CN101898240B - Preparation method of SiC/Al composite material for electronic packaging - Google Patents
Preparation method of SiC/Al composite material for electronic packaging Download PDFInfo
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- CN101898240B CN101898240B CN2010102501088A CN201010250108A CN101898240B CN 101898240 B CN101898240 B CN 101898240B CN 2010102501088 A CN2010102501088 A CN 2010102501088A CN 201010250108 A CN201010250108 A CN 201010250108A CN 101898240 B CN101898240 B CN 101898240B
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Abstract
The invention discloses a preparation method of a SiC/Al composite material for electronic packaging, which comprises the following steps: 1) mixing polyvinyl alcohol solution with saturated SiO2 sol for preparing a binder; 2) adding the binder into beta-SiC particles, mixing, granulating, carrying out die pressing, and preparing a green body; 3) drying the green body, carrying out binder removal, increasing the temperature, keeping the temperature, then carrying out furnace cooling, and preparing a SiC preform; 4) preparing an alloy; and 5) placing the preheated SiC preform into the molten alloy for impregnation and preparing the SiC/Al composite material. The preparation process is simple and does not need complex and expensive equipment, and the impregnation process does not need conditions on vacuum, pressure and atmosphere protection. The preparation method is simple, the requirements on the equipment are low, and the thermophysical property of the prepared material can be regulated within a relatively wide range, thereby being capable of meeting the electronic packaging requirements.
Description
Technical field
The invention belongs to the electronic package material field, be specifically related to a kind of preparation method of used for electronic packaging SiC/Al composite.
Background technology
Development of semiconductor is maked rapid progress, since 1958 first block semiconductor integrated circuits come out, up to the present, the development of IC chip integration is more and more higher, power is increasing, and the raising of integrated level must cause the rising of its heat generation rate, makes the operating temperature of circuit constantly rise, thereby cause the increase of part failure rate, therefore all one's effort is studied and is prepared the novel encapsulated material with high thermal conductance and good combination property and seems particularly important.
In order to satisfy the requirement of high density, miniaturization, high-power integrated circuit, desirable electronic package material must possess following characteristic: (1) has high thermal, the heat that semiconductor chip is produced when working can be distributed in time, lost efficacy in order to avoid chip temperature is too high; (2) lower thermal coefficient of expansion is arranged, and be complementary, in order to avoid chip is because of thermal stress damage with chips such as Si or GaAs; (3) enough strength and stiffness are arranged, can play chip and support and protective effect; (4) good air tightness is arranged, stop steam, harmful ion or gas in the environment to enter in the packing component, cause failure modes such as parameter variation; (5) require density as far as possible little at some special occasions, as aerospace applications, lightweight mobile communication equipment; (6) cost is low as far as possible, to satisfy the large-scale commercial applications application.
Metal-base composites (MMC) can metallic matrix is good heat conductivility and strengthen the low-expansion characteristics of body material and combine, and the SiC/Al composite has effectively utilized the high thermal conductivity coefficient (230Wm of aluminum substrate just
-1K
-1) and the low-expansion coefficient (3.8 * 10 of SiC
-6～4.1 * 10
-6K
-1) combine, have lower density, excellent mechanical property.The SiC/Al composite can with the chip matched coefficients of thermal expansion, efficiently radiates heat has enough support protective effects, and can regulate the volume fraction of SiC particle arbitrarily and change the aluminum matrix alloy composition, to reach the well-designed of composite material combination property.
But because electronic package material requires more than 55% with SiC volume fraction in the SiC/Al composite, and molten aluminum liquid viscosity is big, surface tension is big, wetting hardly with the SiC particle, therefore can not adopt conventional stirring casting, the preparation of methods such as powder metallurgy need realize by means of the technology of complexity and expensive equipment usually, increase the cost of this material greatly, also limited its development and application.
Summary of the invention
The objective of the invention is for overcoming disadvantages of background technology, a kind of preparation method of used for electronic packaging SiC/Al composite is provided, and this preparation method is simple, and equipment is less demanding, the thermophysical property of prepared material can satisfy the Electronic Packaging requirement in regulated in wider range.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of used for electronic packaging SiC/Al composite is characterized in that this method may further comprise the steps:
(1) be that 2%～8% polyvinyl alcohol water solution and mass fraction are 30%～40% SiO with mass fraction
2Colloidal sol is mixed and made into binding agent;
(2) binding agent described in the step (1) is added in β-SiC particle mix, the cylindrical steel molding jig is put in granulation then, is pressed into base substrate under 30MPa～80MPa pressure;
(3) base substrate described in the step (2) being placed drying box, is under 100 ℃～180 ℃ the condition dry 1～3 hour in temperature; Be binder removal twice respectively under 250 ℃, 450 ℃ the condition in temperature with dried base substrate, each binder removal time is 1 hour; Base substrate behind the binder removal is put into resistance furnace, is to be warming up to 1100 ℃～1200 ℃ under the condition of 10 ℃/min～50 ℃/min at heating rate, is incubated 1～2 hour, obtains the SiC precast body with the stove cooling then;
(4) aluminium block, MAG block and silico briquette are placed the induction furnace melting by mass ratio at 100: 8: 13, the cooling back forms alloy, and alloy is cut into piece;
(5) alloy that cuts into piece in the step (4) is placed corundum crucible, put into the resistance furnace heat fused then, obtain the alloy liquation; SiC precast body described in the step (3) is preheated to 700 ℃～800 ℃ in another resistance furnace; SiC precast body after the preheating is put into the alloy liquation rapidly infiltrate, add by SiO simultaneously
2Powder and CaF
2The slag former that powder mixes by mass ratio 1: 1～5; form the fine and close slag blanket of one deck at the alloy molten surface in order to protection alloy liquation; be warming up to 850 ℃～950 ℃ then rapidly; and be incubated 1～3 hour; treat to remove when the alloy liquation is cooled to 680 ℃ the fine and close slag blanket of alloy molten surface; the SiC precast body is taken out from the alloy liquation, and cooling promptly obtains the SiC/Al composite.
Polyvinyl alcohol water solution and SiO described in the above-mentioned steps (1)
2The volume ratio of colloidal sol is 1: 1～2.
β described in the above-mentioned steps (2)-SiC particle is that β-SiC of 50 μ m and β-SiC that granularity is 10 μ m mix by mass ratio 10: 1～3 by granularity; The mass ratio of binding agent and β-SiC particle is 3～5: 100 described in the step (2).
The porosity of SiC precast body is 30%～42% described in the above-mentioned steps (3).
The quality purity of aluminium block is 99.7% described in the above-mentioned steps (4), and the quality purity of MAG block is 99.5%, and the quality purity of silico briquette is 99%, and the temperature of melting is 1650 ℃, and the time of melting is 5 minutes.
The temperature of fusing is 680 ℃ described in the above-mentioned steps (5), and the thickness of fine and close slag blanket is 10mm～20mm.
The present invention compared with prior art has the following advantages:
1, preparation process does not need the support of vacuum equipment, press device, protective atmosphere; Raw material sources are wide, low price, can at utmost reduce material cost and simplify preparation technology.
2, the alloy that is adopted can substantially improve with the wetability of SiC particle and stop bad interfacial reaction, solves the key issue of this composite of preparation, and infiltration process is carried out smoothly.
3, the slag protection method that is adopted can make the alloy liquation repeatedly use under air conditions.
4, the prepared SiC/Al composite of the present invention is selected β-SiC for use, substitutes the α-SiC of equal volume mark, can make the thermal conductivity of composite improve 4%～6%, and thermal coefficient of expansion reduces by 5%～8%, can satisfy the requirement of Electronic Packaging fully.
5, the prepared SiC/Al composite property of the present invention is good, and relative density is 98.2%～99.4%, and thermal conductivity is 166～189Wm
-1K
-1, thermal coefficient of expansion is 6.4 * 10
-6～7.8 * 10
-6K
-1, the volume fraction of β-SiC is 58%～70%.
Description of drawings
Fig. 1 is the micro-organization chart according to the SiC/Al composite of the embodiment of the invention 1 preparation.
Fig. 2 is the micro-organization chart according to the SiC/Al composite of the embodiment of the invention 2 preparations.
Fig. 3 is the micro-organization chart according to the SiC/Al composite of the embodiment of the invention 3 preparations.
Fig. 4 is the micro-organization chart according to the SiC/Al composite of the embodiment of the invention 4 preparations.
The specific embodiment
(1) be that 4% polyvinyl alcohol water solution and mass fraction are 30% SiO with mass fraction
2Colloidal sol was mixed and made into binding agent in 1: 1 by volume;
(2) adopting granularity is β-SiC particle that β-SiC of 50 μ m and β-SiC that granularity is 10 μ m mix by mass ratio at 10: 1, binding agent and β-SiC particle are mixed by mass ratio at 5: 100, granulation is put into the cylindrical steel molding jig and be pressed into base substrate under the pressure of 55MPa;
(3) base substrate is placed drying box, drying is 2 hours under 120 ℃ of conditions, under 250 ℃, 450 ℃ conditions, distinguish binder removal 1 hour then, put into resistance furnace subsequently, speed with 30 ℃/min is warming up to 1200 ℃, be incubated 1 hour, obtaining porosity with stove cooling then is 30% SiC precast body;
(4) with the aluminium block of quality purity 99.7%, the MAG block of quality purity 99.5%, the silico briquette of quality purity 99% places induction furnace by mass ratio at 100: 8: 13, and melting is 5 minutes under 1650 ℃ of conditions, and the cooling back forms alloy, cuts into piece;
(5) alloy that will cut into piece places corundum crucible, puts into resistance furnace then and is heated to 680 ℃ of fusings, obtains the alloy liquation; The SiC precast body is preheated to 700 ℃ in another resistance furnace; SiC precast body after the preheating is put into the alloy liquation infiltrate, add by SiO simultaneously
2Powder and CaF
2The slag former that powder mixes by mass ratio at 1: 1; form the thick fine and close slag blanket of one deck 10mm at the alloy molten surface in order to protection alloy liquation; be warming up to 850 ℃ then rapidly; be incubated 3 hours; treat to remove when the alloy liquation is cooled to 680 ℃ the fine and close slag blanket of alloy molten surface; the SiC precast body is taken out from the alloy liquation, and it is 98.2% that cooling promptly obtains relative density, and thermal conductivity is 189Wm
-1K
-1, thermal coefficient of expansion is 7.8 * 10
-6K
-1, the volume fraction of β-SiC is 58% SiC/Al composite.
Micro-organization chart such as Fig. 1 according to the SiC/Al composite of present embodiment preparation, the grey bulk is distributed as β-SiC particle among the figure, the zone of brilliant white is an alloy substrate, be distributed in the alloy substrate to β-SiC uniform particles, granule β-SiC is distributed in around bulky grain β-SiC, the interface combination of composite is good, dense structure, defectives such as pore-free.
Embodiment 2
(1) be that 2% polyvinyl alcohol water solution and mass fraction are 40% SiO with mass fraction
2Colloidal sol was mixed and made into binding agent in 1: 1 by volume;
(2) β-SiC particle that to adopt granularity be β-SiC of 50 μ m and β-SiC that granularity is 10 μ m mixes by 10: 3 mass ratio, binding agent and β-SiC particle are mixed by mass ratio at 3: 100, granulation is put into the cylindrical steel molding jig and be pressed into base substrate under the pressure of 30MPa;
(3) base substrate is placed drying box, drying is 1 hour under 180 ℃ of conditions, under 250 ℃, 450 ℃ conditions, distinguish binder removal 1 hour then, put into resistance furnace subsequently, speed with 50 ℃/min is warming up to 1100 ℃, be incubated 2 hours, obtaining porosity with stove cooling then is 42% SiC precast body;
(4) with the aluminium block of quality purity 99.7%, the MAG block of quality purity 99.5%, the silico briquette of quality purity 99% places induction furnace by mass ratio at 100: 8: 13, and melting is 5 minutes under 1650 ℃ of conditions, and the cooling back forms alloy, cuts into piece;
(5) alloy that will cut into piece places corundum crucible, puts into resistance furnace then and is heated to 680 ℃ of fusings, obtains the alloy liquation; The SiC precast body is preheated to 800 ℃ in another resistance furnace; SiC precast body after the preheating is put into the alloy liquation infiltrate, add by SiO simultaneously
2Powder and CaF
2The slag former that powder mixes by mass ratio at 1: 5; form the thick fine and close slag blanket of one deck 20mm at the alloy molten surface in order to protection alloy liquation; be warming up to 950 ℃ then rapidly; be incubated 1 hour; treat to remove when the alloy liquation is cooled to 680 ℃ the fine and close slag blanket of alloy molten surface; the SiC precast body is taken out from the alloy liquation, and it is 98.8% that cooling promptly obtains relative density, and thermal conductivity is 178Wm
-1K
-1, thermal coefficient of expansion is 7.1 * 10
-6K
-1, the volume fraction of β-SiC is 70% SiC/Al composite.
Micro-organization chart such as Fig. 2 according to the SiC/Al composite of present embodiment preparation, the grey bulk is distributed as β-SiC particle among the figure, the zone of brilliant white is an alloy substrate, be distributed in the alloy substrate to β-SiC uniform particles, granule β-SiC is distributed in around bulky grain β-SiC, the interface combination of composite is good, dense structure, defectives such as pore-free.
Embodiment 3
(1) be that 5% polyvinyl alcohol water solution and mass fraction are 38% SiO with mass fraction
2Colloidal sol was mixed and made into binding agent in 1: 1.5 by volume;
(2) adopting granularity is β-SiC particle that β-SiC of 50 μ m and β-SiC that granularity is 10 μ m mix by mass ratio at 10: 2, binding agent and β-SiC particle are mixed by mass ratio at 4: 100, granulation is put into the cylindrical steel molding jig and be pressed into base substrate under the pressure of 80MPa;
(3) base substrate is placed drying box, drying is 2 hours under 140 ℃ of conditions, under 250 ℃, 450 ℃ conditions, distinguish binder removal 1 hour then, put into resistance furnace subsequently, speed with 10 ℃/min is warming up to 1150 ℃, be incubated 2 hours, obtaining porosity with stove cooling then is 36% SiC precast body;
(4) with the aluminium block of quality purity 99.7%, the MAG block of quality purity 99.5%, the silico briquette of quality purity 99% places induction furnace by mass ratio at 100: 8: 13, and melting is 5 minutes under 1650 ℃ of conditions, and the cooling back forms alloy, cuts into piece;
(5) alloy that will cut into piece places corundum crucible, puts into resistance furnace then and is heated to 680 ℃ of fusings, obtains the alloy liquation; The SiC precast body is preheated to 750 ℃ in another resistance furnace; SiC precast body after the preheating is put into the alloy liquation infiltrate, add by SiO simultaneously
2Powder and CaF
2The slag former that powder mixes by mass ratio at 1: 3; form the thick fine and close slag blanket of one deck 15mm at the alloy molten surface in order to protection alloy liquation; be warming up to 900 ℃ then rapidly; be incubated 2 hours; treat to remove when the alloy liquation is cooled to 680 ℃ the fine and close slag blanket of alloy molten surface; the SiC precast body is taken out from the alloy liquation, and it is 98.9% that cooling promptly obtains relative density, and thermal conductivity is 172Wm
-1K
-1, thermal coefficient of expansion is 6.8 * 10
-6K
-1, the volume fraction of β-SiC is 68% SiC/Al composite.
Micro-organization chart such as Fig. 3 according to the SiC/Al composite of present embodiment preparation, the grey bulk is distributed as β-SiC particle among the figure, the zone of brilliant white is an alloy substrate, be distributed in the alloy substrate to β-SiC uniform particles, granule β-SiC is distributed in around bulky grain β-SiC, the interface combination of composite is good, dense structure, defectives such as pore-free.
Embodiment 4
(1) be that 8% polyvinyl alcohol water solution and mass fraction are 35% SiO with mass fraction
2Colloidal sol was mixed and made into binding agent in 1: 2 by volume;
(2) adopting granularity is β-SiC particle that β-SiC of 50 μ m and β-SiC that granularity is 10 μ m mix by mass ratio at 10: 3, binding agent and β-SiC particle are mixed by mass ratio at 5: 100, granulation is put into the cylindrical steel molding jig and be pressed into base substrate under the pressure of 60MPa;
(3) base substrate is placed drying box, drying is 3 hours under 100 ℃ of conditions, under 250 ℃, 450 ℃ conditions, distinguish binder removal 1 hour then, put into resistance furnace subsequently, speed with 30 ℃/min is warming up to 1200 ℃, be incubated 1.5 hours, obtaining porosity with stove cooling then is 40% SiC precast body;
(4) with the aluminium block of quality purity 99.7%, the MAG block of quality purity 99.5%, the silico briquette of quality purity 99% places induction furnace by mass ratio at 100: 8: 13, and melting is 5 minutes under 1650 ℃ of conditions, and the cooling back forms alloy, cuts into piece;
(5) alloy that will cut into piece places corundum crucible, puts into resistance furnace then and is heated to 680 ℃ of fusings, obtains the alloy liquation; The SiC precast body is preheated to 780 ℃ in another resistance furnace; SiC precast body after the preheating is put into the alloy liquation infiltrate, add by SiO simultaneously
2Powder and CaF
2The slag former that powder mixes by mass ratio at 1: 3; form the thick fine and close slag blanket of one deck 20mm at the alloy molten surface in order to protection alloy liquation; be warming up to 880 ℃ then rapidly; be incubated 2 hours; treat to remove when the alloy liquation is cooled to 680 ℃ the fine and close slag blanket of alloy molten surface; the SiC precast body is taken out from the alloy liquation, and it is 99.4% that cooling promptly obtains relative density, and thermal conductivity is 166Wm
-1K
-1, thermal coefficient of expansion is 6.4 * 10
-6K
-1, the volume fraction of β-SiC is 64% SiC/Al composite.
Micro-organization chart such as Fig. 4 according to the SiC/Al composite of present embodiment preparation, the grey bulk is distributed as β-SiC particle among the figure, the zone of brilliant white is an alloy substrate, be distributed in the alloy substrate to β-SiC uniform particles, granule β-SiC is distributed in around bulky grain β-SiC, the interface combination of composite is good, dense structure, defectives such as pore-free.
Claims (6)
1. the preparation method of a used for electronic packaging SiC/Al composite is characterized in that, this method may further comprise the steps:
(1) be that 2%～8% polyvinyl alcohol water solution and mass fraction are 30%～40% SiO with mass fraction
2Colloidal sol is mixed and made into binding agent;
(2) binding agent described in the step (1) is added in β-SiC particle mix, the cylindrical steel molding jig is put in granulation then, is pressed into base substrate under 30MPa～80MPa pressure;
(3) base substrate described in the step (2) being placed drying box, is under 100 ℃～180 ℃ the condition dry 1～3 hour in temperature; With dried base substrate be in temperature under 250 ℃, 450 ℃ the condition respectively binder removal once, each binder removal time is 1 hour; Base substrate behind the binder removal is put into resistance furnace, is to be warming up to 1100 ℃～1200 ℃ under the condition of 10 ℃/min～50 ℃/min at heating rate, is incubated 1～2 hour, obtains the SiC precast body with the stove cooling then;
(4) aluminium block, MAG block and silico briquette are placed the induction furnace melting by mass ratio at 100: 8: 13, the cooling back forms alloy, and alloy is cut into piece;
(5) alloy that cuts into piece in the step (4) is placed corundum crucible, put into the resistance furnace heat fused then, obtain the alloy liquation; SiC precast body described in the step (3) is preheated to 700 ℃～800 ℃ in another resistance furnace; SiC precast body after the preheating is put into the alloy liquation rapidly infiltrate, add by SiO simultaneously
2Powder and CaF
2The slag former that powder mixes by mass ratio 1: 1～5; form the fine and close slag blanket of one deck at the alloy molten surface in order to protection alloy liquation; be warming up to 850 ℃～950 ℃ then rapidly; and be incubated 1～3 hour; treat to remove when the alloy liquation is cooled to 680 ℃ the fine and close slag blanket of alloy molten surface; the SiC precast body is taken out from the alloy liquation, and cooling promptly obtains the SiC/Al composite.
2. the preparation method of a kind of used for electronic packaging SiC/Al composite according to claim 1 is characterized in that, polyvinyl alcohol water solution and SiO described in the step (1)
2The volume ratio of colloidal sol is 1: 1～2.
3. the preparation method of a kind of used for electronic packaging SiC/Al composite according to claim 1, it is characterized in that β described in the step (2)-SiC particle is that β-SiC of 50 μ m and β-SiC that granularity is 10 μ m mix by mass ratio 10: 1～3 by granularity; The mass ratio of binding agent and β-SiC particle is 3～5: 100 described in the step (2).
4. the preparation method of a kind of used for electronic packaging SiC/Al composite according to claim 1 is characterized in that, the porosity of SiC precast body is 30%～42% described in the step (3).
5. the preparation method of a kind of used for electronic packaging SiC/Al composite according to claim 1, it is characterized in that, the quality purity of aluminium block is 99.7% described in the step (4), the quality purity of MAG block is 99.5%, the quality purity of silico briquette is 99%, the temperature of melting is 1650 ℃, and the time of melting is 5 minutes.
6. the preparation method of a kind of used for electronic packaging SiC/Al composite according to claim 1 is characterized in that, the temperature of fusing is 680 ℃ described in the step (5), and the thickness of fine and close slag blanket is 10mm～20mm.
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| CN103060596A (en) * | 2012-12-17 | 2013-04-24 | 华南理工大学 | Preparation method for SiC reinforced Al-matrix composite material |
| CN103240402B (en) * | 2013-05-17 | 2018-03-09 | 山西银光华盛镁业股份有限公司 | A kind of production method of particle enhanced aluminum-based composite material ingot casting |
| CN104073675B (en) * | 2014-07-01 | 2016-05-18 | 广东省工业技术研究院(广州有色金属研究院) | The preprocess method of silicon-carbide particle for a kind of aluminum matrix composite |
| CN105349817A (en) * | 2015-10-29 | 2016-02-24 | 无锡桥阳机械制造有限公司 | Technology for preparing composite material |
| CN105543576A (en) * | 2015-12-22 | 2016-05-04 | 中国航空工业集团公司北京航空材料研究院 | Electronic encapsulating material |
| CN115161529B (en) * | 2022-06-28 | 2023-06-20 | 广东昭信照明科技有限公司 | Aluminum-based silicon carbide composite material and preparation method and application thereof |
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| CN100449012C (en) * | 2007-03-08 | 2009-01-07 | 北京科技大学 | Method of preparing SiCp/Al composite material with complicated shape and high volume percent ratio |
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