CN115537611A - High-thermal-conductivity low-expansion Al-Si-Ni-based alloy and preparation method thereof - Google Patents
High-thermal-conductivity low-expansion Al-Si-Ni-based alloy and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of cast aluminum alloy, and discloses high-thermal-conductivity low-expansion Al-Si-Ni-based alloy and a preparation method thereof. The alloy comprises the following components in percentage by mass: 20 to 30 percent of Si, 10 to 20 percent of Ni, 1 to 3 percent of Cu, 0 to 1 percent of Mg, 0.1 to 0.3 percent of P and the balance of Al. The method comprises the following steps: 1) Preparing an Al-Si-Ni alloy melt; 2) Adding micro-alloying elements Cu and Mg; 3) Refining and P modification treatment; 4) Sub-rapid solidification; 5) And (6) heat treatment. The method is simple and low in cost; the obtained alloy has high heat-conducting property, low thermal expansion coefficient, low melting point and better casting property, is suitable for a smelting casting process, and has high casting density; the alloy of the invention has higher strength. The alloy of the invention meets the performance requirements of aluminum-based alloy for electronic packaging.
Description
Technical Field
The invention relates to the technical field of cast aluminum alloy, in particular to high-thermal-conductivity low-expansion cast aluminum alloy and a preparation method thereof.
Background
With the development of electronic component technology and the continuous improvement of integrated technology, integrated circuits have the development trends of high power, high integration degree, miniaturization and light weight. The problem that follows is that the heat generation of the integrated circuit is increased sharply, which is liable to cause thermal fatigue of the chip or the device and thermal mismatch between materials to cause the life of the device to be reduced. Therefore, in the field of electronic packaging, there is an increasing demand for high thermal conductivity and low expansion materials, and in order to achieve light weight of devices and products, the electronic packaging materials also need to have a lower density. The aluminum alloy has the advantages of high heat conductivity, high specific strength, good processing performance, corrosion resistance and the like, and is widely applied to the fields of automobiles, aerospace, communication, electronics, buildings and the like at present. The aluminum matrix composite has excellent properties of high thermal conductivity, low expansion, low density and better welding and surface plating properties, and is currently applied to shells, cover plates and the like in the packaging of electronic power devices such as microwave power devices, integrated power modules, T/R modules and the like. In addition, the aluminum alloy and the aluminum-based composite material have the advantages of low density and easiness in recovery, and are more favorable for realizing light weight of products and reducing carbon emission, so that the development of the aluminum alloy or the aluminum-based composite material with high heat conduction and low expansion characteristics has important research significance.
Among high thermal conductivity low expansion materials for electronic packaging, high Si content Si/Al and high SiC content SiC/Al composites are the most attractive material systems (Zhang Di, et Al, current application and development trends of metal matrix composites for thermal management, chinese material evolution, 2018, 37 (12): 994-1001), which are mainly manufactured by spray molding and powder metallurgy. Particularly, the Si/Al alloy composite material with high Si content (50-70%) has low cost and stable performance, and is most concerned in a heat management material system. But the melting point is very high (> 1200 ℃), and the structure is very thick and large after the molding based on the common casting process, the brittleness is high, and the processing and using requirements of the heat management device cannot be met.
The development of aluminum matrix composite systems with both high thermal conductivity and low expansion has been receiving much attention. For example, the invention patent with the publication number of CN103014400B discloses an oriented high-thermal-conductivity low-expansion graphite-aluminum composite material and a preparation method thereof. The invention takes the crystalline flake graphite with high graphitization degree, adopts impact vibration to lead the graphite crystalline flake to present regular directional arrangement, and strengthens the interface combination between the graphite and the aluminum matrix by forced pressurization, thus leading the metal to deeply infiltrate into the interior of the graphite crystalline flake and preparing the crystalline flake graphite aluminum metal matrix composite material with excellent service performance. The composite material has excellent performance, and a prefabricated body is required to be obtained firstly in the preparation process, then metal is smelted, and the composite material is obtained by adopting an extrusion infiltration method. The method has the advantages of complex process flow, harsh required equipment and preparation process conditions, relatively high preparation cost, obvious anisotropy of material performance and unsuitability for large-scale industrial application.
Chinese patent CN103160716A discloses a low-expansion high-strength AlN-Si-Al hybrid material and a preparation method thereof, and the invention prepares an aluminum-based composite material with uniform tissue, high heat conduction and low expansion by using granular AlN and Si as reinforcing phases through a powder metallurgy process. However, the method has high requirements on the particle size of the raw material, the preparation process of the powder metallurgy process is complex, the equipment requirement is high, the compactness of the material needs to be improved by matching with the hot pressing process, and the production cost is high.
The patent technology relates to a high-thermal-conductivity low-expansion aluminum-based composite material, a high-thermal-conductivity aluminum alloy and a preparation process thereof, and although the high-thermal-conductivity low-expansion aluminum alloy shows excellent high-thermal-conductivity and low-expansion characteristics, the preparation mainly adopts solid powder metallurgy and powder injection molding, the process flow is complex, the requirement on production equipment is high, and the manufacturing cost is high. In the traditional manufacturing process, the casting method is a low-cost manufacturing process which can realize the preparation of complex parts and has relatively simple production flow. For Si/Al alloy with high Si content, the melting point is high, the solidification interval is large, and the alloy is difficult to form by using a common casting process.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention provides a high-thermal-conductivity low-expansion alloy system suitable for a smelting casting process and a preparation method thereof, namely a high-thermal-conductivity low-expansion Al-Si-Ni-based cast aluminum alloy and a preparation method thereof, and a preparation process with low cost is realized while the thermal performance requirements of electronic packaging materials are met.
In the invention, the Ni element has low solid solubility in alpha-Al and has small influence on the heat conductivity in the alloy, and the formed Al 3 The Ni phase has a low coefficient of thermal expansion. In particular, the Al-Si-Ni ternary alloy has a eutectic point content of 11% by weight Si-5% by weight Ni, and a eutectic point of 567 ℃,even 10 ℃ lower than the Al-Si (12.6%) eutectic temperature. Namely, the melting point of the Al-Si alloy is slightly influenced and even slightly reduced after a larger amount of Ni element is added into the Al-Si alloy, and eutectic reaction also exists. Therefore, the invention provides and designs the high-alloying Al-Si-Ni-based alloy by utilizing the characteristic, which is not only beneficial to further reducing the thermal expansion coefficient of the alloy on the premise of ensuring high heat conduction, but also beneficial to reducing the melting point and accompanying eutectic reaction in the solidification process, thereby ensuring that the high-quality preparation can be carried out by utilizing the common solidification casting process technology. In the casting preparation of high-alloying alloy, the improvement of the cooling rate is beneficial to realizing the refinement of the alloy phase. The sub-rapid solidification of the alloy is realized through the water-cooling copper mold, the process is simple and convenient, the primary phase in the alloy can be effectively refined, and the thermal conductivity is improved. The heat treatment can effectively improve the heat conductivity of the Al-Si alloy, and the second phase dispersed and precipitated in the aging process can ensure the hardness and strength of the alloy. Aiming at the problems of high melting point, complex preparation process, high preparation cost and the like of the high-content Al-Si alloy for electronic packaging at present, the invention provides an Al-Si-Ni alloy system which is based on hypereutectic Al-Si-Ni alloy, assisted with elements such as Cu, mg and the like to carry out micro alloying treatment and P modification treatment, and carries out sub-rapid solidification and heat treatment on the alloy system to obtain high heat conduction, low expansion, low density and low melting point and is suitable for a smelting and casting process, and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
a high-thermal-conductivity low-expansion Al-Si-Ni-based alloy comprises the following components in percentage by mass:
the balance being Al.
Preferably, it is
The balance being Al.
The preparation method of the high-thermal-conductivity low-expansion Al-Si-Ni-based alloy comprises the following steps of:
(1) Preparing an Al-Si-Ni alloy melt: melting pure aluminum, al-Si intermediate alloy and pure Ni, stirring, standing and preserving heat to obtain Al-Si-Ni alloy melt;
(2) Adding micro-alloying elements Cu and Mg: adding an Al-Cu and Al-Mg intermediate alloy into the Al-Si-Ni alloy melt, melting, stirring, standing and preserving heat to obtain an aluminum alloy melt;
(3) Refining and P modification treatment: adding Ni-P intermediate alloy into the aluminum alloy melt obtained in the step (2), melting, stirring, standing and preserving heat to obtain an aluminum alloy melt subjected to modification treatment; refining and deslagging the alloy melt subjected to the modification treatment to obtain a treated aluminum alloy melt;
(4) Sub-rapid solidification: cooling the mold with water, and adding the aluminum alloy melt treated in the step (3) into the cooled mold to obtain a hypereutectic Al-Si-Ni alloy casting;
(5) And (3) heat treatment: the casting of the hypereutectic Al-Si-Ni alloy is subjected to heat preservation treatment for 6 to 8 hours at the temperature of between 510 and 530 ℃, water quenching and aging treatment for 8 to 12 hours at the temperature of between 210 and 230 ℃ to obtain the high-heat-conductivity low-expansion Al-Si-Ni-based alloy.
The melting temperature in the step (1) is 850-950 ℃; stirring for 1-2 min, standing and preserving heat for 8-12 min, wherein the Al-Si intermediate alloy is Al-50Si intermediate alloy.
The melting temperature in the step (2) is 850-950 ℃; the stirring time is 1-2 min, and the standing and heat preservation time is 8-12 min.
The Al-Cu intermediate alloy is Al-50Cu intermediate alloy; the Al-Mg intermediate alloy is Al-10Mg intermediate alloy.
And (3) removing scum on the surface of the Al-Si-Ni alloy melt before adding the Al-Cu and Al-Mg intermediate alloy into the Al-Si-Ni alloy melt in the step (2).
In the step (3), refining deslagging is carried out by adding a refining agent and a deslagging agent by using a nitrogen blowing method;
the commercial brands of the refining agent and the deslagging agent are YT-J-1 and YT-D-4 respectively, according to the proportion of 1:1, mixing, and then uniformly mixing, wherein the total addition amount is 1 percent of the weight of the melt.
The melting temperature in the step (3) is 850-950 ℃; the stirring time is 1-2 min, and the standing and heat preservation time is 10-25 min.
And (4) in the process of adding the aluminum alloy melt treated in the step (3) into the cooled mold, the mold is cooled by water all the time.
The die in the step (4) is a copper die; and starting a cooling water circulation system in the water-cooled copper mold, and quickly casting the melt into the water-cooled copper mold.
The principle of the invention is as follows:
si is an effective element for realizing low expansion, the higher the content is, the lower the expansion coefficient is, but the higher the melting point of the alloy is, the cast molding is not facilitated, the Si phase is easy to be coarse, the brittleness of the alloy is high, and the alloy has better casting performance when the Si content is 10-30%. Ni element can generate Al in Al alloy 3 The Ni phase is a neutral phase with good heat conductivity and low thermal expansion coefficient, and the addition of the Ni element is beneficial to the reduction of the melting point of the alloy, and a ternary eutectic reaction occurs in the solidification process. The sub-rapid solidification can ensure that the cooling rate of the melt reaches more than 100 ℃/s, the structure of the alloy can be effectively refined, and the refining effect of the primary Si phase is obvious. The addition of the P element can form a fine AlP phase in the melt to become a nucleation core for Si phase precipitation, so that the primary Si phase is further refined. Cu and Mg elements are respectively Al in Al-Si-Ni alloy 2 Cu phase and Mg 2 The Si phase exists, al can be made by aging heat treatment 2 Cu phase and Mg 2 Si phase is dispersed and precipitated in the matrix, and the hardness and the strength of the alloy are improved.
The Ni element is mainly Al in the Al-Si alloy 3 The Ni phase exists in the form of a low expansion phase, and the rising amplitude of the melting point of the alloy added with the Ni element in the Al-Si alloy is far smaller than that of the alloy added with the Si element with the same content. The invention uses Ni element with low solid solubility to replace partial Si element in Al-Si alloy with high content, thereby ensuring excellent performances of high heat conduction, low expansion and low density, and simultaneously ensuring that the alloy has better casting performance and lower melting point. The P element can form an AlP phase in the Al alloy and provide a nucleation site for a primary Si phasePoint, thereby refining the Si phase; the addition of Cu and Mg further reduces the melting point of the alloy, improves the casting performance of the alloy, and can disperse and separate out Al after heat treatment 2 Cu-bonded Mg 2 Si phase, which ensures the alloy strength. The sub-rapid solidification can effectively refine the primary phase in the alloy, and the heat treatment can spheroidize the eutectic phase in the alloy and disperse and separate out solid solution atoms in the form of a second phase, so that the heat conductivity of the alloy is improved. The hypereutectic Al-Si-Ni alloy is suitable for common smelting and casting processes, and compared with a spray deposition method and a powder metallurgy method, the sub-rapid solidification method has the advantages of simpler preparation process, lower preparation cost and higher density.
Compared with the existing high-content Al-Si alloy and the preparation process thereof, the invention has the following advantages and beneficial effects:
(1) The invention obtains an alloy system which has high heat conduction, low expansion and low melting point and is suitable for common smelting and casting processes and a preparation process technology thereof.
(2) Aiming at the problems of high melting point and complex preparation process of the high-content Al-Si alloy for electronic packaging at present, the alloy system provided by the invention has low melting point and good casting performance and is suitable for common smelting and casting processes.
(3) Aiming at the aluminum alloy for electronic packaging, the invention realizes the synchronous improvement of heat conduction and thermal expansion performance, improves the heat conductivity of the alloy through the regulation and control of the structure morphology, and realizes the reduction of the thermal expansion coefficient by adding Ni element. The heat conductivity of the alloy prepared by the invention can reach 100-120W/(m.K), and the average thermal expansion coefficient can reach 10-11.5 multiplied by 10 -6 /K。
(4) Aiming at the aluminum alloy for electronic packaging, the invention leads the alloy hardness to reach more than 200HV through the processes of sub-rapid solidification, micro-alloying treatment, modification treatment, heat treatment and the like.
In a word, the method of the invention is simple and has low cost; the obtained alloy has high heat-conducting property, low thermal expansion coefficient, low melting point and good casting property, is suitable for smelting casting process, and has high casting density; the alloy of the invention has higher strength. The alloy of the invention can meet the performance requirements of aluminum-based alloy for electronic packaging.
Drawings
FIG. 1 is an optical microstructure of an alloy of comparative example 1;
FIG. 2 is an optical microstructure of an alloy of comparative example 2;
FIG. 3 is an optical microstructure of the alloy prepared in example 1;
FIG. 4 is an SEM microstructure of the alloy prepared in example 1;
figure 5 is an XRD pattern of the alloy prepared in example 1.
Detailed Description
In order to more intuitively explain the implementation effect of the invention, the preparation process of the high-thermal-conductivity low-expansion aluminum alloy and the structure and performance characteristics of the high-thermal-conductivity low-expansion aluminum alloy are explained by combining the attached drawings, the comparative examples and the embodiments.
Comparative example 1: ordinary solidification casting forming of Al-50Si alloy
The material used in the comparative example is Al-50Si intermediate alloy, the die adopts a No. 45 steel sheet die with the thickness of 100mm multiplied by 45mm multiplied by 15mm, and the preparation process and the parameters thereof are as follows:
(1) Alloy smelting: melting the weighed Al-50Si alloy at 1250 ℃. Stirring for 2min after the materials are completely melted to make the components uniform, and standing for 10min under the condition of heat preservation.
(2) Casting and molding: adding a refining agent and a slag removing agent, stirring for 1-2 min, removing floating slag on the surface of the melt, casting into a mold, and molding.
In order to characterize the structural and performance properties of the above alloys, the microstructure of the alloys was observed using an optical microscope (model: lecia DFC, standard: JB/T7946-2017) and a scanning electron microscope (model: zeiss Merlin). The coefficient of linear expansion of the alloy was measured using a thermomechanical analyzer (model: TMA Q400, dimensions: 4 mm. Times.4 mm. Times.15 mm standard: GB/T4339-2008). Using a flash thermal conductivity meter (model: NETZSCHLFA, size:
and (3) standard: GB/T22588-2008) testThermal conductivity.
The Al-50Si alloy structure consists of primary Si phase and eutectic Si phase combined alpha-Al dendrite. Because the Si content is too high, the primary Si phase is extremely coarse, and the coarse Si phases are mutually overlapped in the early stage of the solidification process, so that the casting performance of the alloy is deteriorated, the liquid phase flow is hindered, and more casting defects such as air holes exist in the alloy. Too high Si content also leads to an alloy melting point as high as 1150 ℃, and the melting temperature needs to be over 1250 ℃ in order to ensure that a certain degree of superheat can realize casting. The alloy has a thermal conductivity of 80W/(m.K) at 25 ℃ and an average linear expansion coefficient of 10.45 multiplied by 10 at 25-100 DEG C -6 The hardness is 72HV. The thermal expansion coefficient is determined by the volume fraction of low-expansion phases in the alloy and is insensitive to the structure morphology of the alloy, and the Al-50Si alloy has low thermal expansion coefficient, but has poor casting performance, low thermal conductivity and high melting point. The Al-50Si alloy cast by the smelting process cannot meet the performance requirements of the current electronic packaging material.
FIG. 1 is an optical microstructure of the alloy of comparative example 1.
To further illustrate the effects of the present invention, the following examples are given to illustrate the present invention.
Example 1: al-20Si-20Ni-1Cu-0.5Mg alloy
Compared with the proportion 1, in addition to the optimization of the alloy system, the embodiment adopts the water-cooled copper mold to perform the sub-rapid solidification, and the heat treatment process is added.
The alloy prepared by the embodiment comprises Al-20Si-20Ni-1Cu-0.5Mg, and is prepared from the following raw materials in percentage by mass: 20% of Si, 20% of Ni, cu:1%, mg:0.5%, P:0.3 percent and the balance of Al.
The preparation method comprises the following specific steps:
(1) Alloy smelting:
melting weighed industrial pure aluminum, al-50Si intermediate alloy and pure Ni at 870 ℃, stirring for 2min after all the materials are melted, and standing for 10min under the condition of heat preservation; adding Al-50Cu intermediate alloy and Al-10Mg intermediate alloy into the melt, stirring for 2min after the alloy is completely melted, and standing for 10min while keeping the temperature to obtain the melt with uniform components.
(2) Modification and refining
Adding Ni-18P intermediate alloy into the melt in the step (1), stirring for 2min after the melt is completely melted, and standing for 20min under the condition of heat preservation. Adding a refining agent and a deslagging agent by using a nitrogen blowing method, wherein the commercial brands of the refining agent and the deslagging agent are YT-J-1 and YT-D-4 respectively, and the refining agent and the deslagging agent are added according to the proportion of 1:1 ingredient (mass ratio), then evenly mixing, wherein the total addition amount is 1 percent of the weight of the melt, and removing scum on the surface of the melt after stirring for 1-2 min.
(3) Sub-rapid solidification and heat treatment
And (3) starting a cooling water system in the water-cooled copper mold, and quickly pouring the melt in the step (2) into the water-cooled copper mold with the thickness of 100mm multiplied by 45mm multiplied by 15mm to obtain a hypereutectic Al-Si-Ni alloy casting. The Al-20Si-20Ni-1Cu-0.5Mg alloy casting is subjected to solution treatment (520 ℃ multiplied by 6h + water quenching), and then is subjected to aging (220 ℃ multiplied by 10 h).
The alloy of this example was subjected to structure observation and phase analysis, and the aged Al-20Si-20Ni-1Cu-0.5Mg alloy consisted essentially of an alpha-Al matrix, al 3 Ni phase, si phase and a small amount of net Al-Ni-Cu ternary phase. Compared with the comparative example, the structure is obviously refined, the primary Si phase is irregular small block, and Al 3 The Ni phase is in a strip shape, the primary Si phase is refined through sub-rapid solidification and P modification treatment, the casting performance of the alloy is improved, and compared with a comparative example, the density of the component casting is higher and the casting quality is better. The alloy has the melting point of 810 ℃, the thermal conductivity of 105.25W/(m.K) at 25 ℃ and the average linear expansion coefficient of 10.58 multiplied by 10 at 25-100 ℃ according to tests -6 and/K, hardness 223HV.
Therefore, the components of the embodiment have lower thermal expansion coefficient, lower melting point and better casting performance, are suitable for a smelting casting process, are matched with a sub-rapid solidification and heat treatment process and modification treatment, have obviously refined alloy tissues, obtain better heat-conducting performance and meet the thermal performance requirement of the aluminum-based alloy for electronic packaging.
FIG. 3 is an optical microstructure of the alloy prepared in example 1; FIG. 4 is an SEM microstructure of the alloy prepared in example 1; figure 5 is an XRD pattern of the alloy prepared in example 1.
Example 2: al-25Si-15Ni-3Cu-0.5Mg alloy
The preparation process of the embodiment is basically consistent with that of the embodiment 1, and only differences exist in smelting temperature and heat treatment process parameters.
The alloy prepared by the embodiment comprises Al-25Si-15Ni-3Cu-0.5Mg, and is prepared from the following raw materials in percentage by mass: 25% of Si, 15% of Ni, cu:3%, mg:0.5%, P:0.3 percent and the balance of Al.
The preparation method comprises the following specific steps:
(1) Alloy smelting:
melting weighed industrial pure aluminum, al-50Si intermediate alloy and pure Ni at 895 ℃, stirring for 2min after all the materials are melted, and standing for 10min under the condition of heat preservation. Adding Al-50Cu intermediate alloy and Al-10Mg intermediate alloy into the melt, stirring for 2min after the alloy is completely melted, and standing for 10min under the condition of heat preservation to obtain the melt with uniform components.
(2) Modification and refining
Adding Ni-18P intermediate alloy into the melt in the step (1), stirring for 2min after the melt is completely melted, and standing for 20min under the condition of heat preservation. Adding a refining agent and a deslagging agent by using a nitrogen blowing method, wherein the commercial brands of the refining agent and the deslagging agent are YT-J-1 and YT-D-4 respectively, and the refining agent and the deslagging agent are added according to the proportion of 1:1, mixing materials, then uniformly mixing, wherein the total addition amount is 1 percent of the weight of the melt, and removing scum on the surface of the melt after stirring for 1-2 min.
(3) Sub-rapid solidification and heat treatment
And (3) starting a cooling water system in the water-cooled copper mold, and quickly pouring the melt in the step (2) into the water-cooled copper mold with the thickness of 100mm multiplied by 45mm multiplied by 15mm to obtain the hypereutectic Al-Si-Ni alloy casting. The Al-25Si-15Ni-3Cu-0.5Mg alloy casting is subjected to solution treatment (510 ℃ multiplied by 7h + water quenching), and then is aged (210 ℃ multiplied by 12 h).
The alloy of the embodiment is subjected to structure observation and phase analysis, the structure appearance of the aging Al-25Si-15Ni-3Cu-0.5Mg alloy is similar to that of the embodiment 1, and the alloy mainly comprises an alpha-Al matrix and Al 3 Ni phase, and Si phase and a small amount of stripsForm Al 3 Ni 2 The phase and an Al-Ni-Cu ternary phase, wherein the Al-Si-Ni ternary phase is wrapped in Al 3 The Ni phase is in the middle. Small amount of Al due to increased Ni content and copper content 3 The Ni phase is wrapped by Al-Ni-Cu ternary phase for growth. Compared with the comparative example, the structure is obviously refined, the primary Si phase is irregular small block, and Al 3 The Ni phase is thick and long. The primary Si phase is refined through sub-rapid solidification and P modification, the casting performance of the alloy is improved, and compared with a comparative example, the density of the component casting is higher and the casting quality is better. The alloy is tested to have a melting point of 835 ℃, a thermal conductivity of 108.7W/(m.K) at 25 ℃ and an average linear expansion coefficient of 11.18 multiplied by 10 at 25-100 DEG C -6 and/K, hardness 241HV.
Therefore, the components of the embodiment have lower thermal expansion coefficient, lower melting point and better casting performance, are suitable for a smelting casting process, are matched with a sub-rapid solidification and heat treatment process and modification treatment, have obviously refined alloy tissues, obtain better heat-conducting performance and meet the thermal performance requirement of the aluminum-based alloy for electronic packaging.
Example 3: al-30Si-10Ni-2Cu-0.5Mg alloy
The preparation process of the embodiment is basically consistent with that of the embodiment 1, and only differences exist in smelting temperature and heat treatment process parameters.
The alloy prepared by the embodiment comprises Al-30Si-10Ni-2Cu-0.5Mg, and is prepared from the following raw materials in percentage by mass: 30% of Si, 10% of Ni, cu:2%, mg:0.5%, P:0.3 percent and the balance of Al.
The preparation method comprises the following specific steps:
(1) Alloy melting
Melting weighed industrial pure aluminum, al-50Si intermediate alloy and pure Ni at 940 ℃, stirring for 2min after all the materials are melted, and standing for 10min under the condition of heat preservation. Adding Al-50Cu intermediate alloy and Al-10Mg intermediate alloy into the melt, stirring for 2min after the alloy is completely melted, and standing for 10min under the condition of heat preservation to obtain the melt with uniform components.
(2) Modification and refining
Adding Ni-18P intermediate alloy into the melt in the step (1), stirring for 2min after the melt is completely melted, and standing for 20min under the condition of heat preservation. Adding a refining agent and a deslagging agent by using a nitrogen blowing method, wherein the commercial brands of the refining agent and the deslagging agent are YT-J-1 and YT-D-4 respectively, and the refining agent and the deslagging agent are added according to the proportion of 1:1, mixing materials, then uniformly mixing, wherein the total addition amount is 1 percent of the weight of the melt, and removing scum on the surface of the melt after stirring for 1-2 min.
(3) Sub-rapid solidification and heat treatment
And (3) starting a cooling water system in the water-cooled copper mold, and quickly pouring the melt in the step (2) into the water-cooled copper mold with the thickness of 100mm multiplied by 45mm multiplied by 15mm to obtain a hypereutectic Al-Si-Ni alloy casting. The Al-30Si-10Ni-2Cu-0.5Mg alloy casting is subjected to solution treatment (530 ℃ multiplied by 8h + water quenching), and then is aged (230 ℃ multiplied by 12 h).
The alloy of this example was subjected to structure observation and phase analysis, and the aged Al-30Si-10Ni-2Cu-0.5Mg alloy had a structure similar to that of example 1, and consisted essentially of an α -Al matrix, al 3 Ni phase, and Si phase with a small amount of Al in the form of a strip 3 Ni 2 The phase and the Al-Ni-Cu ternary phase form a small amount of Al-Si-Ni ternary phase to wrap Al 3 The surface of Ni phase. Compared with the comparative example, the structure is obviously refined, the primary Si phase is irregular small block, and Al 3 The Ni phase is thick and long. The primary Si phase is refined through sub-rapid solidification and P modification treatment, the casting performance of the alloy is improved, and compared with a comparative example, the density of the component casting is higher and the casting quality is better. The alloy has a melting point of 880 ℃, a thermal conductivity of 115.83W/(m.K) at 25 ℃ and an average linear expansion coefficient of 10.83 multiplied by 10 at 25-100 ℃ according to tests -6 The hardness is 190HV.
Therefore, the components of the embodiment have lower thermal expansion coefficient, lower melting point and better casting performance, are suitable for a smelting casting process, are matched with a sub-rapid solidification and heat treatment process and modification treatment, have obviously refined alloy tissues, obtain better heat-conducting performance and meet the thermal performance requirement of the aluminum-based alloy for electronic packaging.
Example 4: al-22Si-18Ni-3Cu-0.8Mg alloy
The preparation process of the embodiment is basically consistent with that of the embodiment 1, and only differences exist in smelting temperature and heat treatment process parameters.
The alloy prepared by the embodiment comprises Al-22Si-18Ni-3Cu-0.8Mg, and is prepared from the following raw materials in percentage by mass: 22% of Si, 18% of Ni, cu:3%, mg:0.8%, P:0.3 percent and the balance of Al.
The preparation method comprises the following specific steps:
(1) Alloy melting
Melting weighed industrial pure aluminum, al-50Si intermediate alloy and pure Ni at 880 ℃, stirring for 2min after all the materials are melted, and standing for 10min under the condition of heat preservation. Adding Al-50Cu intermediate alloy and Al-10Mg intermediate alloy into the melt, stirring for 2min after the alloy is completely melted, and standing for 10min under the condition of heat preservation to obtain the melt with uniform components.
(2) Modification and refining
Adding Ni-18P intermediate alloy into the melt in the step (1), stirring for 2min after the melt is completely melted, and standing for 20min under the condition of heat preservation. Adding a refining agent and a deslagging agent by using a nitrogen blowing method, wherein the commercial brands of the refining agent and the deslagging agent are YT-J-1 and YT-D-4 respectively, and the refining agent and the deslagging agent are added according to the proportion of 1:1, mixing materials, then uniformly mixing, wherein the total addition amount is 1 percent of the weight of the melt, and removing scum on the surface of the melt after stirring for 1-2 min.
(3) Sub-rapid solidification and heat treatment
And (3) starting a cooling water system in the water-cooled copper mold, and quickly pouring the melt in the step (2) into the water-cooled copper mold with the thickness of 100mm multiplied by 45mm multiplied by 15mm to obtain a hypereutectic Al-Si-Ni alloy casting. The Al-22Si-18Ni-3Cu-0.8Mg alloy casting is subjected to solution treatment (530 ℃ for 8h + water quenching), and then is aged (210 ℃ for 12 h).
The alloy of the embodiment is subjected to structure observation and phase analysis, the structure appearance of the aging Al-22Si-18Ni-3Cu-0.8Mg alloy is similar to that of the embodiment 1, and the alloy mainly comprises an alpha-Al matrix and Al 3 Ni phase, si phase and net Al-Ni-Cu ternary phase. Compared with the comparative example, the structure is obviously refined, the primary Si phase is irregular small block, and Al 3 The Ni phase is thick and long. This is due to sub-rapid solidification and P deteriorationThe primary Si phase is treated and refined, the casting performance of the alloy is improved, and compared with a comparative example, the density of the component casting is higher and the casting quality is better. The alloy has a melting point of 820 ℃, a thermal conductivity of 102.52W/(m.K) at 25 ℃ and an average linear expansion coefficient of 11.28 multiplied by 10 at 25-100 ℃ according to tests -6 The hardness is 248HV.
Therefore, the components of the embodiment have lower thermal expansion coefficient, lower melting point and better casting performance, are suitable for a smelting casting process, are matched with a sub-rapid solidification and heat treatment process and modification treatment, have obviously refined alloy tissues, obtain better heat-conducting performance and meet the thermal performance requirement of the aluminum-based alloy for electronic packaging.
Example 5: al-24Si-16Ni-2Cu-1Mg alloy
The preparation process of the embodiment is basically consistent with that of the embodiment 1, and only differences exist in smelting temperature and heat treatment process parameters.
The alloy prepared in the embodiment comprises Al-24Si-16Ni-2Cu-1Mg, and is prepared from the following raw materials in percentage by mass: 25% of Si, 15% of Ni, cu:3%, mg:0.5%, P:0.3 percent and the balance of Al.
The preparation method comprises the following specific steps:
(1) Alloy smelting:
melting weighed industrial pure aluminum, al-50Si intermediate alloy and pure Ni at 890 ℃, stirring for 2min after all melting, and standing for 10min under heat preservation. Adding Al-50Cu intermediate alloy and Al-10Mg intermediate alloy into the melt, stirring for 2min after the alloy is completely melted, and standing for 10min under the condition of heat preservation to obtain the melt with uniform components.
(2) Modification and refining
Adding Ni-18P intermediate alloy into the melt in the step (1), stirring for 2min after the melt is completely melted, and standing for 20min under the condition of heat preservation. Adding a refining agent and a deslagging agent by using a nitrogen blowing method, wherein the commercial brands of the refining agent and the deslagging agent are YT-J-1 and YT-D-4 respectively, and the refining agent and the deslagging agent are added according to the proportion of 1:1, mixing materials, then uniformly mixing, wherein the total addition amount is 1 percent of the weight of the melt, and removing scum on the surface of the melt after stirring for 1-2 min.
(3) Sub-rapid solidification and heat treatment
And (3) starting a cooling water system in the water-cooled copper mold, and quickly pouring the melt in the step (2) into the water-cooled copper mold with the thickness of 100mm multiplied by 45mm multiplied by 15mm to obtain a hypereutectic Al-Si-Ni alloy casting. The Al-24Si-16Ni-2Cu-1Mg alloy casting is subjected to solution treatment (520 ℃ multiplied by 8h + water quenching), and then is aged (230 ℃ multiplied by 8 h).
The alloy of the embodiment is subjected to structure observation and phase analysis, the structure appearance of the aging Al-24Si-16Ni-2Cu-1Mg alloy is similar to that of the embodiment 1, and the alloy mainly comprises an alpha-Al matrix and Al 3 Ni phase, and Si phase and a small amount of strip Al 3 Ni 2 The phase and the Al-Ni-Cu ternary phase, and a small amount of the Al-Cu-Ni ternary phase is coated on Al 3 The Ni phase is in the middle. Compared with the comparative example, the structure is obviously refined, the primary Si phase is irregular small block, and Al 3 The Ni phase is thick and long. The primary Si phase is refined through sub-rapid solidification and P modification treatment, the casting performance of the alloy is improved, and compared with a comparative example, the density of the component casting is higher and the casting quality is better. The alloy has a melting point of 830 ℃, a thermal conductivity of 110.88W/(m.K) at 25 ℃ and an average linear expansion coefficient of 11.05X 10 at 25-100 DEG C -6 and/K, hardness 220HV.
Therefore, the components of the embodiment have lower thermal expansion coefficient, lower melting point and better casting performance, are suitable for a smelting casting process, are matched with a sub-rapid solidification and heat treatment process and modification treatment, have obviously refined alloy tissues, obtain better heat-conducting performance and meet the thermal performance requirement of the aluminum-based alloy for electronic packaging.
Example 6: al-26Si-14Ni-1Cu-0.5Mg alloy
The preparation process of the embodiment is basically consistent with that of the embodiment 1, and only differences exist in smelting temperature and heat treatment process parameters.
The alloy prepared by the embodiment comprises Al-26Si-14Ni-1Cu-0.5Mg, and is prepared from the following raw materials in percentage by mass: 25% of Si, 15% of Ni, cu:3%, mg:0.5%, P:0.3 percent and the balance of Al.
The preparation method comprises the following specific steps:
(1) Alloy smelting:
melting weighed industrial pure aluminum, al-50Si intermediate alloy and pure Ni at 915 ℃, stirring for 2min after all the materials are melted, and standing for 10min under the condition of heat preservation. Adding Al-50Cu intermediate alloy and Al-10Mg intermediate alloy into the melt, stirring for 2min after the alloy is completely melted, and standing for 10min while keeping the temperature to obtain the melt with uniform components.
(2) Modification and refining
Adding Ni-18P intermediate alloy into the melt in the step (1), stirring for 2min after the melt is completely melted, and standing for 20min under the condition of heat preservation. Adding a refining agent and a deslagging agent by using a nitrogen blowing method, wherein the commercial brands of the refining agent and the deslagging agent are YT-J-1 and YT-D-4 respectively, and the refining agent and the deslagging agent are added according to the proportion of 1:1, mixing materials, then uniformly mixing, wherein the total addition amount is 1 percent of the weight of the melt, and removing scum on the surface of the melt after stirring for 1-2 min.
(3) Sub-rapid solidification and heat treatment
And (3) starting a cooling water system in the water-cooled copper mold, and quickly pouring the melt in the step (2) into the water-cooled copper mold with the thickness of 100mm multiplied by 45mm multiplied by 15mm to obtain a hypereutectic Al-Si-Ni alloy casting. The alloy casting is subjected to solution treatment (510 ℃ for multiplied by 8h + water quenching), and then aging (230 ℃ for multiplied by 12 h).
The alloy of the embodiment is subjected to structure observation and phase analysis, the structure appearance of the aging Al-26Si-14Ni-1Cu-0.5Mg alloy is similar to that of the embodiment 1, and the aging Al-26Si-14Ni-1Cu-0.5Mg alloy mainly comprises an alpha-Al matrix, an Al3Ni phase, an Si phase and a small amount of strip Al 3 Ni 2 The phase and the Al-Ni-Cu ternary phase, and a small amount of the Al-Cu-Ni ternary phase is coated on Al 3 The Ni phase is in the middle. Compared with the comparative example, the structure is obviously refined, the primary Si phase is irregular small block, and Al 3 The Ni phase is thick and long. The primary Si phase is refined through sub-rapid solidification and P modification treatment, the casting performance of the alloy is improved, and compared with a comparative example, the density of the component casting is higher and the casting quality is better. The alloy has the melting point of 855 ℃, the thermal conductivity of 112.5W/(m.K) at 25 ℃ and the average linear expansion coefficient of 10.85 multiplied by 10 at 25-100 ℃ through tests -6 The hardness is 203HV.
Therefore, the components of the embodiment have lower thermal expansion coefficient, lower melting point and better casting performance, are suitable for a smelting casting process, are matched with a sub-rapid solidification and heat treatment process and modification treatment, have obviously refined alloy tissues, obtain better heat-conducting performance and meet the thermal performance requirement of the aluminum-based alloy for electronic packaging.
The properties of the alloys of comparative example 1 and examples 1 to 6 are shown in Table 1.
TABLE 1 Properties of alloys of comparative example 1 and examples
Comparative example 2: common solidification casting forming of Al-20Si-20Ni alloy
The comparative example adopts industrial pure aluminum, al-50Si intermediate alloy and high-purity Ni as raw materials, and the components are in mass percent: 20% of Si, 20% of Ni and the balance of Al.
The die adopts a No. 45 steel sheet die with the thickness of 100mm multiplied by 45mm multiplied by 15mm, and the preparation process and the parameters thereof are as follows:
(1) Alloy smelting: melting the weighed Al-50Si alloy at 870 ℃. Stirring for 2min after the materials are completely melted to make the components uniform, and standing for 10min under the condition of heat preservation.
(2) Casting and forming: adding a refining agent and a slag removing agent, stirring for 1-2 min, removing floating slag on the surface of the melt, and casting into a mold.
The Al-20Si-20Ni alloy structure consists of Si phase, al 3 Ni phase and alpha-Al phase. The Al-20Si-20Ni alloy formed by common casting and solidification has coarse texture, the primary Si phase is coarse block, and Al 3 The Ni phase is long dendritic. The alloy has a melting point of 810 ℃, a thermal conductivity of 72.82W/(m.K) at 25 ℃ and an average linear expansion coefficient of 10.78 multiplied by 10 at 25-100 DEG C -6 The hardness is 145HV. Al-20S prepared by common solidification processThe performance of the i-20Ni alloy cannot meet the performance requirements of electronic packaging materials.
FIG. 2 is an optical microstructure of the alloy of comparative example 2.
Comparative example 3: common solidification casting forming of Al-20Si-20Ni-1Cu-0.5Mg alloy
The raw materials of the comparative example are prepared from industrial pure aluminum, al-50Si intermediate alloy and high-purity Ni, and the components are in mass percent: 20% of Si, 20% of Ni, 1% of Cu, and a weight ratio of Mg:0.5 percent, and the balance of Al.
The die adopts a No. 45 steel sheet die with the thickness of 100mm multiplied by 45mm multiplied by 15mm, and the preparation process and the parameters thereof are as follows:
(1) Alloy smelting: melting weighed industrial pure aluminum, al-50Si intermediate alloy and pure Ni at 870 ℃, stirring for 2min after all the materials are melted, and standing for 10min under the condition of heat preservation; adding Al-50Cu intermediate alloy and Al-10Mg intermediate alloy into the melt, stirring for 2min after the alloy is completely melted, and standing for 10min under the condition of heat preservation to obtain the melt with uniform components.
(2) Casting and forming: adding a refining agent and a slag removing agent, stirring for 1-2 min, removing floating slag on the surface of the melt, and casting into a mold.
(3) And (3) heat treatment: the alloy casting is subjected to solution treatment (520 ℃ for multiplied by 6h + water quenching), and then aging (220 ℃ for multiplied by 10 h).
The Al-20Si-20Ni-1Cu-0.5Mg alloy structure consists of Si phase and Al 3 Ni phase, alpha-Al phase, al 2 Cu-bonded Mg 2 And (4) Si phase composition. The Al-20Si-20Ni alloy formed by common casting and solidification has coarse texture, the primary Si phase is coarse block, and Al 3 The Ni phase is long dendritic. After solid solution and aging, fine Al is dispersed and precipitated in the alpha-Al matrix 2 Cu phase and Mg 2 A Si phase. The alloy has a melting point of 810 ℃, a thermal conductivity of 78.5W/(m.K) at 25 ℃ and an average linear expansion coefficient of 10.62 multiplied by 10 at 25-100 DEG C -6 The hardness is 165HV. The performance of the Al-20Si-20Ni-1Cu-0.5Mg alloy prepared by the common solidification process cannot meet the performance requirement of the electronic packaging material.
Comparative example 4: common solidification casting forming of Al-20Si-20Ni-1Cu-0.5Mg-0.3P alloy
The alloy components of the comparative example are Al-20Si-20Ni-1Cu-0.5Mg-0.3P, the raw materials are prepared from industrial pure aluminum, al-50Si intermediate alloy, high-purity Ni, al-50Cu intermediate alloy and Al-10Mg intermediate alloy, and the components are in mass percentage: 20% of Si, 20% of Ni, cu:1%, mg:0.5%, P:0.3 percent and the balance of Al.
The method comprises the following specific steps:
(1) Alloy smelting:
melting weighed industrial pure aluminum, al-50Si intermediate alloy and pure Ni at 870 ℃, stirring for 2min after all the materials are melted, and standing for 10min under the condition of heat preservation; adding Al-50Cu intermediate alloy and Al-10Mg intermediate alloy into the melt, stirring for 2min after the alloy is completely melted, and standing for 10min while keeping the temperature to obtain the melt with uniform components.
(2) Modification and refining
Adding Ni-18P intermediate alloy into the melt in the step (1), stirring for 2min after the melt is completely melted, and standing for 20min under the condition of heat preservation; adding a refining agent and a slag removing agent, stirring for 1-2 min, removing floating slag on the surface of the melt, and casting into a mold.
(3) And (3) heat treatment: the alloy casting is subjected to solution treatment (520 ℃ multiplied by 6h + water quenching) and then aged (220 ℃ multiplied by 10 h).
The Al-20Si-20Ni-1Cu-0.5Mg alloy structure consists of Si phase, al 3 Ni phase, alpha-Al phase, al 2 Cu-bonded Mg 2 The Si phase. The Si phase of the Al-20Si-20Ni-1Cu-0.5Mg alloy after P modification is obviously refined. After solid solution and aging, al is dispersed and precipitated in the alpha-Al matrix 2 Cu phase and Mg 2 A Si phase. The alloy has a melting point of 810 ℃, a thermal conductivity of 85W/(m.K) at 25 ℃ and an average linear expansion coefficient of 10.52 multiplied by 10 at 25-100 DEG C -6 The hardness is 178HV. The performance of the Al-20Si-20Ni-1Cu-0.5Mg-0.3P alloy prepared by the common solidification process is improved to a certain extent but can not meet the performance requirement of the electronic packaging material.
All embodiments of the invention have the characteristics of high heat conduction and low expansion, and the alloy system has good casting performance, lower melting point and higher hardness, the preparation process cost is low, the process is simple, and the performance requirements of the existing electronic packaging material are met. Among them, the embodiment with higher Cu and Mg contents can obtain higher hardness, and the embodiment with higher Si content can obtain lower thermal expansion and higher thermal conductivity.
The embodiments of the present invention are not limited to the embodiments described above, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and they are included in the scope of the present invention.
Claims (9)
1. A high heat conduction low expansion Al-Si-Ni based alloy is characterized in that: comprises the following components by mass percent:
Si 20～30％
Ni 10～20％
Cu 1～3％
Mg 0～1％
P 0.1～0.3％
the balance of Al;
the high-thermal-conductivity low-expansion Al-Si-Ni-based alloy is prepared by the following method:
(1) Preparing an Al-Si-Ni alloy melt:
(2) Adding micro-alloying elements Cu and Mg: adding Al-Cu and Al-Mg intermediate alloy into the Al-Si-Ni alloy melt to obtain an aluminum alloy melt;
(3) Refining and P modification treatment: adding Ni-P intermediate alloy into the aluminum alloy melt in the step (2) for modification treatment, and then carrying out refining deslagging treatment to obtain a treated aluminum alloy melt;
(4) And (3) sub-rapid solidification: cooling the mold with water, and adding the aluminum alloy melt treated in the step (3) into the cooled mold to obtain a hypereutectic Al-Si-Ni alloy casting;
(5) And (3) heat treatment: and carrying out solid solution treatment and aging treatment on the hypereutectic Al-Si-Ni alloy casting to obtain the high-heat-conductivity low-expansion Al-Si-Ni-based alloy.
2. The high thermal conductivity low expansion Al-Si-Ni based alloy according to claim 1, characterized in that: comprises the following components by mass percent:
Si 25～30％
Ni 10～15％
Cu 1～3％
Mg 0.1～1％
P 0.1～0.3％
the balance being Al.
3. The method for producing a high thermal conductivity low expansion Al-Si-Ni based alloy according to claim 1 or 2, characterized in that: the method comprises the following steps:
(1) Preparing an Al-Si-Ni alloy melt: melting pure aluminum, al-Si intermediate alloy and pure Ni, stirring, standing and preserving heat to obtain Al-Si-Ni alloy melt;
(2) Adding micro-alloying elements Cu and Mg: adding an Al-Cu and Al-Mg intermediate alloy into the Al-Si-Ni alloy melt, melting, stirring, standing and preserving heat to obtain an aluminum alloy melt;
(3) Refining and P modification treatment: adding Ni-P intermediate alloy into the aluminum alloy melt in the step (2), melting, stirring, standing and preserving heat to obtain an aluminum alloy melt subjected to modification treatment; refining and deslagging the alloy melt subjected to the modification treatment to obtain a treated aluminum alloy melt;
(4) And (3) sub-rapid solidification: cooling the mold with water, and adding the aluminum alloy melt treated in the step (3) into the cooled mold to obtain a hypereutectic Al-Si-Ni alloy casting;
(5) And (3) heat treatment: the casting of the hypereutectic Al-Si-Ni alloy is subjected to heat preservation treatment for 6 to 8 hours at the temperature of between 510 and 530 ℃, water quenching and aging treatment for 8 to 12 hours at the temperature of between 210 and 230 ℃ to obtain the high-heat-conductivity low-expansion Al-Si-Ni-based alloy.
4. The method for producing a high thermal conductivity low expansion Al-Si-Ni based alloy according to claim 3, characterized in that:
the melting temperature in the step (1) is 850-950 ℃; stirring for 1-2 min, and standing for 8-12 min;
the melting temperature in the step (2) is 850-950 ℃; stirring for 1-2 min, and standing for 8-12 min;
and (5) in the step (4), the mold is cooled by water all the time in the process of adding the aluminum alloy melt treated in the step (3) into the cooled mold.
5. The method for producing a high thermal conductivity low expansion Al-Si-Ni based alloy according to claim 3, characterized in that:
the Al-Si intermediate alloy is Al-50Si intermediate alloy;
the Al-Cu intermediate alloy is Al-50Cu intermediate alloy; the Al-Mg intermediate alloy is Al-10Mg intermediate alloy;
the Ni-P intermediate alloy is Ni-18P intermediate alloy;
the melting temperature in the step (3) is 850-950 ℃; the stirring time is 1-2 min, and the standing and heat preservation time is 10-25 min.
6. The method for producing a high thermal conductivity low expansion Al-Si-Ni based alloy according to claim 3, characterized in that: the die in the step (4) is a copper die; and starting a cooling water circulation system in the water-cooled copper mold, and quickly casting the melt into the water-cooled copper mold.
7. The method for producing a high thermal conductivity low expansion Al-Si-Ni based alloy according to claim 3, characterized in that:
removing scum on the surface of the Al-Si-Ni alloy melt before adding the Al-Cu and Al-Mg intermediate alloy into the Al-Si-Ni alloy melt in the step (2);
and (4) refining and deslagging in the step (3) by using a nitrogen blowing method and adding a refining agent and a deslagging agent.
8. The method for producing a high thermal conductivity low expansion Al-Si-Ni based alloy according to claim 7, characterized in that: the commercial brands of the refining agent and the deslagging agent are YT-J-1 and YT-D-4 respectively, and the refining agent and the deslagging agent are prepared according to the proportion of 1:1, mixing, and then uniformly mixing, wherein the total addition amount is 1 percent of the weight of the melt.
9. Use of the high thermal conductivity low expansion Al-Si-Ni based alloy according to claim 1 or 2, characterized in that: the high-thermal-conductivity low-expansion Al-Si-Ni-based alloy is used for electronic packaging materials.
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