CN108866360A - A kind of preparation method of Al-Si composites used for electronic packaging - Google Patents
A kind of preparation method of Al-Si composites used for electronic packaging Download PDFInfo
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- CN108866360A CN108866360A CN201810776288.XA CN201810776288A CN108866360A CN 108866360 A CN108866360 A CN 108866360A CN 201810776288 A CN201810776288 A CN 201810776288A CN 108866360 A CN108866360 A CN 108866360A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/12—Making non-ferrous alloys by processing in a semi-solid state, e.g. holding the alloy in the solid-liquid phase
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/02—Alloys based on aluminium with silicon as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
- C22F1/043—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with silicon as the next major constituent
Abstract
The invention discloses a kind of preparation methods of Al-Si composites used for electronic packaging, it is characterised in that includes the following steps：S1：It prepares fine aluminium and pure silicon, melting alusil alloy obtains Al-Si alloy melt；S2：Gas-atomized powder is carried out to Al-Si alloy melt, screening obtains alusil alloy powder；S3：Cold moudling is carried out to alusil alloy powder, obtains alusil alloy green compact；S4：Semi-solid forming is carried out to the alusil alloy powder compact after cold pressing, obtains Al-Si composites；S5：Al-Si composites are made annealing treatment.The Al-Si composites used for electronic packaging prepared using the method for the present invention, silicon phase size is tiny, silicon phase corner angle are passivated, and is uniformly distributed in aluminum substrate, has good Microstructure characteristics and comprehensive performance.
Description
Technical field
The present invention relates to the processing and forming fields of electronic package material, and in particular to a kind of aluminium silicon composite wood used for electronic packaging
The preparation method of material.
Background technique
Conditional electronic encapsulating material mainly includes Cu, Al, Ti, Kovar (or Invar), W/Cu (or Mo/Cu), Al2O3Deng,
Its main performance is as shown in table 1.As modern electronic devices are to miniaturization, lightweight, high working frequency, high power density, more
The directions such as function and high reliability are developed, conventional encapsulant heating conduction, matched coefficients of thermal expansion and in terms of
It has been difficult to be competent at.
Table 1 often uses electronic package material main performance
To meet requirement of the modern high integration electronic device to material property, western developed country fabric study and exploitation
A variety of electronic package materials, wherein acieral and composite material, mainly aluminum silicon carbide composite material and alusil alloy
Development and application are very fast.The function admirables such as the mechanical performance of aluminum silicon carbide composite material, thermally conductive, thermal expansion, therefore obtain a large amount of
Research and development, such as number of patent application 201110327434.9,201410308106.8.But aluminum silicon carbide composite material
Laser welding, coating surface and machining are difficult, limit the application of aluminum silicon carbide composite material.Al-Si composites in addition to
With the performances such as same excellent mechanical performance, thermally conductive, thermal expansion, it is also easy to realize machining, coating surface and laser
Welding, becomes the METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING of excellent combination property of new generation, such as United States Patent (USP)：Patent No. 6312535B1,
4917359,6759269B2, Chinese patent：Patent No. 1531072A, 1877821A.
Al-Si composites can obtain the material of different performance by adjusting silicone content according to the requirement of electronic package system
Material, it is controllable with thermal expansion coefficient, density is low, thermal conductivity is high, good conductivity is (with excellent electromagnetic interference/radio frequency interference screen
Cover performance), hardness is high, thermo mechanical stability is excellent, density is small, machinability is good, the protection of easy plating, micro- electricity with standard
Subgroup fills the features such as process compatible, can satisfy the growth requirement of modern electronic devices.
However the Al-Si composites of the prior art, it is general to be prepared using the ingot blank semi-solid forming that founding obtains,
Since the cooling velocity of fusion-casting process is low, coarse primary silicon phase and acicular eutectic silicon are formed in ingot blank, then through semisolid
After molding, this institutional framework can be left in the material after semi-solid forming, to deteriorate the comprehensive performance of material.Therefore,
Existing Al-Si composites used for electronic packaging are usually present the problems such as silicon phase size is coarse, processing performance is low.
Summary of the invention
It is an object of the invention to overcome shortcoming and defect in the prior art, it is compound to provide a kind of aluminium silicon used for electronic packaging
The preparation method of material produces alusil alloy powder using quick solidification gas atomization, silicon phase in powder (including primary crystal and eutectic
Silicon) it is tiny, uniform, Al-Si composites are manufactured by semi-solid forming again after powder cold pressing, it is ensured that the material tool produced
There are good Microstructure characteristics and comprehensive performance.
The present invention is achieved by the following technical solutions：
A kind of preparation method of Al-Si composites used for electronic packaging, it is characterised in that include the following steps：
S1：It prepares fine aluminium and pure silicon, melting alusil alloy obtains Al-Si alloy melt；
S2：Gas-atomized powder is carried out to Al-Si alloy melt, screening obtains alusil alloy powder；
S3：Cold moudling is carried out to alusil alloy powder, obtains alusil alloy green compact；
S4：Semi-solid forming is carried out to the alusil alloy powder compact after cold pressing, obtains Al-Si composites；
S5：Al-Si composites are made annealing treatment.
Further, high-purity aluminium ingot and monocrystalline silico briquette is respectively adopted in fine aluminium and pure silicon in the S1, and the purity of aluminium ingot is
99.95%, alloying ingredient ingredient is by weight percentage：Silicon is 22~70%, and aluminium is surplus.
Further, the melting of alusil alloy is warming up to 780~860 DEG C first and melts aluminium ingot, after being completely melt rapidly
1200~1600 DEG C are warming up to, the monocrystalline silico briquette for preparing weight is added, 850~1450 DEG C are cooled to after silicon is completely melt.
Preferably, 10~15min is stood after the alusil alloy melting of S1 to carry out again in next step.It is molten to be conducive to alloy in this way
The homogenization of temperature.
Further, the atomization gas of gas-atomized powder is nitrogen in S2, and atomization pressure is 0.8~1.3MPa, sieve
Get the particle no more than 74 μm.
Further, the pressing pressure when cold moudling of S3 is 200~300MPa, and the dwell time is 10~30s.
Further, the temperature of semi-solid forming is 580~800 DEG C in S4.
Preferably, 5~15min, then semi-solid forming, semisolid are kept the temperature in S4 before semi-solid forming at 580~800 DEG C
80~120MPa of briquetting pressure；After semi-solid forming, cooling rate is 30~50 DEG C/min, can be in heating furnace surrounding band water cooling
The mode fast cooling of set, guarantee reduces silicon the case where obtaining compact tissue is mutually roughened rate, so that the performance of alloy is improved,
Especially machining property.
Preferably, the melting of the alusil alloy of S1 use the complex salt slag making of 30%NaCl+47%KCl+23% ice crystal, six
Chlorohexane degasification can reach refining purpose and prevent from introducing impurity；The mold of semi-solid forming uses graphite jig in S4, uses
It is preceding to coat one layer of boron nitride in advance in graphite mold surface, be conducive to demould in this way.
Further, in step S5, the annealing temperature of semi-solid-state shaping alusil alloy is 350~400 DEG C, heat preservation 4~
12h obtains Al-Si composites used for electronic packaging.
The present invention produces alloy powder using quickly solidification gas atomization, silicon phase in alloy powder obtained (including it is first
Brilliant and Eutectic Silicon in Al-Si Cast Alloys) it is tiny, uniform, to guarantee that the alloy that semi-solid forming produces has good microstructure on raw material
Feature.Since the solid liquid phase temperature difference of alusil alloy is very big, eutectic temperature is 577 DEG C, and the fusing point of silicon reaches 1414 DEG C, this
Sample just to the semi-solid forming temperature of this alloy to select to bring very big difficulty.To solve this critical issue, this patent benefit
With aluminium silicon binary alloy phasor and differential thermal analysis, determine specific composition alloy in certain liquid phase (20%~50%) content item
Corresponding temperature range under part.In addition, to guarantee that there is a phenomenon where liquid phases to ooze out in semi-solid forming process for powder compact, this
The matching property for inventing the molding die used is preferable.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) thermal expansion coefficient controllable (7 × 10 of the alusil alloy used for electronic packaging of the method for the present invention preparation-6~20 × 10-6/ K), thermal conductivity it is high (>110W/mK), intensity be higher than 140MPa and density it is low (<2.7g/cm3)；
(2) the method for the present invention preparation silicon from aluminum-silicon alloy phase size used for electronic packaging it is tiny (<30 μm), silicon phase corner angle are blunt
Change, is uniformly distributed in aluminum substrate；
(3) according to the specific requirement of Electronic Packaging box body, alusil alloy used for electronic packaging prepared by the present invention can be used
Machining obtains the exemplar of certain size and shape, and can carry out coating surface and laser welding；
(4) method (powder semi-solid forming) that the present invention prepares alusil alloy used for electronic packaging contains suitable for bigger silicon
It measures range (22%~70%), Electronic Packaging aluminium silicon shell and cover plate materials can be obtained；
(5) it can be applied to the Electronic Packaging material in the fields such as Aeronautics and Astronautics, naval vessel using alusil alloy produced by the present invention
Material.
In order to better understand and implement, the present invention will be described in detail With reference to embodiment.
Detailed description of the invention
Fig. 1 is the preparation process flow of present invention Al-Si composites used for electronic packaging；
Fig. 2 is the Al-50%Si alloy powder macro morphology photo after aerosolization of the invention；
Fig. 3 is the section microstructure photo of the Al-50%Si alloy powder after aerosolization of the invention.
Specific embodiment
It is multiple to aluminium silicon used for electronic packaging provided by the invention combined with specific embodiments below for a further understanding of the present invention
The preparation method of condensation material is described in detail, and protection scope of the present invention is not limited by the following examples.Fig. 1 is the present invention
The preparation process flow of Al-Si composites used for electronic packaging.
Embodiment 1
The preparation method of Al-22%Si electronic packaging composite material, includes the following steps：
(1) raw material is monocrystalline silicon, fine aluminium (purity 99.95%), and alloying component carries out ingredient by weight percentage, ingredient at
It is divided into：Silicon：22%, aluminium：78%；
(2) in intermediate frequency furnace, 780 DEG C is warming up to and melts aluminium, is brought rapidly up after being completely melt to 1200~1350
DEG C, the silicon for preparing weight is added, 5~15min is sufficiently stirred using graphite rod, by 30%NaCl+47%KCl+23% ice crystal
It is placed in graphite cover, protrudes into melt bottom and carry out slag making, and with hexachlorethane degasification, be cooled to 850~950 DEG C, and stand
10min；
(3) tundish crucible and keeps the temperature 30min using resistance heating to 700~800 DEG C, and alloy melt poured into
Between packet crucible, open atomization gas source, be atomized by atomizer, gas pressure is 0.7~0.9MPa, and draft-tube diameter is
2.5mm；
(4) it is greater than 74 μm of part using particle size in standard screen removal alloy powder, vacuum packaging is saved to prevent
Oxidation and water suction；
(5) by load weighted alloy powder, on 400t hydraulic press, 50 millimeters of diameter of green compact is cold-pressed into using punching block,
Pressing pressure is 200MPa, dwell time 10s；
(6) alloy powder green compact is placed in graphite jig, under inert gas shielding, powder compact is warming up to 580~620
DEG C, apply 80MPa pressure, and heat-insulation pressure keeping 5min after keeping the temperature 10min, by mechanical pressure by powder compact in semi-solid state
Block Al-22%Si alloy material is made with 30 DEG C/min cooling after molding in lower molding；
(7) alloy is placed in chamber type electric resistance furnace, is warming up to 340 DEG C with 15 DEG C/min, constant temperature keeps the temperature 6h, after heat preservation
It cools to 150~200 DEG C with the furnace, is air-cooled to room temperature later, that is, produce aluminium silicon Electronic Packaging alloy.
It is detected by structure property, using in the Al-22%Si alloy of alloy powder semi-solid forming, silicon is mutually with tiny
Particle is uniformly distributed in aluminum substrate, and the thermal expansion coefficient of alloy is 20.1 ± 0.5 × 10-6/ K, thermal conductivity are 180 ± 15W/
MK, tensile strength are 153 ± 12MPa, density 2.60g/cm3, plating performance and welding performance are excellent.
Embodiment 2
The preparation method of Al-50%Si electronic packaging composite material, include the following steps：
(1) raw material is monocrystalline silicon, fine aluminium (purity 99.95%), and alloying component carries out ingredient by weight percentage, ingredient at
It is divided into：Silicon：50%, aluminium：50%；
(2) in intermediate frequency furnace, 860 DEG C is warming up to and melts aluminium, is brought rapidly up after being completely melt to 1300~1450
DEG C, the silicon for preparing weight is added, 5~15min is sufficiently stirred using graphite rod, by 30%NaCl+47%KCl+23% ice crystal
It is placed in graphite cover, protrudes into melt bottom and carry out slag making, and with hexachlorethane degasification, be cooled to 950~1100 DEG C, and stand
15min；
(3) tundish crucible and keeps the temperature 30min using resistance heating to 750~850 DEG C, and alloy melt poured into
Between packet crucible, open atomization gas source, be atomized by atomizer, gas pressure is 0.9~1.2MPa, and draft-tube diameter is
3.2mm；
(4) it is greater than 74 μm of part using particle size in standard screen removal alloy powder, vacuum packaging is saved to prevent
Oxidation and water suction；
(5) by load weighted alloy powder, on 400 t hydraulic press, 50 millimeters of diameter of green compact is cold-pressed into using punching block,
Pressing pressure is 250MPa, dwell time 20s；
(6) alloy powder green compact is placed in graphite jig, under inert gas shielding, powder compact is warming up to 600~700
DEG C, apply 100MPa pressure, and heat-insulation pressure keeping 5min after keeping the temperature 12min, by mechanical pressure by powder compact in semisolid shape
It is formed under state, with 50 DEG C/min cooling after molding, block of aluminum silicon alloy material is made.
(7) block alloy is placed in chamber type electric resistance furnace, is warming up to 375 DEG C with 15 DEG C/min, constant temperature keeps the temperature 6h, heat preservation knot
It cools to 150~200 DEG C after beam with the furnace, is air-cooled to room temperature later, that is, produce aluminium silicon Electronic Packaging alloy.
It is detected by structure property, using in the Al-50%Si alloy of alloy powder semi-solid forming, silicon is mutually with network-like
Structure is uniformly distributed in aluminum substrate, and the thermal expansion coefficient of alloy is 11.5 ± 0.5 × 10-6/ K, thermal conductivity are 147 ± 14W/
MK, tensile strength are 185 ± 18MPa, density 2.49g/cm3, plating performance and welding performance are excellent.
Embodiment 3
The preparation method of Al-70%Si electronic packaging composite material, includes the following steps：
(1) raw material is monocrystalline silicon, rafifinal (purity 99.95%), and alloying component carries out ingredient, ingredient by weight percentage
Ingredient is：Silicon：70%, aluminium：30%；
(2) in intermediate frequency furnace, 810 DEG C is warming up to and melts aluminium, is brought rapidly up after being completely melt to 1400~1600
DEG C, the silicon for preparing weight is added, 5~15min is sufficiently stirred using graphite rod, by 30%NaCl+47%KCl+23% ice crystal
It is placed in graphite cover, protrudes into melt bottom and carry out slag making, and with hexachlorethane degasification, be cooled to 1300~1450 DEG C, and stand
12min；
(3) tundish crucible and keeps the temperature 30min using resistance heating to 800~900 DEG C, and alloy melt poured into
Between packet crucible, open atomization gas source, be atomized by atomizer, gas pressure is 0.9~1.3MPa, and draft-tube diameter is
4.0mm；
(4) it is greater than 74 μm of part using particle size in standard screen removal alloy powder, vacuum packaging is saved to prevent
Oxidation and water suction；
(5) by load weighted alloy powder, on 400t hydraulic press, it is cold-pressed into the green compact of diameter 50mm using punching block, presses
Pressing pressure is 300MPa, dwell time 30s；
(6) alloy powder green compact is placed in graphite jig, under inert gas shielding, powder compact is warming up to 750~850
DEG C, apply 120MPa pressure, and heat-insulation pressure keeping 15min after keeping the temperature 15min, by mechanical pressure by powder compact in semisolid shape
It is formed under state, with 40 DEG C/min cooling after molding, block of aluminum silicon alloy material is made.
(7) block alloy is placed in chamber type electric resistance furnace, is warming up to 400 DEG C with 15 DEG C/min, constant temperature keeps the temperature 8h, heat preservation knot
It cools to 150~200 DEG C after beam with the furnace, is air-cooled to room temperature later, that is, produce aluminium silicon Electronic Packaging alloy.
It is detected by structure property, using in the Al-70%Si alloy of alloy powder semi-solid forming, silicon is mutually with network-like
Structure is uniformly distributed in aluminum substrate, and the thermal expansion coefficient of alloy is 7.2 ± 0.5 × 10-6/ K, thermal conductivity are 113 ± 12W/m
K, tensile strength are 176 ± 22MPa, density 2.42g/cm3, plating performance and welding performance are excellent.
The invention is not limited to above embodiment, if not departing from the present invention to various changes or deformation of the invention
Spirit and scope, if these changes and deformation belong within the scope of claim and equivalent technologies of the invention, then this hair
It is bright to be also intended to encompass these changes and deformation.
Claims (10)
1. a kind of preparation method of Al-Si composites used for electronic packaging, it is characterised in that include the following steps：
S1：It prepares fine aluminium and pure silicon, melting alusil alloy obtains Al-Si alloy melt；
S2：Gas-atomized powder is carried out to Al-Si alloy melt, screening obtains alusil alloy powder；
S3：Cold moudling is carried out to alusil alloy powder, obtains alusil alloy green compact；
S4：Semi-solid forming is carried out to the alusil alloy powder compact after cold pressing, obtains Al-Si composites；
S5：Al-Si composites are made annealing treatment.
2. the preparation method of Al-Si composites used for electronic packaging according to claim 1, it is characterised in that：In the S1
High-purity aluminium ingot and monocrystalline silico briquette is respectively adopted in fine aluminium and pure silicon, and the purity of aluminium ingot is 99.95%, alloying ingredient ingredient by weight hundred
Divide than meter：Silicon is 22~70%, and aluminium is surplus.
3. the preparation method of Al-Si composites used for electronic packaging according to claim 2, it is characterised in that：Alusil alloy
Melting be warming up to 780~860 DEG C first and melt aluminium ingot, be brought rapidly up after being completely melt to 1200~1600 DEG C, addition is matched
The monocrystalline silico briquette of good weight, is cooled to 850~1450 DEG C after silicon is completely melt.
4. the preparation method of Al-Si composites used for electronic packaging according to claim 3, it is characterised in that：The aluminium silicon of S1
10~15min is stood after alloy melting to carry out again in next step.
5. the preparation method of Al-Si composites used for electronic packaging according to claim 1, it is characterised in that：Aerosol in S2
The atomization gas for changing powder processed is nitrogen, and atomization pressure is 0.8~1.3MPa, and screening obtains the particle no more than 74 μm.
6. the preparation method of Al-Si composites used for electronic packaging according to claim 2, it is characterised in that：The cold pressing of S3
Pressing pressure when molding is 200~300MPa, and the dwell time is 10~30s.
7. the preparation method of Al-Si composites used for electronic packaging according to claim 1, it is characterised in that：Half is solid in S4
The molding temperature of state is 580~800 DEG C.
8. the preparation method of Al-Si composites used for electronic packaging according to claim 7, it is characterised in that：Half is solid in S4
5~15min, then semi-solid forming, 80~120MPa of semi-solid forming pressure are kept the temperature at 580~800 DEG C before state molding；Half is solid
After state molding, cooling rate is 30~50 DEG C/min.
9. the preparation method of Al-Si composites used for electronic packaging according to claim 1, it is characterised in that：The aluminium silicon of S1
The melting of alloy uses the complex salt slag making of 30%NaCl+47%KCl+23% ice crystal, hexachlorethane degasification；In S4 semisolid at
The mold of type uses graphite jig, coats one layer of boron nitride in advance in graphite mold surface using preceding.
10. the preparation method of Al-Si composites used for electronic packaging according to claim 1, it is characterised in that：Step S5
In, the annealing temperature after semi-solid-state shaping is 350~400 DEG C, keeps the temperature 4~12h, obtains Al-Si composites used for electronic packaging.
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|---|---|---|---|---|
| CN101440440A (en) * | 2008-12-19 | 2009-05-27 | 江苏技术师范学院 | Aluminum based composite material and method and apparatus for forming aluminum based composite material part |
| JP4391999B2 (en) * | 2006-03-24 | 2009-12-24 | 日精樹脂工業株式会社 | Method for producing composite metal molding material and method for producing composite metal molded product |
| CN102978485A (en) * | 2011-09-07 | 2013-03-20 | 长沙华希金属材料有限公司 | Novel high-silicon aluminum alloy electronic packaging material and preparation method thereof |
| CN103639413A (en) * | 2013-12-06 | 2014-03-19 | 莱芜职业技术学院 | Method for manufacturing high-performance complex aluminum alloy part |
| CN106086544A (en) * | 2016-08-08 | 2016-11-09 | 中南大学 | A kind of alloying element strengthens high aluminium silicon composite material and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4391999B2 (en) * | 2006-03-24 | 2009-12-24 | 日精樹脂工業株式会社 | Method for producing composite metal molding material and method for producing composite metal molded product |
| CN101440440A (en) * | 2008-12-19 | 2009-05-27 | 江苏技术师范学院 | Aluminum based composite material and method and apparatus for forming aluminum based composite material part |
| CN102978485A (en) * | 2011-09-07 | 2013-03-20 | 长沙华希金属材料有限公司 | Novel high-silicon aluminum alloy electronic packaging material and preparation method thereof |
| CN103639413A (en) * | 2013-12-06 | 2014-03-19 | 莱芜职业技术学院 | Method for manufacturing high-performance complex aluminum alloy part |
| CN106086544A (en) * | 2016-08-08 | 2016-11-09 | 中南大学 | A kind of alloying element strengthens high aluminium silicon composite material and preparation method thereof |
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Application publication date: 20181123 |
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| RJ01 | Rejection of invention patent application after publication |