CN109943755B - Preparation method of aluminum-based composite material for electronic packaging - Google Patents
Preparation method of aluminum-based composite material for electronic packaging Download PDFInfo
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- CN109943755B CN109943755B CN201910319162.4A CN201910319162A CN109943755B CN 109943755 B CN109943755 B CN 109943755B CN 201910319162 A CN201910319162 A CN 201910319162A CN 109943755 B CN109943755 B CN 109943755B
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Abstract
The invention relates to a preparation method of an aluminum-based composite material for electronic packaging, which is characterized by comprising the following steps: preparing SiC particles coated with cobalt on the surface; uniformly mixing SiC particles, Al-Si alloy powder and pure aluminum powder by ball milling to obtain prefabricated powder A; uniformly mixing the SiC particles prepared in the step (a), Al-Si alloy powder and pure aluminum powder to obtain matrix powder B; uniformly mixing the prefabricated powder A and the matrix powder B to obtain powder C; cold isostatic pressing; gradient sintering and hot isostatic pressing. The preparation method can prepare the aluminum matrix composite material with better performance and has lower cost.
Description
Technical Field
The invention relates to an electronic packaging material, in particular to a preparation method of an aluminum-based composite material for electronic packaging.
Background
The electronic packaging material is a sealing body of an integrated circuit, has mechanical support and environmental protection effects on a chip, and prevents the chip from being polluted and corroded by water vapor, impurities and various chemical atmospheres in the atmosphere, so that the integrated circuit chip can stably play a normal electrical function, and the packaging material plays a very important role in thermal performance and even reliability of electronic devices and circuits.
The electronic packaging materials commonly used in the prior art comprise plastics, ceramics, metals and the like, wherein the aluminum-based composite material promotes the packaged products due to the advantages of light weight, high strength, low expansion, high heat conductivity and the likeThe development of high density, miniaturization and high power is advanced. The aluminum-based composite material in the prior art comprises an Al-Si packaging material (the Si content is 27-70 wt%), but the rigidity of the material is poor; in the prior art, an aluminum matrix composite material with SiC particles as a reinforcing phase is also available, but the high-temperature reaction of SiC and Al can form Al4C3Brittle phase, Al4C3The phase at the interface of SiC and the aluminum matrix can reduce the mechanical property and the corrosion resistance of the aluminum matrix composite. Therefore, there is a need for a method for preparing an aluminum matrix composite for electronic packaging with better performance, which is required to reduce the cost as much as possible for the convenience of industrial application.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of an aluminum-based composite material for electronic packaging, which can prepare the aluminum-based composite material with better performance and lower cost, aiming at the current situation of the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the aluminum-based composite material for electronic packaging is characterized by comprising the following steps:
(a) preparing SiC particles coated with cobalt on the surface;
(b) uniformly mixing the SiC particles prepared in the step (a), Al-Si alloy powder and pure aluminum powder by ball milling to obtain prefabricated powder A;
(c) uniformly mixing the SiC particles prepared in the step (a), Al-Si alloy powder and pure aluminum powder to obtain matrix powder B;
(d) uniformly mixing the prefabricated powder A and the matrix powder B to obtain powder C;
(e) carrying out cold isostatic pressing on the powder C to prepare an ingot blank;
(f) carrying out three-section gradient sintering on the ingot blank at the temperature of 380-950 ℃ and including a low-temperature section, a medium-temperature section and a high-temperature section;
(g) carrying out hot isostatic pressing on the sintered blank, and then cooling to obtain a finished product, wherein the mass fraction of SiC particles in the finished product is 0-70% (excluding 0), the mass fraction of Si-phase particles is 0-70% (excluding 0), and the balance is Al;
the Si content of the Al-Si alloy powder is 30-70% by weight.
The Si phase in the finished product of the invention is all from Al-Si alloy powder. The mixing in steps (c) and (d) of the present invention may be carried out by a conventional mixing method such as mixing using a blender, without using a ball mill.
When the material is prepared, the mass ratio of the prefabricated powder A relative to the matrix powder B can be automatically adjusted according to the requirement; and the component ratios of the SiC particles, the Al-Si alloy powder and the pure aluminum powder in the prefabricated powder A and the matrix powder B can be automatically adjusted according to the requirements. The gradient sintering of the invention can select three temperatures from low to high to carry out three-stage gradient sintering of a low temperature stage, a medium temperature stage and a high temperature stage within the range of 380-950 ℃ according to specific requirements.
Preferably, the mass fraction of the SiC particles in the finished product of the step (g) is 10-30%, the mass fraction of the Si phase particles is 10-50%, and the balance is Al. The performance of the finished product in this range is better.
For cost saving, the pre-formed powder A accounts for 5wt% -50 wt% of the total mass of the powder C. And a small amount of powder is subjected to ball milling, so that the cost can be reduced as far as possible on the basis of ensuring the subsequent sintering performance.
Preferably, the pressure of the cold isostatic pressing in the step (e) is 160-220 MPa.
Preferably, the temperature of the low temperature section in the step (f) is 380-550 ℃, and the sintering time is 0.5-3 h; the temperature range of the medium temperature section is 450-650 ℃, and the sintering time is 0.5-3 h; the temperature range of the high-temperature section is 540-950 ℃, and the sintering time is 0.5-3 h.
Preferably, the hot isostatic pressing in step (g) has a temperature of 550-650 ℃, a pressure of 180-220MPa, and a dwell time of 0.5-2 hours.
Preferably, SiC particles are added to CoCl dissolved and dispersed in an ethanol solvent2The solution is placed for 0.5 to 1.5 hours and then is roasted for 2 to 3 hours at the temperature of 850 ℃ and 1000 ℃.
Preferably, the particle size distribution of the SiC particles is 20-50 μm, the particle size distribution of the Al-Si alloy powder is 20-50 μm, and the pure aluminum powder is selected from the range of 100-300 meshes.
Compared with the prior art, the invention has the advantages that:
the surface of the treated SiC particles is coated with Co, so that the high-temperature reaction of SiC and Al to form Al can be reduced4C3The tendency of brittle phase, thereby improving the mechanical property and the corrosion resistance of the composite material;
2. on the basis of adding SiC particles, Si-phase particles are added to reduce the thermal stress of the material and improve the processing performance of the material;
3. compared with the Al-Si packaging material (the Si content is 27-70 percent by weight), the rigidity of the material is increased, and the growth tendency of the Si phase can be effectively inhibited in the high-temperature heating preparation process;
4. the Al-Si alloy powder can use Al-Si over-spraying powder byproducts generated by a rapid cooling or spray deposition process, so that the cost is reduced;
5. the powder C is divided into the preformed powder A prepared by ball milling and the common mixed matrix powder B, only the preformed powder A needs to be ball milled, the cost is greatly reduced, the addition of the ball milled preformed powder A can further ensure that the material tissue is compact, uniform and fine, and the activity after ball milling can increase the sintering power and improve the sintering efficiency;
6. the gradient sintering at the temperature of 380-950 ℃ is adopted, so that the probability of generating defects such as holes, uneven component distribution, SiC particle agglomeration and the like in a microstructure can be reduced;
7. the obtained packaging material has low expansion, good heat conductivity and good strength.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention.
Example 1Al-27 wt% Si-23 wt% SiC Low expansion high thermal conductivity encapsulation Material
Adding SiC particles with the particle size distribution of 20-50 mu m into CoCl dissolved and dispersed by an ethanol solvent2Then, the mixture was left to stand for 0.5 hour and baked at 920 ℃ for 2.5 hours. This example uses CoCl2Saturated solution of ethanol of (1), CoCl2With ethanolThe proportion can be adjusted as required, so as to be subject to successful coating.
Selecting Al-Si alloy powder (Si content 50 wt%) with 20-50 micrometers of grain size distribution, in which the Al-Si alloy powder is obtained by spray powder and grain size screening.
Mixing the SiC particles, the Al-Si alloy powder and the pure aluminum powder, putting the mixture into a ball mill for ball milling and mixing, and introducing argon gas for protection in the ball milling process to prepare prefabricated powder A; the pure aluminum powder of this example is 200 mesh atomized aluminum powder.
And fourthly, mixing the SiC particles, the Al-Si alloy powder and the pure aluminum powder according to a certain weight percentage to obtain matrix powder B.
Fifthly, putting the prefabricated powder A and the matrix powder B into a mixer to be uniformly mixed (the adding mass ratio of the A to the B is 1:9) to obtain powder C.
Sixthly, performing isostatic cool pressing on the powder C under 180MPa to prepare an ingot blank with the diameter of 250 mm;
seventhly, carrying out gradient sintering on the ingot blank at 550 ℃ for 1 hour, 650 ℃ for 0.5 hour and 950 ℃ for 0.5 hour;
and carrying out hot isostatic pressing on the sintered ingot blank at 550 ℃ and 200MPa for 1 hour, and then cooling along with the furnace.
The obtained packaging material has the thermal conductivity of 180W/mk, the tensile strength of 190MPa and the expansion coefficient of 10.5 multiplied by 10-6/℃。
Example 2Al-47 wt% Si-23 wt% SiC Low expansion high thermal conductivity encapsulation Material
Adding SiC particles with the particle size distribution of 20-50 mu m into CoCl dissolved and dispersed by an ethanol solvent2After standing for 1 hour, the mixture was calcined at 920 ℃ for 2.5 hours.
Selecting Al-Si alloy powder (Si content 30 wt%) with 20-50 micrometer grain size distribution, in which the Al-Si alloy powder is obtained by spray powder and grain size screening.
Mixing the SiC particles, the Al-Si alloy powder and the pure aluminum powder, putting the mixture into a ball mill for ball milling and mixing, and introducing argon gas for protection in the ball milling process to prepare prefabricated powder A; the pure aluminum powder of this example is 200 mesh atomized aluminum powder.
And fourthly, mixing the SiC particles, the Al-Si alloy powder and the pure aluminum powder according to a certain weight percentage to obtain matrix powder B.
Fifthly, putting the prefabricated powder A and the matrix powder B into a mixer to be uniformly mixed (the adding mass ratio of the A to the B is 2:8) to obtain powder C.
Sixthly, performing isostatic cool pressing on the powder C under 220MPa to prepare an ingot blank with the diameter of 200 mm;
seventhly, carrying out gradient sintering on the ingot blank at the temperature of 450 ℃ for 1 hour, at the temperature of 600 ℃ for 2.5 hours and at the temperature of 800 ℃ for 0.5 hour;
subjecting the sintered ingot blank to hot isostatic pressing at 650 ℃ and 180MPa, keeping the pressure for 0.5 hour, and then cooling along with the furnace.
Thermal conductivity 152W/mk, tensile strength 160MPa, and expansion coefficient 6.9X 10-6/℃.
Example 3Al-30 wt% Si-30 wt% SiC Low expansion high thermal conductivity encapsulation Material
Adding SiC particles with the particle size distribution of 20-50 mu m into CoCl dissolved and dispersed by an ethanol solvent2After standing for 1 hour, the mixture was calcined at 920 ℃ for 2.5 hours.
Selecting Al-Si alloy powder (Si content 70 wt%) with 20-50 micrometer grain size distribution, in which the Al-Si alloy powder is obtained by spray powder and grain size screening.
Mixing the SiC particles, the Al-Si alloy powder and the pure aluminum powder, putting the mixture into a ball mill for ball milling and mixing, and introducing argon gas for protection in the ball milling process to prepare prefabricated powder A; the pure aluminum powder of this example is 200 mesh atomized aluminum powder.
And fourthly, mixing the SiC particles, the Al-Si alloy powder and the pure aluminum powder according to a certain weight percentage to obtain matrix powder B.
Fifthly, putting the prefabricated powder A and the matrix powder B into a mixer to be uniformly mixed (the adding mass ratio of the A to the B is 3:7) to obtain powder C.
Sixthly, performing isostatic cool pressing on the powder C under 160MPa to prepare an ingot blank with the diameter of 250 mm;
seventhly, sintering the ingot blank at 380 ℃ for 1 hour, 450 ℃ for 2.5 hours and 540 ℃ for 1.5 in a gradient manner;
and carrying out hot isostatic pressing on the sintered ingot blank at 550 ℃ and 180MPa for 2 hours, and then cooling along with the furnace.
158W/mk thermal conductivity, 170MPa tensile strength and 8.2X 10 expansion coefficient-6/℃。
The technical means disclosed in the invention scheme are not limited to the technical means disclosed in the above embodiments, but also include the technical scheme formed by any combination of the above technical features. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and such improvements and modifications are also considered to be within the scope of the present invention.
Claims (6)
1. A preparation method of an aluminum-based composite material for electronic packaging is characterized by comprising the following steps:
(a) preparing SiC particles coated with cobalt on the surface; the specific process for coating cobalt comprises the following steps: adding SiC particles into CoCl dissolved and dispersed in ethanol solvent2The solution is placed for 0.5 to 1.5 hours and then is roasted for 2 to 3 hours at the temperature of 850-;
(b) uniformly mixing the SiC particles prepared in the step (a), Al-Si alloy powder and pure aluminum powder by ball milling to obtain prefabricated powder A;
(c) uniformly mixing the SiC particles prepared in the step (a), Al-Si alloy powder and pure aluminum powder to obtain matrix powder B;
(d) uniformly mixing the prefabricated powder A and the matrix powder B to obtain powder C;
(e) carrying out cold isostatic pressing on the powder C to prepare an ingot blank;
(f) carrying out three-section gradient sintering on the ingot blank at the temperature of 380-950 ℃ and including a low-temperature section, a medium-temperature section and a high-temperature section; the temperature range of the low-temperature section is 380-550 ℃, and the sintering time is 0.5-3 h; the temperature range of the medium temperature section is 450-650 ℃, and the sintering time is 0.5-3 h; the temperature range of the high-temperature section is 540-950 ℃, and the sintering time is 0.5-3 h;
(g) carrying out hot isostatic pressing on the sintered blank, and then cooling to obtain a finished product, wherein the mass fraction of SiC particles in the finished product is 0-70%, excluding 0; the mass fraction of the Si-phase particles is 0-70%, excluding 0, and the balance is Al;
the Si content of the Al-Si alloy powder is 30-70% by weight.
2. The method for preparing an aluminum-based composite material for electronic packaging according to claim 1, characterized in that: the mass fraction of SiC particles in the finished product in the step (g) is 10-30%, the mass fraction of Si phase particles is 10-50%, and the balance is Al.
3. The method for preparing an aluminum-based composite material for electronic packaging according to claim 1, characterized in that: the preformed powder A accounts for 5-50 wt% of the total mass of the powder C.
4. The method for preparing an aluminum-based composite material for electronic packaging according to claim 1, characterized in that: the pressure of the cold isostatic pressing in the step (e) is 160-220 MPa.
5. The method for preparing an aluminum-based composite material for electronic packaging according to claim 1, characterized in that: the hot isostatic pressing in the step (g) is carried out at the temperature of 550-650 ℃, the pressure of 180-220MPa and the pressure maintaining time of 0.5-2 hours.
6. The method for preparing an aluminum-based composite material for electronic packaging according to any one of claims 1 to 5, characterized in that: the grain size distribution of the SiC grains is 20-50 mu m, the grain size distribution of the Al-Si alloy powder is 20-50 mu m, and the pure aluminum powder is selected from the range of 100-300 meshes.
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| CN112030027B (en) * | 2020-09-02 | 2022-09-27 | 宁波乌卡科技有限公司 | Preparation method of multifunctional induction aluminum alloy manipulator material |
| CN114540671A (en) * | 2022-02-18 | 2022-05-27 | 河北新立中有色金属集团有限公司 | Aluminum-silicon alloy-based composite material and preparation method and application thereof |
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