CN109576541B - Composite microalloyed silicon-aluminum alloy and preparation method thereof - Google Patents

Composite microalloyed silicon-aluminum alloy and preparation method thereof Download PDF

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CN109576541B
CN109576541B CN201910103628.7A CN201910103628A CN109576541B CN 109576541 B CN109576541 B CN 109576541B CN 201910103628 A CN201910103628 A CN 201910103628A CN 109576541 B CN109576541 B CN 109576541B
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aluminum
alloy
silicon
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silicon alloy
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CN109576541A (en
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蔡志勇
王日初
彭超群
冯艳
王小锋
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Central South University
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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
    • C22C21/02—Alloys based on aluminium with silicon 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
    • 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
    • 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
    • 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
    • C22F1/043—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 silicon as the next major constituent

Abstract

The invention provides a composite microalloyed aluminum-silicon alloy and a preparation method thereof, wherein the aluminum-silicon alloy comprises the following components in percentage by mass: si: 48.0-52.0%; x: 0.1-0.4%; y: 0.1-0.5%; the balance of Al; the X comprises Nb; the Y comprises one or more of Mg, Cu and Mn. According to the invention, Mg and/or Cu and/or Mn is added into the aluminum-silicon alloy, and Nb elements are also added, the Nb atoms interact with various atoms of Si, Al, Mg and/or Cu and/or Mn to form a second phase, and the Nb atoms greatly vibrate near the equilibrium position of the Nb atoms due to the great structural difference and uneven acting force between the Nb atoms and other atoms, so that the heat conductivity of the aluminum-silicon alloy is improved. Meanwhile, the mechanical strength of the aluminum-silicon alloy can be improved by Mg, Cu and Mn, and the hardness of Nb can be enhanced under the condition that Nb contains a plurality of elements, so that the strength of the aluminum-silicon alloy is further enhanced.

Description

Composite microalloyed silicon-aluminum alloy and preparation method thereof
Technical Field
The invention relates to the field of alloy preparation, in particular to a composite microalloyed silicon-aluminum alloy and a preparation method thereof.
Background
The electronic packaging material is a key material of electronic components, assemblies and parts, and the performance of the electronic packaging material is directly related to the structural design, the service life and the operational reliability of the whole equipment. With the development of miniaturization, integration, high power density, and high reliability of modern electronic systems, the amount of heat generated by semiconductor integrated circuit chips has increased rapidly. At present, 30% of chip performance is limited by packaging materials, and the development of high-performance electronic packaging materials is not slow and draws general attention at home and abroad.
The aluminum-silicon alloy electronic packaging material is hypereutectic alloy (12.6 percent, mass fraction, the same below) with high Si content, has the advantages of small density, high thermal conductivity, low thermal expansion coefficient, good process performance and the like, and has important application value in the high-tech fields of military affairs, aviation, aerospace and the like. In the conventional cast aluminum-silicon alloy, because the cooling rate is low (less than 100 ℃/s) in the preparation process, the Si phase is serious in macrosegregation and poor in distribution uniformity, the primary Si phase is in various forms such as lath, star and polyhedron, the size is large (more than 100 mu m), the edge angle is sharp, and the continuity of an Al matrix is seriously cracked, so that the heat-conducting property of the aluminum-silicon alloy is reduced. Electronic packaging shells made of aluminum-silicon alloys are generally thin-walled parts (the wall thickness is about 1.5 mm) with complex structures, and are also designed with micro-beams, small holes and the like, so that the aluminum-silicon alloys are required to have high mechanical properties.
At present, the general means for improving the mechanical property of the aluminum-silicon alloy is to regulate and control the distribution of Si phase by adjusting the solidification process of an aluminum-silicon alloy melt, but the method is limited by a binary alloy system and has limited effect. Therefore, micro-alloying means is tried, namely some micro-alloy elements, mainly Mg and Cu metal elements, are added into the aluminum-silicon alloy, but the method can reduce the thermal conductivity of the material while improving the mechanical property, and is difficult to meet the requirement of the electronic packaging material on the thermal conductivity.
Disclosure of Invention
Based on the above, the invention provides the composite microalloyed aluminum-silicon alloy and the preparation method thereof, which can simultaneously improve the strength and the thermal conductivity of the aluminum-silicon alloy.
The composite microalloyed aluminum-silicon alloy comprises the following components in percentage by mass:
Si：48.0～52.0％；
X：0.1～0.4％；
Y：0.1～0.5％；
the balance of Al;
the X comprises Nb; the Y comprises one or more of Mg, Cu and Mn.
Compared with the prior art, the aluminum-silicon alloy has the advantages that Mg and/or Cu and/or Mn is added into the aluminum-silicon alloy, Nb atoms interact with various atoms of Si, Al, Mg and/or Cu and/or Mn to form a second phase, and are positioned at the edges of crystal lattices, because the Nb atoms and other atoms have extremely high structural difference and the acting force is uneven, the Nb atoms vibrate greatly near the equilibrium position of the Nb atoms, and the heat conductivity of the solid depends on the vibration in the crystal lattices, so that the heat conductivity of the aluminum-silicon alloy can be obviously improved by adding Nb, namely the heat conductivity is improved. Meanwhile, the mechanical strength of the aluminum-silicon alloy can be improved by Mg, Cu and Mn, and the hardness of Nb can be enhanced under the condition that Nb contains a plurality of elements, so that the strength of the aluminum-silicon alloy is further enhanced.
Further, the thermal conductivity of the composite microalloyed aluminum-silicon alloy is 147-162W/(m.K).
Furthermore, the tensile strength of the composite microalloyed aluminum-silicon alloy is 315-353 MPa, the bending strength is 397-440 MPa, and the hardness is 193-215 HB.
Further, the X also comprises one or two of Sc and Zr.
The preparation method of the composite microalloyed aluminum-silicon alloy provided by the invention comprises the following steps:
s1, melting a silicon source, an aluminum source, an X source and a Y source together to obtain a melt;
s2, applying atomization pressure to the melt to atomize and deposit the melt to form a billet;
s3, sequentially densifying and thermally treating the billet to obtain the composite microalloyed silicon-aluminum alloy;
wherein the X source comprises Nb element, and the Y source comprises one or more elements of Mg, Cu and Mn.
Further, the smelting temperature is 750-1300 ℃.
Further, the atomization pressure in step S2 is 0.9 to 1.3 MPa.
Further, in step S3, the densification is performed by applying a pressure of 45 to 180MPa to the ingot at 520 to 600 ℃.
Further, the silicon source is monocrystalline silicon; the aluminum source is pure aluminum; the X source is Al-Nb intermediate alloy, and the Y source is pure Cu and/or pure Mg and/or Al-Mn intermediate alloy.
Further, the X source also comprises an intermediate alloy of Sc and/or Zr.
Drawings
FIG. 1 is a microstructure of Al of example 1-50% Si-0.3% Nb-0.3% Mn;
FIG. 2 is a microstructure of Al of example 2-50% Si-0.1% Sc-0.5% Cu;
FIG. 3 is a microstructure of example 3 Al-50% Si-0.2% Zr-0.3% Mg;
FIG. 4 is a case after working with example 3 Al-50% Si-0.2% Zr-0.3% Mg.
Detailed Description
According to the invention, the Nb element and one or more of Mg, Cu and Mn are added into the silicon-aluminum alloy at the same time, and the mechanical strength is improved by utilizing the mutual synergistic effect of one or more of Mg, Cu and Mn and the silicon-aluminum alloy, and meanwhile, the Nb atom generates large vibration in the alloy, so that the thermal conductivity is improved. The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
In the embodiment, monocrystalline silicon is used as a silicon source, high-purity aluminum with the content of 99.998-99.999% is used as an aluminum source, an Al-Nb intermediate alloy with the Nb content of 50% is used as an X source, an Al-Mn intermediate alloy with the Mn content of 10% is used as a Y source, and Nb and Mn are doped into the silicon-aluminum alloy according to the mass ratio of 50% of Si, 0.3% of Nb0.3% of Mn and the balance of aluminum, and the preparation method specifically comprises the following steps:
s1, melting a silicon source, an aluminum source, an X source and a Y source together to obtain a melt;
heating high-purity aluminum to 800-870 ℃ to gradually melt the high-purity aluminum. And after the high-purity aluminum is completely melted, continuously heating to 1200-1400 ℃, and adding the monocrystalline silicon in batches. And after the monocrystalline silicon is completely melted, cooling to 750-820 ℃, adding the Al-Mn intermediate alloy, then adding the Al-Nb intermediate alloy, and fully stirring for 5-10 min to obtain a melt.
S2, applying atomization pressure to the melt to atomize and deposit the melt to form a billet;
the melt was then slagged with a slag former comprising 30% NaCl, 47% KCl, 23% cryolite and degassed with hexachlorohexane. And standing for 10min, and pouring the melt into a tundish with the preheating temperature of 900-1000 ℃, preferably 955-965 ℃. And simultaneously opening high-pressure nitrogen, applying atomization pressure of 0.9-1.3 MPa to the melt at the atomization temperature of 780-850 ℃ to atomize the melt into powder, and obtaining a deposition billet with the diameter of 350mm and the height of 560mm on a deposition disc with the receiving distance of 630 mm.
And S3, sequentially densifying and thermally treating the billet to obtain the composite microalloyed silicon-aluminum alloy.
Densification treatment: and (3) placing the deposition billet in a hot isostatic pressing furnace, heating the deposition billet to 520-600 ℃, and simultaneously applying pressure of 45-180 MPa, preferably 180MPa and maintaining the pressure for 1-3 hours.
And (3) heat treatment: and cutting the densified alloy ingot into small blocks with the size of 85mm multiplied by 10mm, and putting the small blocks into a box-type resistance furnace to be heated to 500-525 ℃ at the speed of 5-25 ℃/min. And (4) performing oil quenching on the steel plate by using oil at the temperature of 80-120 ℃ after heat preservation for 2-8 h. And finally, placing the small blocks in a box-type resistance furnace, heating to 150-220 ℃ at the speed of 5-25 ℃/min, preserving heat for 24-72 hours, taking out, and air-cooling to obtain the final composite microalloyed silicon-aluminum alloy Al-50% Si-0.3% Nb-0.3% Mn alloy.
The heat conductivity of the prepared Al-50% Si-0.3% Nb-0.3% Mn alloy is 162W/(m.K) through detection, and the thermal expansion coefficient is 11.3 multiplied by 10-6K-1The tensile strength was 315MPa, the bending strength was 397MPa, and the hardness was 193 HB.
Referring to FIG. 1, the microstructure of the Al-50% Si-0.3% Nb-0.3% Mn alloy is reflected. As can be seen from FIG. 1, the composite microalloyed Al-50% Si-0.3% Nb-0.3% Mn alloy has uniform and fine structure, smooth and round Si particle surface and no sharp edges.
In addition, XRD characterization shows that Nb atoms interact with Si, Al and Mn atoms to form a new crystal lattice. Because the structural difference of Nb atoms and other atoms is very large, the acting forces are different, so that the Nb atoms generate large vibration near the equilibrium position, and the heat-conducting property of the solid depends on the vibration in crystal lattices, so that the heat-conducting property of the aluminum-silicon alloy can be obviously improved by adding Nb, namely the heat conductivity is improved.
Example 2
In the embodiment, monocrystalline silicon is used as a silicon source, high-purity aluminum with the content of 99.998-99.999% is used as an aluminum source, an Al-Sc intermediate alloy with the Sc content of 2% is used as an X source, pure Cu is used as a Y source, and Sc and Cu are doped into the silicon-aluminum alloy according to the mass ratio of 50% of Si, 0.1% of Sc, 0.5% of Cu and the balance of aluminum, and the preparation method specifically comprises the following steps:
s1, melting a silicon source, an aluminum source, an X source and a Y source together to obtain a melt;
high purity aluminum is gradually melted by heating to 850 ℃. After the high-purity aluminum is completely melted, the temperature is continuously raised to 1300 ℃, and the monocrystalline silicon is added in batches. And after the monocrystalline silicon is completely melted, cooling to 760 ℃, adding Cu, then adding Al-Sc intermediate alloy, and fully stirring for 5min to obtain a melt.
S2, applying atomization pressure to the melt to atomize and deposit the melt to form a billet;
the melt was then slagged with a slag former comprising 30% NaCl, 47% KCl, 23% cryolite and degassed with hexachlorohexane. Standing for 10min, and pouring the melt into a tundish with a preheating temperature of 950 ℃. Simultaneously, high-pressure nitrogen is opened, and 1.2MPa of atomization pressure is applied to the melt to atomize the melt into powder, so that a deposition billet with the diameter of 350mm and the height of 560mm is obtained on a deposition disc with the receiving distance of 630 mm.
And S3, sequentially densifying and thermally treating the billet to obtain the composite microalloyed silicon-aluminum alloy.
Densification treatment: the deposition ingot was placed in a hot isostatic pressing furnace, which was heated to a temperature of 540 ℃ while applying a pressure of 180MPa and maintaining the pressure for 2 h.
And (3) heat treatment: the densified alloy ingot is cut into small blocks with the size of 85mm multiplied by 10mm, and the small blocks are placed in a box-type resistance furnace to be heated to 515 ℃ at the speed of 20 ℃/min. After keeping the temperature for 4h, oil quenching is carried out on the mixture by using oil at the temperature of 90 ℃. And finally, placing the small blocks in a box-type resistance furnace, heating to 180 ℃ at the speed of 20 ℃/min, preserving the temperature for 24 hours, taking out, and air-cooling to obtain the final composite microalloyed silicon-aluminum alloy Al-50% Si-0.1% Sc-0.5% Cu alloy.
Referring to FIG. 2, the microstructure of the Al-50% Si-0.1% Sc-0.5% Cu alloy is reflected. As can be seen from FIG. 2, the composite microalloyed Al-50% Si-0.1% Sc-0.5% Cu alloy has uniform and fine structure, smooth and round Si particle surface and no sharp edges. The heat conductivity of the Al-50% Si-0.1% Sc-0.5% Cu alloy is 147W/(m.K), and the thermal expansion coefficient is 11.1X 10-6K-1The tensile strength is 353MPa, the bending strength is 440MPa, and the hardness is 215 HB.
The above results may be due to the fact that Sc atoms interact with Si, Al, and Cu atoms to form a new lattice, and the Sc atoms vibrate to a greater extent near their equilibrium positions, thereby improving the thermal conductivity of the aluminum-silicon alloy.
Example 3
In the embodiment, monocrystalline silicon is used as a silicon source, high-purity aluminum with the content of 99.998-99.999% is used as an aluminum source, an Al-Zr intermediate alloy with the Zr content of 10% is used as an X source, pure Mg is used as a Y source, Zr and Mg are doped into the silicon-aluminum alloy according to the mass ratio of 50% of Si, 0.2% of Zrs, 0.3% of Mg and the balance of aluminum, and the preparation method specifically comprises the following steps:
s1, melting a silicon source, an aluminum source, an X source and a Y source together to obtain a melt;
high purity aluminum is gradually melted by heating to 850 ℃. After the high-purity aluminum is completely melted, the temperature is continuously raised to 1300 ℃, and the monocrystalline silicon is added in batches. And (3) cooling to 760 ℃ after the monocrystalline silicon is completely melted, adding Mg, then adding Al-Zr intermediate alloy, and fully stirring for 5min to obtain a melt.
S2, applying atomization pressure to the melt to atomize and deposit the melt to form a billet;
the melt was then slagged with a slag former comprising 30% NaCl, 47% KCl, 23% cryolite and degassed with hexachlorohexane. Standing for 10min, and pouring the melt into a tundish with a preheating temperature of 950 ℃. Simultaneously, high-pressure nitrogen is opened, and 1.2MPa of atomization pressure is applied to the melt to atomize the melt into powder, so that a deposition billet with the diameter of 350mm and the height of 560mm is obtained on a deposition disc with the receiving distance of 630 mm.
And S3, sequentially densifying and thermally treating the billet to obtain the composite microalloyed silicon-aluminum alloy.
Densification treatment: the deposition ingot was placed in a hot isostatic pressing furnace, which was heated to a temperature of 540 ℃ while applying a pressure of 180MPa and maintaining the pressure for 2 h.
And (3) heat treatment: the densified alloy ingot is cut into small blocks with the size of 85mm multiplied by 10mm, and the small blocks are placed in a box-type resistance furnace to be heated to 515 ℃ at the speed of 20 ℃/min. After keeping the temperature for 4h, oil quenching is carried out on the mixture by using oil at the temperature of 90 ℃. And finally, placing the small blocks in a box-type resistance furnace, heating to 180 ℃ at the speed of 20 ℃/min, preserving the temperature for 24 hours, taking out, and air-cooling to obtain the final composite microalloyed silicon-aluminum alloy Al-50% Si-0.2% Zr-0.3% Mg alloy.
Referring to FIG. 3, the microstructure of the Al-50% Si-0.2% Zr-0.3% Mg alloy is reflected. From FIG. 3, it can be seen that the composite microalloyed Al-50% Si-0.2% Zr-0.3% Mg alloy has uniform and fine structure, smooth and round Si particle surface and no sharp edges. Referring to FIG. 4, which shows the case processed using the Al-50% Si-0.2% Zr-0.3% Mg alloy, it can be seen from FIG. 4 that the product processed using the Al-50% Si-0.2% Zr-0.3% Mg alloy is fine and has no cracks.
Furthermore, the results of the tests showed that the Al-50% Si-0.2% Zr-0.3% Mg alloy had a thermal conductivity of 152W/(mK) and a thermal expansion coefficient of 11.3X 10-6K-1The tensile strength was 315MPa, the bending strength was 397MPa, and the hardness was 193 HB.
Comparative example
For comparison, only Y is from a silicon source and an aluminum source and is smelted together to form an alloy, namely monocrystalline silicon is used as the silicon source, high-purity aluminum with the content of 99.998-99.999% is used as the aluminum source, an Al-Mn intermediate alloy with the content of Mn of 10% is used as the Y source, Mn is doped into the silicon-aluminum alloy according to the mass ratio of 50% of Si, 0.3% of Mn and the balance of aluminum, and the preparation steps are as follows:
firstly, smelting a silicon source, an aluminum source, an X source and a Y source together to obtain a melt: specifically, high-purity aluminum is heated to 800-870 ℃ to be gradually melted. And after the high-purity aluminum is completely melted, continuously heating to 1200-1400 ℃, and adding the monocrystalline silicon in batches. And after the monocrystalline silicon is completely melted, cooling to 750-820 ℃, adding an Al-Mn intermediate alloy, and fully stirring for 5-10 min to obtain a melt.
The same operations as in steps S2 and S3 of example 1 were carried out to finally obtain an Al-50% Si-0.3% Mn alloy.
The thermal conductivity of the Al-50% Si-0.3% Mn alloy is 145W/(m.K), and the thermal expansion coefficient is 11.0 multiplied by 10-6K-1The tensile strength is 309MPa,the bending strength is 380MPa, and the hardness is 190 HB. It can be seen that the thermal conductivity and mechanical strength of the Al-50% Si-0.3% Mn alloy are not as good as those of the Nb-added Al-50% Si-0.3% Nb-0.3% Mn alloy.
Compared with the prior art, the aluminum-silicon alloy has the advantages that Mg and/or Cu and/or Mn are added into the aluminum-silicon alloy, Nb, Zr and Sc elements are added, Nb, Zr and Sc atoms interact with various atoms of Si, Al, Mg and/or Cu and/or Mn to form crystal lattices, and the Nb, Zr and Sc atoms have extremely high structural difference with other atoms and act with each other unevenly, so that the Nb, Zr and Sc atoms vibrate greatly near the equilibrium position of the Nb, Zr and Sc atoms, and the heat conductivity of the solid depends on the vibration in the crystal lattices, so that the heat conductivity of the aluminum-silicon alloy can be obviously improved by adding Nb, namely the heat conductivity is improved. Meanwhile, the Mg, the Cu and the Mn can improve the mechanical strength of the aluminum-silicon alloy and further enhance the strength of the aluminum-silicon alloy.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.

Claims (5)

1. The composite microalloyed aluminum-silicon alloy is characterized by comprising the following components in percentage by mass:
Si：48.0～52.0％；
X：0.1～0.4％；
Y：0.1～0.5％；
the balance of Al;
the X comprises Nb, and the rest is one or two of Sc and Zr; y is one or more of Mg, Cu and Mn;
the composite microalloyed aluminum-silicon alloy is prepared by the following preparation steps:
s1, melting a silicon source, an aluminum source, an X source and a Y source together at the temperature of 750-1300 ℃ to obtain a melt;
s2, applying atomization pressure of 0.9-1.3 MPa to the melt, atomizing and depositing to form a billet;
s3, sequentially densifying and thermally treating the alloy billet to obtain the composite microalloyed silicon-aluminum alloy; wherein the densification is performed in an environment with a temperature of 520 to 600 ℃ and a pressure of 45 to 180 MPa.
2. The composite microalloyed aluminum-silicon alloy as claimed in claim 1, wherein: the thermal conductivity of the composite microalloyed aluminum-silicon alloy is 147-162W/(m.K).
3. The composite microalloyed aluminum-silicon alloy as claimed in claim 2, wherein: the tensile strength of the composite microalloyed aluminum-silicon alloy is 315-353 MPa, the bending strength is 397-440 MPa, and the hardness is 193-215 HB.
4. The composite microalloyed aluminum-silicon alloy as claimed in claim 3, wherein: the silicon source comprises monocrystalline silicon; the aluminum source is pure aluminum; the X source comprises an Al-Nb master alloy, and the Y source comprises one or more of pure Cu, pure Mg and an Al-Mn master alloy.
5. The composite microalloyed aluminum-silicon alloy as claimed in claim 4, wherein: the X source also includes master alloys of Sc and/or Zr.
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