy composite materials of examples 1 to 5 of the present invention.
FIG. 4 is a graph showing the tensile properties at high temperature of the heat-resistant aluminum-based alloy composite materials of examples 1 to 5 of the present invention.
FIG. 5 shows different Al's for examples 9 to 12 of the present invention3XRD pattern of heat-resistant aluminum-based alloy composite material with Zr content.
FIG. 6 shows various Al elements in examples 9 to 12 of the present invention3SEM analysis chart of the heat-resistant aluminum-based alloy composite material with Zr content.
FIG. 7 shows different Al's for examples 4 and 9 to 12 of the present invention3The tensile property of the heat-resistant aluminum-based alloy composite material with Zr content at high temperature.
Fig. 8 is a photograph of microstructures of the heat-resistant aluminum alloys of example 1 and example 2 at different high-temperature exposure times.
Detailed Description
The following detailed description is to be read in connection with the accompanying drawings, but it is to be understood that the scope of the invention is not limited to the specific embodiments. The raw materials and reagents used in the examples were all commercially available unless otherwise specified.
Example 1 preparation of Cr-modified Heat-resistant aluminum-based alloy composite Material
The Cr modified heat-resistant aluminum-based alloy composite material comprises the following elements in percentage by mass: cu 8%, Mn 0.4%, V0.4%, Cr 0.6%, and the balance Al.
S1, weighing the raw materials according to the element proportion, wherein Cu is Al-50Cu intermediate alloy, Mn is Al-10Mn intermediate alloy, V is Al-10V intermediate alloy, Cr is Al-10Cr intermediate alloy, and the rest Al is pure aluminum blocks (the purity is 99.9%);
step S2, heating the pure aluminum block to be molten, and slagging off;
step S3, keeping the temperature at 770 ℃, adding Al-10V intermediate alloy, Al-10Mn intermediate alloy and Al-10Cr intermediate alloy to the middle lower part of the melt, adding a covering agent on the surface of the melt, standing and preserving the temperature for 10min, and slagging off; wherein the covering agent is a mixture of KCl and NaCl in a mass ratio of 1: 1;
step S4, keeping the temperature at 755 ℃, adding Al-50Cu master alloy to the middle lower part of the melt, standing and preserving heat for 6min, and slagging off;
step S5, keeping the temperature at 755 ℃, continuously stirring for 4min, then reducing the temperature to 740 ℃, adding hexachloroethane into the melt for degassing, controlling the temperature of the melt to 750 ℃, casting the melt into a mold preheated to 200 ℃, solidifying, cooling and demolding; wherein the addition amount of hexachloroethane is 1% of the total mass of the melt, the addition method comprises pressing hexachloroethane into the melt for 2 times at an interval of 2min, and stirring at a rotation speed of 150r/min for 1min after each pressing;
and S6, performing solid solution treatment on the material obtained in the step S5 at the solid solution temperature of 540 ℃ for 12 hours, performing room-temperature water quenching on the material, performing artificial aging treatment on the material at the artificial aging temperature of 175 ℃ for 8 hours, and finally performing air cooling to obtain the material.
Examples 2 to 5 preparation of Cr-modified Heat-resistant aluminum-based alloy composite Material
The preparation method of the heat-resistant aluminum-based alloy composite material comprises the steps of the process and the steps of the process are the same as those in the embodiment 1, the contents of Al, Cu, Mn and V in raw materials are the same as those in the embodiment 1, and the content of Cr is added according to the table 1, so that the heat-resistant aluminum-based alloy composite materials with different Cr addition amounts are obtained.
TABLE 1 Cr content of examples 2 to 5
| Examples | Cr content (wt.%) in heat-resistant aluminium-base alloy composite material |
| Example 2 | 0 |
| Example 3 | 0.2 |
| Example 4 | 0.4 |
| Example 5 | 0.8 |
Example 6 microstructures of the heat resistant aluminum-based alloy composites of examples 1-5
1. XRD analysis was performed on the heat-resistant aluminum-based alloy composite materials of different Cr contents prepared in examples 1 to 5 using an X-ray diffractometer, and the XRD pattern obtained is shown in FIG. 1, as can be seen from FIG. 1, the materials included an α -Al matrix and Al2Cu phase, Al20Cu2Mn3Phase, Al20Cu3Mn2Phase, Al11V phase, Al12(Cr, Mn) phase 6 main phases,
2. SEM analysis is carried out on the heat-resistant aluminum-based alloy composite materials with different Cr contents prepared in examples 1-5 by adopting a table type scanning electron microscope/energy spectrometer integrated device, and the result is shown in figure 2; in fig. 2, (a) (b) example 2; (c) (d) example 3; (e) (f) example 4; (g) (h) example 1; (i) (j) example 5;
as can be seen from the analysis of FIG. 2, as the addition amount of Cr increases, α -Al becomes slightly larger, smaller and then slightly larger, the addition amount of Cr is 0.4% and is the smallest, and the average size is about 50-60 μm; sheet-like Al2Cu phaseThe surface patterns are fine and clear, and are gradually broken and crushed into 30-40 mu m from the size of about 80 mu m; dark gray massive Al inside11V phase change is large, and the size is about 20 mu m; light grey Al20Cu2Mn3When the patterns appear, the surface patterns are fine and complicated, are distributed on the matrix in a spherical shape and a small block shape, the number of the patterns is gradually increased, and the size of the patterns is gradually increased to be more than 80 mu m; grey block Al20Cu2Mn3Phase and dark grey massive Al11The V phase has a size of 20-60 μm and can almost cover Al with different sizes2A Cu phase; light grey Al12The size of the (Cr, Mn) phase gradually becomes 80 μm or more, and the sharpness becomes more severe. This indicates that the addition of Cr promotes Al in the heat-treated Al-8Cu-0.4Mn-0.4V-xCr heat-resistant aluminum alloy2Refining of Cu phase and promoting Al20Cu2Mn3Phase, Al20Cu3Mn2Formation of phase, promoting Al11V phase, Al12Formation, growth and sharpening of (Cr, Mn) phase.
Example 7 tensile mechanical Properties of the Heat-resistant aluminum-based alloy composites of examples 1-5
1. Tensile mechanical property at room temperature
FIG. 3 is a graph of the tensile properties at room temperature of the heat resistant aluminum-based alloy composite materials of examples 1 to 5, wherein (a) is a stress-strain curve and (b) is a change in elongation after fracture; table 2 shows the tensile mechanical property test data at room temperature for the heat-resistant aluminum-based alloy composite materials of examples 1 to 5;
when the addition amount of Cr is 0 wt.% at room temperature of 25 ℃ (example 2), the mechanical properties of the heat-resistant aluminum-based alloy composite material are optimal, and the tensile strength is 370.49 MPa;
TABLE 2 tensile mechanical Properties at Room temperature for the Heat-resistant aluminum-based alloy composites of examples 1-5
2. High temperature tensile mechanical properties
FIG. 4 is a graph of tensile properties at high temperature for the heat resistant aluminum-based alloy composites of examples 1-5, wherein (a) is a stress-strain curve and (b) is a change in elongation after fracture; table 3 shows the tensile mechanical properties of the heat-resistant aluminum-based alloy composite materials of examples 1 to 5 at high temperature.
When the addition amount of Cr is 0.6 wt.% at a high temperature of 350 ℃ (example 1), the mechanical property of the heat-resistant aluminum-based alloy composite material is optimal, and the tensile strength is 144.26 MPa;
TABLE 3 high temperature tensile mechanical Properties of the Heat-resistant aluminum-based alloy composites of examples 1-5
Although the mechanical properties of the heat-resistant aluminum-based alloy composite material are optimal when the amount of Cr added is 0.6 wt.% at the high temperature 350 (example 1), the addition of Al is further performed by using the case where the amount of Cr is 0.4 wt.% (example 4) in consideration of the increase of Cr, which can improve the mechanical properties at the high temperature but at the same time deteriorate the mechanical properties at the room temperature, in combination with the tensile mechanical property data at the room temperature3And (3) Zr experiment.
Example 8 thermal exposure stability of heat-resistant aluminum-based alloy composite materials prepared in examples 1 and 2
The heat-resistant aluminum-based alloy composite materials prepared in the examples 1 and 2 are respectively exposed for 0h, 12h, 24h and 36h at the high temperature of 350 ℃, and the obtained microstructure photo is shown in FIG. 8. In FIG. 8, the left side is the heat resistant aluminum alloy without Cr addition of example 2, a1 is 0h, a2 is 12h, a3 is 24h, a4 is 36h, the right side is the heat resistant aluminum alloy composite with Cr addition of example 1, a1 is 0h, a2 is 12h, a3 is 24h, and a4 is 36 h.
As can be seen from FIG. 8, as the heat exposure time increased, θ' -Al in the aluminum alloy to which Cr was not added (example 2)2The Cu phase was significantly coarsened, the coarsening speed was high, and the θ' -Al in the Cr-added aluminum alloy composite material (example 1)2The coarsening speed of the Cu phase is slow, which shows that the heat stability of the aluminum alloy material at the high temperature of 350 ℃ is improved after the Cr is added, and the strengthening effect of the strengthening phase at the high temperature is facilitated。
Example 9 preparation of a catalyst containing Al3Cr modified heat-resistant aluminum-based alloy composite material of Zr
Containing Al3The Cr modified heat-resistant aluminum-based alloy composite material of Zr comprises the following elements in percentage by mass: cu 8%, Mn 0.4%, V0.4%, Cr 0.4%, Al 36% of Zr and the balance of Al.
Step S1, weighing the raw materials according to the element proportion, wherein Cu adopts Al-50Cu intermediate alloy, Mn adopts Al-10Mn intermediate alloy, V adopts Al-10V intermediate alloy, Cr adopts Al-10Cr intermediate alloy, and Zr adopts K2ZrF, and pure aluminum blocks (with the purity of 99.9%) are used as the rest Al;
step S2, heating the pure aluminum block to be molten, and slagging off;
step S3, keeping the temperature at 770 ℃, adding Al-10V intermediate alloy, Al-10Mn intermediate alloy and Al-10Cr intermediate alloy to the middle lower part of the melt, adding a covering agent on the surface of the melt, standing and preserving the temperature for 10min, and slagging off; wherein the covering agent is a mixture of KCl and NaCl in a mass ratio of 1: 1;
step S4, keeping the temperature at 755 ℃, adding Al-50Cu master alloy to the middle lower part of the melt, standing and preserving heat for 6min, and slagging off;
step S5, keeping the temperature at 770 ℃, mechanically stirring the melt at the stirring speed of 600r/min to generate vortex for the liquid metal, and spraying the powder K by a powder sprayer2ZrF6Slowly spraying the metal salt into vortex generated by stirring to roll the metal salt into the melt, continuously stirring for 4.5min, standing for 2min, and slagging off;
step S6, keeping the temperature at 755 ℃, continuously stirring for 4min, then reducing the temperature to 740 ℃, adding hexachloroethane into the melt for degassing, controlling the temperature of the melt to 750 ℃, casting the melt into a mold preheated to 200 ℃, solidifying, cooling and demolding; wherein the addition amount of hexachloroethane is 1% of the total mass of the melt, the addition method comprises pressing hexachloroethane into the melt for 2 times at an interval of 2min, and stirring at a rotation speed of 150r/min for 1min after each pressing;
and S7, performing solid solution treatment on the material obtained in the step S6 at the solid solution temperature of 540 ℃ for 12 hours, performing room-temperature water quenching on the material, performing artificial aging treatment on the material at the artificial aging temperature of 175 ℃ for 8 hours, and finally performing air cooling to obtain the material.
Examples 10-12 preparation of alloys containing Al3Cr modified heat-resistant aluminum-based alloy composite material of Zr
Preparation of a catalyst containing Al3The Cr modified heat-resistant aluminum-based alloy composite material of Zr has the same processes in each step as in example 8, and the Al, Cu, Mn, V and Cr contents in the raw materials are the same as in example 8, except that Al3Zr content was added as in Table 4 to obtain different Al3Heat-resistant aluminum-based alloy composite material with Zr addition.
TABLE 4 Al of examples 10 to 123Zr content
| Examples | Al in heat-resistant aluminum-based alloy composite material3Zr content (wt.%) |
| Example 10 | 3 |
| Example 11 | 9 |
| Example 12 | 12 |
Example 13 microstructures of the heat resistant aluminum-based alloy composites of examples 9-12
1. Using an X-ray diffractometer, different Al prepared in examples 9 to 12 were measured3Heat-resistant aluminum-based alloy composite material with Zr contentXRD analysis is carried out, the XRD pattern is obtained and is shown in figure 5, and as can be seen from figure 5, the material comprises an alpha-Al matrix and Al3Zr phase, Al2Cu phase, Al2.5Cu0.5Zr phase, Al85Mn15The 5 main phases of the phase are the phases,
2. different Al prepared in examples 9-12 by using a bench-top scanning electron microscope/spectrometer integrated apparatus3SEM analysis is carried out on the heat-resistant aluminum-based alloy composite material with Zr content, and the result is shown in FIG. 6; in fig. 6, (a) (b) example 10; (c) (d) example 9; (e) (f) example 11; (g) (h) example 12;
as is clear from the analysis of FIG. 6, it follows Al3The content of Zr is increased, the size of alpha-Al is kept unchanged after the size of the alpha-Al is gradually reduced, and when the content of Al is increased, the Al is kept unchanged3The smallest size, on average about 50 μm, is obtained with a Zr content of 6 wt.%, since alpha-Al is associated with Al3The lattice mismatching degree between Zr is very low (10.87%), and alpha-Al can be in Al3Zr surface nucleation grows, and Mn contained in the matrix enables Zr atoms which are slowly diffused to segregate to a coherent interface, so that the interface energy is reduced, the growth of alpha-Al is inhibited, and an effective strengthening effect can be achieved; white land-like Al2A Cu phase with a size of about 5-100 μm, which rapidly decreases in number and disappears; and rod-like, small block-like Al2The Cu phase gradually appears, and the size is 20-40 mu m; dark grey Al85Mn15The phase size becomes smaller and larger, when Al is present3Maximum size with a Zr content of 12 wt.%, average about 20-60 μm; small amount of block-shaped Al covering the land2Cu phase surface, or distributed on the matrix; white Al3Zr phase, Al2.5Cu0.5The Zr phase is kept to be 2-5 mu m in size and kept to be rice grain-shaped, broken block-shaped and small short floccule-shaped, which proves that the Al3Zr phase, Al2.5Cu0.5The Zr phases have better thermal stability because the shapes and the sizes of the Zr phases are almost unchanged after the Zr phases are subjected to heat treatment; the quantity gradually changes more and is more evenly distributed on the substrate, and part of the Al is dark gray85Mn15And (4) intersecting. These observations indicate that Al is present3The increase of Zr content can promote the refinement of alpha-Al and promote Al2The Cu phase changes from a land shape to a rod shape or a small block shape to promote Al2.5Cu0.5Formation and proliferation of Zr phase, but promotion of Al85Mn15Growth of the phases.
Example 14 high temperature tensile mechanical properties of the Heat resistant aluminum-based alloy composites of example 4 and examples 9-12
FIG. 7 is tensile mechanical properties at high temperature of the heat resistant aluminum-based alloy composite materials of example 4 and examples 9 to 12, and Table 5 is experimental data of tensile mechanical properties at high temperature of the heat resistant aluminum-based alloy composite materials of example 4 and examples 9 to 12;
high temperature of 350 ℃ Al3When the Zr content is 6 wt.% (example 8), the mechanical property of the heat-resistant aluminum-based alloy composite material is better, and the tensile strength is 164.12 MPa;
TABLE 5 high temperature tensile mechanical Properties of the Heat-resistant aluminum-based alloy composites of example 4 and examples 9-12
Example 15
The high temperature tensile strength of the heat-resistant aluminum-based alloy composite materials of example 1 and example 9 was compared with other heat-resistant aluminum alloys reported at home and abroad, and the results are shown in table 6:
TABLE 6 comparison of the high temperature tensile strength of the heat resistant aluminum-based alloy composites of examples 1 and 9 with other heat resistant aluminum alloys reported at home and abroad
[1]Pan L,Zhang S,YangY,et al.High-Temperature Mechanical Properties of Aluminum Alloy Matrix Composites Reinforced with Zrand Ni Trialumnides Synthesized by In SituReaction[J].Metallurgical and Materials Transactions A,2020,51(1):214-225.
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As can be seen from table 6, the tensile strength of the heat-resistant aluminum-based alloy composite materials of examples 1 and 9 of the present invention at 350 ℃ is significantly greater than that of other heat-resistant aluminum alloy materials reported at home and abroad.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. The Cr modified heat-resistant aluminum-based alloy composite material is characterized by comprising the following elements in percentage by mass: 6-10% of Cu, 0.2-0.6% of Mn, 0.2-0.6% of V, 0.4-0.8% of Cr and the balance of Al.
2. The heat-resistant aluminum-based alloy composite material according to claim 1, wherein the contents of the respective elements are, in mass percent: cu 8%, Mn 0.4%, V0.4%, Cr 0.6%, and the balance Al.
3. The heat-resistant aluminum-based alloy composite material according to claim 1, characterized in that: the heat-resistant aluminum-based alloy composite material also comprises 4-8% of Al by mass percent3Zr。
4. The heat-resistant aluminum-based alloy composite material according to claim 3, characterized by comprising the following elements in mass percent: cu 8%, Mn 0.4%, V0.4%, Cr 0.4%, Al36% of Zr and the balance of Al.
5. A method of making the heat resistant aluminum-based alloy composite of claim 1, comprising the steps of:
s1, weighing raw materials according to the element proportion, wherein Cu adopts Al-50Cu intermediate alloy, Mn adopts Al-10Mn intermediate alloy, V adopts Al-10V intermediate alloy, Cr adopts Al-10Cr intermediate alloy, and the rest Al adopts pure aluminum blocks;
step S2, heating the pure aluminum block to be molten, and slagging off;
step S3, keeping the temperature at 760-780 ℃, adding an Al-10V intermediate alloy, an Al-10Mn intermediate alloy and an Al-10Cr intermediate alloy to the middle lower part of the melt, adding a covering agent on the surface of the melt, standing and preserving heat for 8-12 min, and slagging off;
step S4, keeping the temperature at 750-760 ℃, adding an Al-50Cu intermediate alloy to the middle lower part of the melt, standing and preserving heat for 4-8 min, and slagging off;
step S5, keeping the temperature at 750-760 ℃, continuously stirring for 3-5 min, then reducing the temperature to 730-750 ℃, adding hexachloroethane into the melt for degassing, controlling the temperature of the melt to 750 ℃, casting the melt into a preheated mold, solidifying and cooling, and demolding;
and S6, carrying out solid solution treatment on the material obtained in the step S5 at the solid solution temperature of 520-560 ℃ for 10-14 h, then carrying out water quenching at room temperature on the material, carrying out artificial aging treatment on the material at the artificial aging temperature of 165-185 ℃ for 7-9 h, and finally carrying out air cooling.
6. The method of claim 5, wherein:
the covering agent in the step S3 is a mixture of KCl and NaCl, and the mass ratio of the KCl to the NaCl is 1: 1;
in the step S5, the addition amount of hexachloroethane is 1% of the total mass of the melt, the addition method is that hexachloroethane is pressed into the melt for 2 times, the interval of 2 times is 2min, and the hexachloroethane is stirred for 1min at the rotating speed of 150r/min after being pressed into the melt for 2 times; the preheating temperature of the die is 200 ℃;
in the step S6, the solid solution temperature is 540 ℃, the solid solution time is 12h, the water temperature of room temperature water quenching is 25 ℃, the artificial aging temperature is 175 ℃, and the artificial aging time is 8 h.
7. A method of making the heat resistant aluminum-based alloy composite of claim 3, comprising the steps of:
step S1, weighing the raw materials according to the element proportion, wherein Cu adopts Al-50Cu intermediate alloy, Mn adopts Al-10Mn intermediate alloy, V adopts Al-10V intermediate alloy, Cr adopts Al-10Cr intermediate alloy, and Zr adopts K2ZrF, and pure aluminum blocks are adopted as the rest Al;
step S2, heating the pure aluminum block to be molten, and slagging off;
step S3, keeping the temperature at 760-780 ℃, adding an Al-10V intermediate alloy, an Al-10Mn intermediate alloy and an Al-10Cr intermediate alloy to the middle lower part of the melt, adding a covering agent on the surface of the melt, standing and preserving heat for 8-12 min, and slagging off;
step S4, keeping the temperature at 750-760 ℃, adding an Al-50Cu intermediate alloy to the middle lower part of the melt, standing and preserving heat for 4-8 min, and slagging off;
step S5, keeping the temperature at 760-780 ℃, mechanically stirring the melt, and adding K while stirring2ZrF6Continuously stirring the metal salt for 4-5 min, standing for 1-3 min, and slagging off;
and step S6, keeping the temperature at 750-760 ℃, continuously stirring for 3-5 min, then reducing the temperature to 730-750 ℃, and adding hexachloroethane into the melt for degassing. Controlling the temperature of the melt to 750 ℃, casting the melt into a preheated mold, and demolding after solidification and cooling;
and S7, carrying out solid solution treatment on the material obtained in the step S6 at the solid solution temperature of 520-560 ℃ for 10-14 h, then carrying out water quenching at room temperature on the material, carrying out artificial aging treatment on the material at the artificial aging temperature of 165-185 ℃ for 7-9 h, and finally carrying out air cooling.
8. The method of claim 7, wherein:
the covering agent in the step S3 is a mixture of KCl and NaCl, and the mass ratio of the KCl to the NaCl is 1: 1;
k in step S52ZrF6The metal salt is in powder form, and K is added2ZrF6The method of the metal salt comprises the following steps: stirring the melt at 600r/min to generate vortex for the liquid metal, and spraying powder K with a powder sprayer2ZrF6Slowly spraying the metal salt into a vortex generated by stirring to enable the metal salt to be rolled into the melt;
in the step S6, the addition amount of hexachloroethane is 1% of the total mass of the melt, the addition method comprises the steps of pressing hexachloroethane into the melt for 2 times, wherein the interval of 2 times is 2min, stirring is carried out for 1min at the rotating speed of 150r/min after each pressing, and the preheating temperature of a die is 200 ℃;
in the step S7, the solid solution temperature is 540 ℃, the solid solution time is 12h, the water temperature of room temperature water quenching is 25 ℃, the artificial aging temperature is 175 ℃, and the artificial aging time is 8 h.
9. A heat-resistant aluminum-based alloy composite material prepared by the method according to claim 5 or 6.
10. A heat resistant aluminum-based alloy composite material prepared by the method of claim 7 or 8.
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