CN112453422B - Light Al-Si-Mg2Si electronic packaging material and preparation method and application thereof - Google Patents

Light Al-Si-Mg2Si electronic packaging material and preparation method and application thereof Download PDF

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CN112453422B
CN112453422B CN202011161484.XA CN202011161484A CN112453422B CN 112453422 B CN112453422 B CN 112453422B CN 202011161484 A CN202011161484 A CN 202011161484A CN 112453422 B CN112453422 B CN 112453422B
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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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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/115—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by spraying molten metal, i.e. spray sintering, spray casting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B22F3/15—Hot isostatic pressing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00—Products made by additive manufacturing
    • 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
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0078—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only silicides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
    • H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment

Abstract

The invention relates to light Al-Si-Mg2The Si electronic packaging material and the preparation method thereof and the application thereof in the field of electronic packaging, wherein the preparation method comprises the following steps: s1: alloy composition design, including Si and Mg2Si phase content and proportion thereof; s2: spraying, depositing and blank making; s3: thermal analysis and thermal stability analysis; s4: hot isostatic compaction and heat treatment; s5: microscopic structure and performance investigation; s6: and (5) processing and checking the shell. Compared with the existing material, Al-Si-Mg2The Si alloy has lower density and higher elastic modulus; compared with the prior art, the method for spray deposition and hot isostatic pressing can effectively control Mg2The size and the shape of Si and Si phase can obtain large-size ingot blank and ensure the good comprehensive performance and the process stability of the alloy. After examination and verification, Al-Si-Mg is sprayed and deposited2The Si alloy is suitable for the field of electronic packaging, and can also be applied to lightweight components such as pistons, brake discs, engine cylinder sleeves and the like.

Description

Light Al-Si-Mg2Si electronic packaging material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of development and preparation of metals and alloys, and particularly relates to light Al-Si-Mg2Si electronic packaging material and a preparation method thereof, and is applied to the field of electronic packaging.
Background
The Metal Matrix Composites (MMCs) have the characteristics of high toughness, high plasticity, good processability of a Metal Matrix, high hardness of a reinforcing phase, excellent wear resistance, heat resistance and the like, can obtain materials with different properties by adjusting the volume fraction of the reinforcing phase, and show good designability. With the rapid development of electronic information, rail transit and automobile industries and the increasingly prominent problems of energy shortage, environmental pollution and the like, the light aluminum-based composite material is receiving more and more attention from the material industry and the industrial industry and is gradually applied to the fields of aerospace, vehicles, sports and the like.
Compared with the traditional external method (Ex-situ), the In-situ self-generation method (In-situ) is a new preparation technology of metal matrix composite materials developed In recent years, and the principle is that one or more reinforcing phases with high hardness and high elastic modulus are generated In situ In a metal matrix through chemical reaction between elements or element compounds under certain conditions, so that the purpose of reinforcing the matrix is achieved. Because the enhanced phase is generated in situ in the matrix in the in-situ authigenic method, the surface is free of pollution, the problem of compatibility with the matrix is avoided, the interface bonding strength is high, and the stable thermodynamic property is realized; meanwhile, the in-situ autogenesis method reduces the procedures of independent synthesis and treatment of particles, addition, mixing and the like in an external addition method, and has simple preparation process and low cost.
High silicon aluminum alloys, also known as Al/Sip composites, generally refer to aluminum silicon alloys having Si contents exceeding the eutectic composition (12 wt.%). A raw material Si block is added into an Al melt, and after smelting and casting, a Si particle reinforced phase is formed in situ in an Al matrix. High silicon aluminum alloys, particularly materials with Si contents up to and exceeding 50 wt.%, have good mechanical and thermophysical properties, are capable of being machined to obtain components of desired shape and size, and have good surface plating and laser welding properties, and have been used in bulk in the field of electronic packaging.
Intermetallic compound Mg2Si has a low density (1.99 g/cm)3) High melting point, high hardness, high elastic modulus, low thermal expansion coefficient and good thermoelectric property, and is very suitable for serving as a reinforcing phase of the aluminum alloy for electronic packaging. Chinese patent CN1215089A discloses an in-situ authigenic Mg2Si particle reinforced aluminum matrix composite material, Chinese patent CN104131190B discloses an in-situ self-generated high volume fraction Mg2Si-reinforced Mg-Al based composite material. However, it is difficult to obtain Al-Mg with high performance due to the small cooling rate of the conventional casting method2An Si alloy.
Based on high-silicon aluminium alloys and intermetallic compounds Mg2The characteristics of Si, the development of light Al-Si-Mg2The Si alloy not only can further reduce the density, but also is expected to improve the mechanical property of the material. But currently the light weight of Al-Si-Mg is limited2The key of popularization and application of the Si alloy lies in primary Mg2The sizes of Si intermetallic compounds and Si phases are large, and edges and corners are sharp, so that the matrix is cut, and the mechanical property and the processability of the material are reduced. Modification of Mg2The shape, size and distribution of Si and Si phases, and the control of the solidification, processing and forming processes of the alloy are the main difficulties for improving the obdurability of the alloy.
Disclosure of Invention
In order to further reduce the density of the high-silicon aluminum alloy and improve the mechanical property of the high-silicon aluminum alloy, the invention provides light Al-Si-Mg2Si electronic packaging material and a preparation method thereof; to overcome Al-Si-Mg2The invention adopts a rapid solidification jet deposition preparation technology and combines thermal analysis and thermal stability analysis to formulate a reasonable densification and heat treatment process; optimizing alloy components through microscopic structure and performance analysis; further, Al-Si-Mg2The Si alloy is used as an electronic packaging cover plate and a shell for examination and verification, thereby being popularized for the materialThe application lays a technical foundation.
The technical scheme adopted by the invention is as follows:
the invention relates to light Al-Si-Mg2The preparation method of the Si electronic packaging material comprises the following steps:
s1: designing alloy components: presetting Si phase and Mg according to the performance requirement of the finished product2The composition of the Si phase, wherein the finished product properties comprise strength, thermal expansion coefficient and thermal conductivity;
s2: spray deposition blank making: according to the alloy components designed in the step S1, pure aluminum, pure silicon and Al-Mg are mixed2Si intermediate alloy, smelting, and spray deposition to obtain Al-Si-Mg2A Si alloy ingot blank; the Al-Mg2In the Si master alloy, Mg2The volume fraction of Si is 50%;
s3: thermal analysis and thermal stability analysis: Al-Si-Mg is obtained by adopting a differential thermal analysis method2The phase transition temperature point of the Si alloy ingot blank, and based on the phase transition temperature point, a series of heating programs are designed, and Al-Si-Mg is heated2Heating Si alloy ingot blank samples under different heating procedures to obtain a series of blank samples, observing microstructures, and establishing Si phase and Mg in the alloy at different heating temperatures2Thermal analysis data of correlation between the coarsening rate of the Si phase and the heat preservation time;
s4: hot isostatic compaction and heat treatment: subjecting the Al-Si-Mg obtained in step S2 to hot isostatic pressing2The Si alloy ingot blank is densified to obtain the hot isostatic pressing alloy, the heating temperature and the holding time of the hot isostatic pressing are selected from the thermal analysis data in the step S3, and Si phase and Mg in the alloy2The sizes of Si phases are all less than or equal to the corresponding ranges of 30 mu m; then annealing the hot isostatic pressing alloy to obtain Al-Si-Mg2A Si alloy;
s5: microscopic structure and performance analysis: testing of Al-Si-Mg2The macroscopic performance of the Si alloy is observed, the microscopic structure and the structure are observed, the relation between the microscopic structure and the macroscopic performance of the alloy is established, if the macroscopic performance meets the requirement, the step S6 is carried out, if the macroscopic performance does not meet the requirement, the alloy is optimized according to the relation between the microscopic structure and the macroscopic performance of the alloyComponent (C), repeating the steps S2-S5;
s6: and (3) checking and verifying the shell: will satisfy macroscopic properties of Al-Si-Mg2And processing the Si alloy into an electronic packaging shell and/or a cover plate for detection.
Further, in the step S1, Si phase and Mg are preset2The specific steps of the composition of the Si phase are as follows:
step a
According to the requirements of the electronic packaging material on the thermal expansion coefficient and the thermal conductivity, the thermal expansion coefficient is firstly calculated by a mixing rule: formula (1), and thermal conductivity formula (2), the Si phase content is preset,
α＝αAl·VAl+αSi·VSi (1)
λ＝λAl·VAl+λSi·VSi (2)
wherein α represents a thermal expansion coefficient, λ represents a thermal conductivity, and V represents a volume fraction;
step b
Then, part of Mg is used2The Si phase is replaced by the Si phase, and the thermal expansion coefficient formula (3) and the thermal conductivity formula (4) are calculated by a mixing rule after the replacement, so that the requirements of the thermal expansion coefficient and the thermal conductivity of the electronic packaging material are met,
Figure BDA0002744449060000032
Figure BDA0002744449060000031
in the practical operation process, according to the requirement of the electronic packaging material on the thermal expansion coefficient matching, the thermal expansion coefficient is 20-200 ℃, and the requirement of the cover plate material is less than 18.0 +/-1.0 multiplied by 10-6The shell material is required to be less than 12.0 +/-1.0 multiplied by 10-6And the thermal conductivity is respectively higher than 150W/mK and 120W/mK. The thermal expansion coefficient and the thermal conductivity are main performance indexes of the electronic packaging material, mainly depend on the type and the content of the reinforcing phase and are less influenced by the process and parameters. Therefore, firstBased on elementary Al, Si and Mg2Basic physical property data of Si, a thermal expansion coefficient (formula 1) and a thermal conductivity (formula 2) are calculated by using a mixing rule to preset Si phase content, and then, part of Mg is adopted2The Si phase is replaced by the Si phase, and the Mg is properly increased under the condition of meeting the requirements of thermal expansion coefficient and thermal conductivity2The Si phase content thus reduces the alloy density and increases the strength.
Further, the Al-Mg2The preparation process of the Si intermediate alloy comprises the following steps: the method comprises the steps of proportioning pure aluminum, pure magnesium and Al-70Si intermediate alloy, melting the pure aluminum and the intermediate alloy, cooling to 1000-1050 ℃, adding the pure magnesium, carrying out in-situ reaction, and generating Mg in the melt2Si, cooling and solidifying after stirring to obtain Al-Mg2A Si master alloy. After the temperature is reduced, pure magnesium is added, so that the burning loss of magnesium can be reduced.
The inventors found that by adding Al-Mg2The Si intermediate alloy can improve the controllability and stability of alloy components. While Al-Mg is added2Mg in Si master alloy2The Si content is set to 50%, the best regulation effect can be achieved, and if Mg is used2If the Si content is set to be too high, Al-Mg will be introduced2Mg having an Si alloy with a melting point too high and too low2The Si content is not favorable for the adjustment of alloy components.
Further, in step S2, the main process parameters of the jet deposition are: the rotating speed of the deposition disc is 300-500r/min, the descending speed of the deposition disc is 10-15mm/min, the diameter of the nozzle is 2.8-3.5mm, the deposition distance is 260-320mm, and the atomization pressure is 0.8-1.2 MPa.
Further, in the step S2, Al-Si-Mg2The density of the Si alloy ingot blank is more than or equal to 85 percent. Control of Al-Si-Mg2The density of the Si alloy ingot blank is not lower than 85%, and the adverse effect on the densification process can be avoided.
Further, in the step S3, Al-Si-Mg is obtained by adopting a differential thermal analysis method2Setting different heating temperatures at intervals of 20 ℃ for the phase transition temperature points of the Si alloy ingot blank, setting 6 temperature points at the temperature of 5-15 ℃ lower than the eutectic reaction temperature point, keeping the temperature for 30-360 min, and setting an interval every 30min(ii) a Combining metallographic structure observation and image analysis software to obtain Si phase and Mg phase in the alloy at different heating temperatures2The relationship curve of Si phase size and holding time.
Further, in the step S4, the hot isostatic pressing pressure is 120-150 MPa.
In the present invention, the hot isostatic pressing temperature and holding time are selected in accordance with the Si phase and Mg in step S32The relationship between the size of the Si phase and the heating temperature and holding time is selected because Al-Si-Mg is contained at a constant content of the reinforcing phase2The macroscopic properties of Si alloys are mainly determined by the Si phase and Mg2Si phase size. Therefore, in the actual selection process, the Si phase and Mg are ensured2The temperature is as high as possible without excessive coarsening of the Si phase to facilitate densification of the deposited ingot, with excessive coarsening being defined as when Al-Si-Mg2When the Si electronic packaging material is applied to a shell, Si phase and Mg2The size of Si phase is less than or equal to 30 mu m, and when Al-Si-Mg2When the Si electronic packaging material is applied as a cover plate, Si phase and Mg2The sizes of Si phases are less than or equal to 15 mu m.
Further, in the step S4, Al-Si-Mg2The annealing temperature of the Si alloy is 280-360 ℃, the heat preservation time is 24-96 h, and the temperature is reduced along with the furnace after the heat preservation is finished. The internal stress of the alloy is eliminated or reduced by annealing treatment. The low-temperature long-time annealing is mainly used for eliminating or reducing the internal stress of the alloy due to Si phase and Mg2The Si phase and the Al matrix have large difference of thermal expansion coefficients and belong to brittle phases, so low-temperature annealing is selected to reduce thermal stress.
In the present invention, the macroscopic properties described in step S5 include mechanical properties including tensile strength, yield strength, elongation, bending strength and hardness, and physical properties including density, thermal conductivity and thermal expansion coefficient.
Further, in the step S5, the chemical composition of the alloy is checked according to the method specified in GB/T20975; the density of the alloy is measured according to the method specified in GB 3850 or GB/T1423, and the specification of a sample piece is as follows: 20 multiplied by 10mm, and the density is the ratio of the measured density to the theoretical density multiplied by 100 percent; measuring the tensile strength of the alloy according to a method specified in GB/T228; measuring the specific heat capacity of the alloy according to a method specified by ASTM E1269 or GJB 330A, measuring the thermal diffusivity of the alloy according to a method specified by GB/T22588 or GJB1201.1, and calculating the thermal conductivity by a classical thermal conductivity formula; the coefficient of thermal expansion of the alloy was measured according to the method specified in GB/T4339 or GJB 332A.
Further, in the step S5, optimizing the alloy composition based on the relationship between the alloy components-microstructure-macroscopic properties, wherein the macroscopic properties firstly consider the requirements of thermal expansion coefficient and thermal conductivity, and secondly comprehensively consider the mechanical property index, so as to obtain higher mechanical properties under the condition of satisfying the requirements of thermal expansion coefficient and thermal conductivity; Al-Si-Mg2The relationship between Si alloy composition-microstructure-macroscopic properties is mainly characterized by the alloy composition in the Si phase and Mg2The size and morphology of the Si phase, and thus the macroscopic properties.
Further, in the step S5, through comparative analysis of the density, mechanical properties and thermophysical properties of the alloy, optimization of alloy components including Si and Mg is performed2Si phase content, Si/Mg2The Si ratio and the matrix alloy components, wherein the matrix alloy components mainly consider the requirements of the mechanical properties of the alloy, and the alloy strength can be effectively improved through matrix alloying.
Further, in the step S6, the examination and verification contents include the machining performance, the surface plating performance, the laser welding performance of the alloy, and the process performance and the application performance such as the air tightness of the sealed and welded shell.
In the practical operation process, Al-Si-Mg is prepared2The Si alloy electronics package housing and/or cover plate is compared to the Al-Si alloy.
The invention also provides the light Al-Si-Mg prepared by the preparation method2A Si electronic packaging material.
The invention also provides the light Al-Si-Mg prepared by the preparation method2Application of Si electronic packaging material, and application of the light Al-Si-Mg2The Si electronic packaging material is applied as an electronic packaging shell material or an electronic packaging cover plate material.
Compared with the prior art, the invention has the beneficial effects that:
(1) reinforcing phase Mg2Si and Si are generated in situ in the aluminum alloy melt, the cooling solidification and the combination of the matrix are good, the problems of interface reaction, oxidation, pollution and the like are avoided, the preparation process is simplified, and the foundation is laid for the large-scale production of the material.
(2) Al-Si-Mg preparation by rapid solidification spray deposition technology2The Si alloy effectively solves the problem of Mg caused by low cooling speed in the traditional casting and metallurgy process2The Si phase and the Si phase are coarse, and the composition segregation phenomenon is avoided, so that the strength and the elastic modulus of the alloy are greatly improved.
(3) Due to Mg2The density of Si is only 1.99g/cm3Reduction of 14.6% relative to Si, Al-Si-Mg2The density of the Si alloy is further reduced, and the Si alloy is favorable for application in the field of aerospace.
(4) The invention adopts the existing spray deposition process and equipment, does not need to modify smelting and forming equipment, and has the advantages that the raw materials Al, Mg and Si are all low-cost materials, thus being extremely easy to popularize.
(5) Al-Si-Mg prepared by the invention2The Si alloy is environmentally friendly because of the reinforcing phase Mg2Si and Si can be completely dissolved in the Al matrix in the remelting process, so that the alloy can be reused only by controlling the content of the enhanced phase and the process parameters in the repeated smelting process.
Drawings
FIG. 1 shows the light weight Al-Si-Mg of the present invention2Si alloy and a preparation and application process flow thereof.
FIG. 2 shows Al-25% Si-25% Mg in example 2 of the present invention2Microstructure of Si alloy.
FIG. 3 shows Al-12% Si-15% Mg in example 1 of the present invention2An electronic package cover plate made of Si alloy;
FIG. 4 shows Al-25% Si-25% Mg in example 2 of the present invention2An electronic packaging shell made of Si alloy.
Detailed Description
For a further understanding of the invention, two specific examples are set forth belowExample, for the light Al-Si-Mg provided by the invention2The Si alloy and its preparation and use are explained in detail, and the scope of protection of the present invention is not limited by the following specific examples.
Example 1
In this example, a light Al-2% Si-25% Mg is prepared2Referring to fig. 1, a Si alloy electronic package cover plate material includes the following steps:
s1: designing alloy components: the main performance index of the electronic packaging cover plate is the thermal expansion coefficient of 18.0 +/-1.0 multiplied by 10-6The thermal conductivity is more than or equal to 150W/mK, and Al, Si and Mg are combined2The performance parameters of Si (Table 1) are that the Si content in Al-Si alloy is designed according to the formula (1) and the formula (2), and then the Al-Si-Mg alloy is designed by adopting the formula (3) and the formula (4)2Mg in Si alloy2The ratio of Si and Si phases.
First, the thermal expansion coefficient is 18.0 +/-1.0 multiplied by 10-6The requirement of/K and formula (1), provided that the Si content is x, the Al content is 1-x, i.e.
23.6·(1-x)+4.2·x＝18±1 (5)
The formula (5) can be used for obtaining the Si with the content of 23.7-34.0 percent, and the requirement of the thermal expansion coefficient can be met.
Further, according to the requirements of thermal conductivity being more than or equal to 150W/mK and the formula (2), namely
237·(1-x)+148·x≥150 (6)
The formula (6) can be used for obtaining the alloy, and the Si content is lower than 98.8 percent, so that the requirement of thermal conductivity can be met.
The Si content is selected to be 27 percent by comprehensively considering the factors of density, strength and the like.
Further using Mg2Si in place of a portion of Si according to a coefficient of thermal expansion of 18.0 + -1.0 × 10-6The requirement of/K and formula (1), provided that Mg2The Si content is x, the Si content is 0.27-x, i.e.
23.6×0.73+4.2·(0.27-x)+7.5·x＝18±1 (7)
Obtainable from formula (7), Mg2The Si content is 0-19.3% and can meet the requirement of thermal expansion coefficient.
Further, according to the requirements of thermal conductivity being more than or equal to 150W/mK and the formula (2), namely
237×0.73+148·(0.27-x)+8·x≥150 (8)
Obtainable from formula (8), Mg2The Si content of less than 45.0 percent can meet the requirement of heat conductivity, namely Mg can be used2Si is completely substituted for Si.
Due to the adoption of Mg2Si is completely substituted for Si to easily generate excessive Mg in the alloy, and the solid solubility of Mg in an Al matrix is higher, so that the heat conductivity of the alloy is not facilitated, and therefore, the selected alloy components are Al-2% Si-25% Mg2Si。
S2: spray deposition blank making: according to the designed alloy composition of the step S1, pure aluminum and Al-Mg are blended2And smelting the Si intermediate alloy, and then carrying out spray deposition to obtain a deposited ingot blank.
Firstly, preparing materials by adopting pure aluminum, pure magnesium and Al-70% Si intermediate alloy, after the pure aluminum and the intermediate alloy are melted, cooling to 1000-1050 ℃ to reduce the burning loss of Mg, pressing a pure magnesium block into the bottom of a melt by adopting a graphite rod, and then carrying out in-situ reaction for 10-20 min under stirring; cooling to 1000-1050 ℃, casting by adopting a water-cooling mold, and cooling to obtain Al-50% Mg2A Si master alloy.
Further, pure aluminum, pure silicon and Al-50% Mg are used2The Si intermediate alloy is proportioned, melted and atomized under high pressure and deposited to obtain a spray deposition ingot blank, and the main technological parameters of spray deposition comprise: the rotating speed of the deposition disc is 300-400r/min, the descending speed of the deposition disc is 10-12mm/min, the diameter of the nozzle is 2.8mm, the deposition distance is 260-280mm, and the atomization pressure is 0.8-1.0 MPa.
Further, the spray deposition of Al-2% Si-25% Mg is obtained by adopting the process2The average density of the Si alloy ingot blank is 92% +/-3%.
S3: thermal analysis and thermal stability analysis: obtaining a phase transition temperature point of a deposition ingot blank by adopting a differential thermal analysis method, designing a series of heating and heat-preserving procedures based on the phase transition temperature point, obtaining a series of blank samples by heating the deposition ingot blank samples under different heating procedures, observing microstructures, and establishing Si phase and Mg phase in alloy2Correlation of the Si phase coarsening rate with the heating temperature and the holding time.
Because no other alloy is added into the alloyGold element, spray-deposited Al-2% Si-25% Mg2The phase transition points of the Si alloy correspond to Mg respectively2Exothermic peak of Si precipitation 636.3 ℃, (Al + Mg)2Si) binary eutectic reaction exothermic peak 585.5 ℃ and (Al + Mg)2Si + Si) ternary eutectic reaction exothermic peak 554.8 ℃, so 530 ℃, 510 ℃, 490 ℃, 470 ℃, 450 ℃ and 430 ℃ are selected for heating and heat preservation, the heat preservation time is 30-360 min, and every 30min is a gradient.
Further, observing the evolution of microstructures at different heating temperatures and different heat preservation times, and drawing Si phase and Mg phase in the alloy by combining with image analysis software2The relationship curve of the coarsening rate of the Si phase and the heating temperature and the holding time shows that Mg2The coarsening of Si and Si phases is obvious after heating and heat preservation at 530 ℃ for +30min and 510 ℃ for +360min, and Mg is obvious at other heating temperatures and heat preservation time2The Si and Si phases are less than 15 μm in size.
S4: hot isostatic compaction and heat treatment: the spray deposition ingot blank is densified by hot isostatic pressing, proper hot isostatic pressing heating temperature and heat preservation time are selected based on the result of the step S3, the hot isostatic pressing pressure is 120-150MPa, and the hot isostatic pressing alloy is subjected to low-temperature long-time stabilization annealing to obtain Al-2% Si-25% Mg2An Si alloy.
According to the heating temperature and the holding time in the step S3, the Si phase and Mg2According to the relation of Si phase size, the hot isostatic pressing heating temperature is 510 ℃, and the heat preservation time is 240 min.
Further, Al-2% Si-25% Mg after hot isostatic pressing2The density of the Si alloy is more than 99 percent.
Further, to eliminate or reduce the internal stress of the alloy, Si phase and Mg are taken into consideration2The Si phase and the Al matrix have large difference of thermal expansion coefficients and belong to brittle phases, Al-2% Si-25% Mg2The stabilizing annealing process of the Si alloy is 280 ℃ plus 96 hours, and the temperature is reduced along with the furnace after the heat preservation is finished.
S5: microscopic structure and performance analysis: testing of Al-2% Si-25% Mg2Mechanical properties and physical properties of the Si alloy, observing a microstructure and a structure, and establishing a relation between the microstructure and the macroscopic properties of the alloy; according to macroscopic performance requirementsParticularly the thermal expansion coefficient and the structural property, and then repeating the steps S2-S5 to obtain the alloy meeting the performance requirements.
Spray deposition of Al-2% Si-25% Mg2The microstructure characterization of the Si alloy comprises metallographic phase, a scanning electron microscope and the like, the mechanical properties comprise tensile strength, yield strength, elongation, bending strength and hardness, and the physical properties comprise density, thermal conductivity and thermal expansion coefficient.
Further, the chemical composition of the alloy is checked according to the method specified in GB/T20975; the density of the alloy is measured according to the method specified in GB 3850 or GB/T1423, and the specification of a sample piece is as follows: 20 multiplied by 10mm, and the density is the ratio of the measured density to the theoretical density multiplied by 100 percent; measuring the tensile strength of the alloy according to a method specified in GB/T228; measuring the specific heat capacity of the alloy according to a method specified by ASTM E1269 or GJB 330A, measuring the thermal diffusivity of the alloy according to a method specified by GB/T22588 or GJB1201.1, and calculating the thermal conductivity by a classical thermal conductivity formula; the coefficient of thermal expansion of the alloy was measured according to the method specified in GB/T4339 or GJB 332A.
Further, the test results showed that Al-2% Si-25% Mg2The thermal expansion coefficient of Si alloy is 18.6X 10-6The thermal conductivity is 165W/mK, and the requirements of a typical electronic packaging cover plate on the thermal expansion coefficient and the thermal conductivity can be met.
Further, Al-2% Si-25% Mg2The density of the Si alloy was 2.51g/cm3The reduction is 3.1 percent relative to Al-27 percent Si alloy; the tensile strength is 185MPa, which is improved by 15.6 percent compared with Al-27 percent Si alloy.
S6: and (3) checking and verifying the shell: al-2% Si-25% Mg2The Si alloy is prepared by spray deposition, is processed into an electronic packaging cover plate (shown in figure 3) after being compacted by hot isostatic pressing and heat treatment, is examined and verified, and is compared with the spray deposition Al-27% Si alloy for analysis.
The examination and verification contents comprise the machining performance, the laser welding performance, the air tightness of the seal welding shell and other process performances and application performances of the alloy.
Further, the examination results show that Al-2% Si-25% Mg2The Si alloy has packaging process performance similar to that of Al-27% Si alloy.
Example 2:
in this example, a light Al-25% Si-25% Mg is prepared2Referring to fig. 1, a Si alloy electronic package casing material includes the following steps:
s1: designing alloy components: the main performance index of the electronic packaging shell is the thermal expansion coefficient of 12.0 +/-1.0 multiplied by 10-6The thermal conductivity is more than or equal to 120W/mK, and Al, Si and Mg are combined2The performance parameters of Si (Table 1) are that the Si content in Al-Si alloy is designed according to the formula (1) and the formula (2), and then the Al-Si-Mg alloy is designed by adopting the formula (3) and the formula (4)2Mg in Si alloy2The ratio of Si and Si phases.
First, the thermal expansion coefficient is 12.0 +/-1.0 multiplied by 10-6The requirement of/K and formula (1), provided that the Si content is x, the Al content is 1-x, i.e.
23.6·(1-x)+4.2·x＝12±1 (9)
The formula (9) can be used, and the Si content of 54.6-64.9% can meet the requirement of thermal expansion coefficient.
Further, according to the requirements of thermal conductivity being more than or equal to 150W/mK and the formula (2), namely
237·(1-x)+148·x≥120 (10)
From equation (10), all Si contents can meet the thermal conductivity requirements.
The Si content is selected to be 60 percent by comprehensively considering the factors of density, strength and the like.
Further using Mg2Si in place of a portion of Si according to a coefficient of thermal expansion of 12.0 + -1.0 × 10-6The requirement of/K and formula (1), provided that Mg2The Si content is x, the Si content is 0.27-x, i.e.
23.6×0.4+4.2·(0.6-x)+7.5·x＝12±1 (11)
Obtainable from formula (11), Mg2The Si content is 0-29.1% and can meet the requirement of thermal expansion coefficient.
Further, according to the requirement that the thermal conductivity is more than or equal to 120W/mK and the formula (2), namely
237×0.4+148·(0.6-x)+8·x≥120 (12)
Obtainable from formula (12), Mg2Si containsThe thermal conductivity requirement can be met when the amount is less than 45.4%.
The alloy composition is Al-31% Si-29% Mg based on the requirement of thermal expansion coefficient and thermal conductivity2Si。
S2: spray deposition blank making: according to the designed alloy composition of the step S1, pure aluminum and Al-Mg are blended2And smelting the Si intermediate alloy, and then carrying out spray deposition to obtain a deposited ingot blank.
Firstly, preparing materials by adopting pure aluminum, pure magnesium and Al-70% Si intermediate alloy, after the pure aluminum and the intermediate alloy are melted, cooling to 1000-1050 ℃ to reduce the burning loss of Mg, pressing a pure magnesium block into the bottom of a melt by adopting a graphite rod, and then carrying out in-situ reaction for 10-20 min under stirring; cooling to 1000-1050 ℃, casting by adopting a water-cooling mold, and cooling to obtain Al-50% Mg2A Si master alloy.
Further, pure aluminum, pure silicon and Al-50% Mg are used2The Si intermediate alloy is proportioned, melted and atomized under high pressure and deposited to obtain a spray deposition ingot blank, and the main technological parameters of spray deposition comprise: the rotating speed of the deposition disc is 400-500r/min, the descending speed of the deposition disc is 12-15mm/min, the diameter of the nozzle is 3.2mm, the deposition distance is 280-320mm, and the atomization pressure is 0.9-1.2 MPa.
Further, the above process is used to obtain spray deposited Al-31% Si-29% Mg2The average density of the Si alloy ingot blank is 91% +/-4%.
S3: thermal analysis and thermal stability analysis: obtaining a phase transition temperature point of a deposition ingot blank by adopting a differential thermal analysis method, designing a series of heating and heat-preserving procedures based on the phase transition temperature point, obtaining a series of blank samples by heating the deposition ingot blank samples under different heating procedures, observing microstructures, and establishing Si phase and Mg phase in alloy2Correlation of the Si phase coarsening rate with the heating temperature and the holding time.
Because the alloy is not added with other alloy elements, Al-31 percent of Si-29 percent of Mg are sprayed and deposited2Phase transition point of Si alloy and Al-12% Si-15% Mg2The Si alloy is similar, so that the heating and heat preservation are carried out at 530 ℃, 510 ℃, 490 ℃, 470 ℃, 450 ℃ and 430 ℃, the heat preservation time is 30-360 min, and one Si alloy is used every 30minAnd (4) gradient.
Further, observing the evolution of microstructures at different heating temperatures and different heat preservation times, and drawing Si phase and Mg phase in the alloy by combining with image analysis software2The relationship curve of the coarsening rate of the Si phase and the heating temperature and the holding time shows that Mg2The coarsening of Si and Si phases is obvious after heating and heat preservation at 530 ℃ for +30min and 510 ℃ for +240min, and Mg is obvious at other heating temperatures and heat preservation time2The Si and Si phases are less than 30 μm in size.
S4: hot isostatic compaction and heat treatment: the spray deposition ingot blank is densified by hot isostatic pressing, proper hot isostatic pressing heating temperature and heat preservation time are selected based on the result of the step S3, the hot isostatic pressing pressure is 120-150MPa, and the hot isostatic pressing alloy is subjected to low-temperature long-time stabilization annealing to obtain Al-31% Si-29% Mg2An Si alloy.
According to the heating temperature and the holding time in the step S3, the Si phase and Mg2According to the relation of Si phase size, the hot isostatic pressing heating temperature is selected to be 510 ℃, and the holding time is 210 min.
Further, Al-31% Si-29% Mg after hot isostatic pressing treatment2The density of the Si alloy is more than 99 percent.
Further, to eliminate or reduce the internal stress of the alloy, Si phase and Mg are taken into consideration2The Si phase and the Al matrix have large difference of thermal expansion coefficients and belong to brittle phases, Al is 31 percent of Si and 29 percent of Mg2The stabilization annealing process of the Si alloy is 360 ℃ plus 24 hours, and the temperature is reduced along with the furnace after the heat preservation is finished.
S5: microscopic structure and performance analysis: test Al-31% Si-29% Mg2Mechanical properties and physical properties of the Si alloy, observing a microstructure and a structure, and establishing a relation between the microstructure and the macroscopic properties of the alloy; optimizing the alloy components according to the macroscopic property requirements, particularly the thermal expansion coefficient and the structural property relation, and then repeating the steps S2-S5 to obtain the alloy meeting the property requirements.
Spray deposition of Al-31% Si-29% Mg2The microstructure characterization of the Si alloy comprises metallographic phase, a scanning electron microscope and the like, the mechanical properties comprise tensile strength, yield strength, elongation, bending strength and hardness, and the physical properties compriseDensity, thermal conductivity, and coefficient of thermal expansion.
Further, the chemical composition of the alloy is checked according to the method specified in GB/T20975; the density of the alloy is measured according to the method specified in GB 3850 or GB/T1423, and the specification of a sample piece is as follows: 20 multiplied by 10mm, and the density is the ratio of the measured density to the theoretical density multiplied by 100 percent; measuring the tensile strength of the alloy according to a method specified in GB/T228; measuring the specific heat capacity of the alloy according to a method specified by ASTM E1269 or GJB 330A, measuring the thermal diffusivity of the alloy according to a method specified by GB/T22588 or GJB1201.1, and calculating the thermal conductivity by a classical thermal conductivity formula; the coefficient of thermal expansion of the alloy was measured according to the method specified in GB/T4339 or GJB 332A.
Further, the test results showed that Al-31% Si-29% Mg2The thermal expansion coefficient of the Si alloy is 12.7X 10-6And the thermal conductivity is 116W/mK, which indicates that the thermal conductivity cannot meet the requirement of the electronic packaging shell.
From the formula (12), Mg is reduced2The Si content is beneficial to improving Al-Si-Mg2The thermal conductivity of the Si alloy is optimized, so that the alloy components are Al-35% Si-25% Mg2Si。
The steps S2-S5 were repeated, and the results of the tests showed that Al-35% Si-25% Mg was spray deposited2The thermal expansion coefficient of the Si alloy is 12.6X 10-6The thermal conductivity is 122W/mK, and the requirement of a typical electronic packaging cover plate on the thermal expansion coefficient and the thermal conductivity can be met.
Further, Al-35% Si-25% Mg2The density of the Si alloy is 2.38g/cm3The reduction is 3.3 percent relative to Al-60 percent Si alloy; the tensile strength is 246MPa, which is improved by 12.1 percent compared with Al-60 percent Si alloy.
S6: and (3) checking and verifying the shell: al-35% Si-25% Mg2The Si alloy is prepared by spray deposition, is processed into an electronic packaging shell (shown in figure 4) after being compacted and thermally treated by hot isostatic pressing, is examined and verified, and is compared with the spray deposition Al-60% Si alloy for analysis.
The examination and verification contents comprise the machining performance, the surface plating performance, the laser welding performance of the alloy, the air tightness of a sealing and welding shell and other process performances and application performances.
Furthermore, the examination result shows that Al is 35 percent of Si to 25 percent of Mg2The Si alloy has the packaging process performance similar to that of Al-60% Si alloy.
TABLE 1 Al, Si and Mg in the invention2Partial performance parameters of Si
Figure BDA0002744449060000121
Figure BDA0002744449060000131

Claims (9)

1. Light Al-Si-Mg2The preparation method of the Si electronic packaging material is characterized by comprising the following steps: the method comprises the following steps:
s1: designing alloy components: presetting Si phase and Mg according to the performance requirement of the finished product2The composition of the Si phase, the finished properties including strength, coefficient of thermal expansion, and thermal conductivity;
s2: spray deposition blank making: according to the alloy components designed in the step S1, pure aluminum, pure silicon and Al-Mg are mixed2Si intermediate alloy, smelting, and spray deposition to obtain Al-Si-Mg2A Si alloy ingot blank; the Al-Mg2In the Si master alloy, Mg2The volume fraction of Si is 50%;
s3: thermal analysis and thermal stability analysis: Al-Si-Mg is obtained by adopting a differential thermal analysis method2The phase transition temperature point of the Si alloy ingot blank, and based on the phase transition temperature point, a series of heating programs are designed, and Al-Si-Mg is heated2Heating Si alloy ingot blank samples under different heating procedures to obtain a series of blank samples, observing the microstructure, and establishing Si phase and Mg in the alloy at different heating temperatures2Thermal analysis data of the correlation of the Si phase size and the incubation time;
s4: hot isostatic compaction and heat treatment: subjecting the Al-Si-Mg obtained in step S2 to hot isostatic pressing2Densifying Si alloy ingot to obtain hot isostatic pressing alloyThe heating temperature and holding time of the hot isostatic pressing are selected from the thermal analysis data in step S3, and Si phase and Mg in the alloy2Corresponding ranges of the Si phase sizes which are all less than or equal to 30 mu m; then annealing the hot isostatic pressing alloy to obtain Al-Si-Mg2A Si alloy;
s5: microscopic structure and performance analysis: testing of Al-Si-Mg2The macroscopic performance of the Si alloy is observed, the microscopic structure and the structure are observed, the relation between the microscopic structure and the macroscopic performance of the alloy is established, if the macroscopic performance meets the requirement, the step S6 is carried out, if the macroscopic performance does not meet the requirement, the alloy components are optimized according to the relation between the microscopic structure and the macroscopic performance of the alloy, and the steps S2-S5 are repeated;
s6: and (3) checking and verifying the shell and/or the cover plate: will satisfy macroscopic properties of Al-Si-Mg2And processing the Si alloy into an electronic packaging shell and/or a cover plate for detection.
2. A light weight Al-Si-Mg as claimed in claim 12The preparation method of the Si electronic packaging material is characterized by comprising the following steps:
in the step S1, Si phase and Mg are preset2The specific steps of the composition of the Si phase are as follows:
step a
According to the requirements of electronic packaging materials on the thermal expansion coefficient and the thermal conductivity, the thermal expansion coefficient is firstly calculated by a mixing rule: formula (1), and thermal conductivity formula (2), the Si phase content is preset,
Figure 367153DEST_PATH_IMAGE002
Figure 815452DEST_PATH_IMAGE004
wherein the content of the first and second substances,αwhich represents the coefficient of thermal expansion of the material,𝜆which represents the thermal conductivity of the material,Vrepresents a volume fraction;
step b
Then, part of Mg is used2Substitution of Si phaseThe Si phase is substituted and then the thermal expansion coefficient formula (3) and the thermal conductivity formula (4) are calculated by a mixing rule, so that the requirements of the thermal expansion coefficient and the thermal conductivity of the electronic packaging material are met,
Figure 126348DEST_PATH_IMAGE006
Figure 285671DEST_PATH_IMAGE008
。
3. a light weight Al-Si-Mg as claimed in claim 12The preparation method of the Si electronic packaging material is characterized by comprising the following steps:
in the step S2, the Al-Mg2The preparation process of the Si intermediate alloy comprises the following steps: the method comprises the steps of proportioning pure aluminum, pure magnesium and Al-70Si intermediate alloy, melting the pure aluminum and the Al-70Si intermediate alloy, cooling to 1000-1050 ℃, adding the pure magnesium, carrying out in-situ reaction, and generating Mg in the melt2Si, cooling and solidifying after stirring to obtain Al-Mg2A Si master alloy.
4. A light weight Al-Si-Mg as claimed in claim 12The preparation method of the Si electronic packaging material is characterized by comprising the following steps:
in step S2, the main process parameters of the spray deposition are: the rotating speed of the deposition disc is 300-500r/min, the descending speed of the deposition disc is 10-15mm/min, the diameter of the nozzle is 2.8-3.5mm, the deposition distance is 260-320mm, and the atomization pressure is 0.8-1.2 MPa.
5. A light weight Al-Si-Mg as claimed in claim 12The preparation method of the Si electronic packaging material is characterized by comprising the following steps:
in the step S2, Al-Si-Mg2The density of the Si alloy ingot blank is more than or equal to 85 percent.
6. A light weight Al-Si-Mg as claimed in claim 12Si electronic packaging materialThe preparation method of the material is characterized by comprising the following steps: in the step S4, the hot isostatic pressure is 120-150 MPa.
7. A light weight Al-Si-Mg as claimed in claim 12The preparation method of the Si electronic packaging material is characterized by comprising the following steps: in the step S4, Al-Si-Mg2The annealing temperature of the Si alloy is 280-360 ℃, the heat preservation time is 24-96 h, and the temperature is reduced along with the furnace after the heat preservation is finished.
8. Light Al-Si-Mg produced by the production method according to any one of claims 1 to 72A Si electronic packaging material.
9. Light Al-Si-Mg produced by the production method according to any one of claims 1 to 72The application of the Si electronic packaging material is characterized in that: the light Al-Si-Mg2The Si electronic packaging material is applied as an electronic packaging shell material or an electronic packaging cover plate material.
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