CN103160716B - Low-heat-expansion high-intensity alumina-silicon-aluminum (AlN-Si-Al) mixed composite material and preparation method thereof - Google Patents
Low-heat-expansion high-intensity alumina-silicon-aluminum (AlN-Si-Al) mixed composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a low-heat-expansion high-intensity alumina-silicon-aluminum (AlN-Si-Al) mixed composite material and a preparation method thereof. The AlN-Si-Al mixed composite material comprises 10wt% to 25wt% of AlN, 40 wt% to 45 wt% of Si and 30 wt% to 50 wt% of Al, wherein the AlN and the Si are used as reinforcing materials and distributed in a continuous aluminum substrate in the form of particles in a dispersive mode, so that a reinforced aluminium base composite material mixed with AlN particles and Si particles is formed. The AlN-Si-Al mixed composite material is prepared by adoption of a powder metallurgy preparation process. The low-heat-expansion high-intensity AlN-Si-Al mixed composite material has low heat expansion and high intensity. The composite material is uniform in microstructure, completely compact and of a good machining process performance. The AlN-Si-Al mixed composite material is expected to be a substitute material of a high-silicon-content Si/Al packaging material and a substitute material of high-silicon-carbide (SiC)-content SiC/Al packaging material.
Description
Technical field
The present invention relates to and a kind ofly comprise hybrid composite of aluminium, silicon and aluminium nitride and preparation method thereof, particularly a kind of AlN-Si-Al hybrid composite with low-thermal-expansion and high strength and preparation method thereof, belongs to metal-base composites technical field.
Background technology
Aluminum matrix composite has the over-all properties advantages such as specific tenacity is high, specific rigidity is high, thermal conductivity is high, thermal expansivity is adjustable, thus obtains important application at aerospace, microelectronics and field of traffic.Aluminum matrix composite adopts particle or the whiskers such as silicon carbide, aluminum oxide, silicon, aluminium nitride, norbide mostly, and fiber etc. is as strongthener.Wherein, silicon is the desirable strongthener of a kind of lightweight, low-thermal-expansion, high strength; Density (the 2.33g/cm of silicon
3) lower than aluminium alloy by 14%, it has the extremely low coefficient of expansion (2.6 × 10
-6k
-1), higher thermal conductivity and Young's modulus, silicon has good process for machining and manufacturing performance compared with other several ceramic reinforcing materials, therefore aluminium silicon composite material (Si/Al) obtains great attention in the nearest more than ten years, most is representational is take microelectronics Packaging as the low-gravity of application background, low bulk, high heat conduction, high silicon content Si/Al matrix material (volumn concentration of silicon is 40wt.% ~ 75wt.%), its processing and preparation technology's window relatively wide, abroad part realize through engineering approaches apply.But over-all properties and the manufacturing property of Si/Al matrix material prepared at present are still difficult to meet application demand.Thermal expansivity is that Si/Al encapsulates one of performance index of matrix material most critical, and for 60vol% ~ 70vol%Si/Al, its thermal expansivity is 7.5 ~ 10.5 × 10
-6ppm/K, but due to material main component be hard fragility silicon, and material internal unavoidably causes the process for machining poor-performing of material containing the factor such as defectiveness, be difficult to the precision manufactureing requirement meeting small size, thin-wall construction electronic encapsulation shell part; Reduce the obdurability that silicone content can promote matrix material, improve machining characteristics, but the thermal expansivity of matrix material increases, the index request of packaged piece cannot be met.
Aluminium nitride (AlN) is also one of conventional ceramic reinforcing material, and AlN has the advantages such as high heat conduction, high-modulus, low bulk.AlN is as strongthener, and the effect of its activeness and quietness and the thermal expansion of reduction alumina-base material is all good than Si, but AlN belongs to covalent linkage compound, powder sintered poor performance, and nonwetting with metallic aluminium, the difficulty preparing the AlN/Al matrix material of high AlN content is larger.Adopt the Al based composites that the thermal expansivity of the Al based composites of AlN and Si hybrid buildup should strengthen lower than the single Si of employing, and the density of AlN-Si-Al is only 2.55 ~ 2.7g/cm
3, be starkly lower than the 55% ~ 70%SiC/Al electronic packaging composite material obtaining application; The preparation and fabrication manufacturability of this matrix material is better than AlN/Al and SiC/Al.Preparation AlN-Si-Al hybrid composite is one of new way realizing Advanced Electronic Encapsulating material low-gravity, low-thermal-expansion and high strength over-all properties.
Summary of the invention
Main purpose of the present invention is the AlN-Si-Al hybrid composite providing a kind of low-thermal-expansion and high strength, and this material height is fine and close, homogeneous microstructure.
Above-mentioned purpose of the present invention reaches by the following technical programs:
The AlN-Si-Al hybrid composite of a kind of low-thermal-expansion and high strength; its weight percent consists of: AlN:10wt.% ~ 25wt.%; Si:40wt.% ~ 45wt.%; Al:30wt.% ~ 50wt.%; wherein; AlN and Si as strongthener in granular form even dispersion be distributed in continuous print aluminum substrate, form the aluminum matrix composite that AlN particle and Si confusion strengthen.Powder metallurgical technique can be adopted to prepare, and obtained matrix material has uniform microtexture and densification completely.
In order to realize the lower thermal expansivity of matrix material, the weight percent sum of AlN and Si enhanced granule is selected between 50wt.% ~ 70wt.%; In order to the machinability keeping matrix material good, the content of AlN is no more than 30wt.%.
In order to select rational enhanced granule size to meet the high strength requirement of matrix material, preferred Si particle and the ratio of the particle mean size of AlN are greater than or close to 2, such as be more than or equal to 1.75, to make undersized AlN particles filled to large-sized Si particulate interspaces, make when particle total content is determined, at utmost improve Granular composite homogeneity; Preferred AlN particle mean size is selected between 3 μm ~ 20 μm, and Si particle mean size is selected between 5 μm ~ 50 μm.
When the total content of AlN particle and Si particle is more than 50wt.%, in AlN-Si-Al mixed powder, the mean particle size of Al powder is preferably not more than the mean particle size of Si powder or the mean particle size of AlN powder, and the median size of Al powder is selected between 3 μm ~ 20 μm.
Another object of the present invention is to provide a kind of preparation technology, the AlN-Si-Al matrix material adopting this technique to prepare has low thermal coefficient of expansion, high strength; Obtained composite machine process industrial art performance is good, and conventional machining means can be adopted to be processed into containing thin-walled, the isostructural microelectronic package of aperture.
The preparation method of the AlN-Si-Al hybrid composite of low-thermal-expansion and high strength, based on powder metallurgy preparation technique, by selecting the content of suitable AlN and Si enhanced granule, select rational powder particle size proportioning, control powder consolidation and densification process prepare described low-thermal-expansion, high strength AlN-Si-Al hybrid composite billet, and concrete implementation step is as follows.
A preparation method for the AlN-Si-Al hybrid composite of low-thermal-expansion and high strength, adopts powder metallurgy preparation technique, comprises the steps:
(1) Al powder, AlN powder and Si powder are respectively AlN:10wt.% ~ 25wt.% according to the massfraction accounting for above-mentioned three kinds of total mixed powders, Si:40wt.% ~ 45wt.%, Al:30wt.% ~ 50wt.%, batching also Homogeneous phase mixing makes AlN-Si-Al mixed powder;
(2) gained mixed powder is carried out cold isostatic compaction and make isostatic cool pressing blank;
(3) isostatic cool pressing blank is carried out vacuum hotpressing densification, obtain fully dense AlN-Si-Al hybrid composite billet;
(4) the matrix material billet of vacuum hotpressing densification is formed Electronic Packaging parts through conventional mechanical workout.
In above-mentioned steps (1), in order to realize the lower thermal expansivity of matrix material, the low bulk meeting Electronic Packaging requires (thermal expansivity of electronic encapsulation shell material is generally at 6.0 ~ 13.0ppm/K), the weight percent of enhanced granule is selected between 50wt.% ~ 70wt.%, and namely the weight percent sum of preferred AlN and Si enhanced granule is between 50wt.% ~ 70wt.%.
In above-mentioned steps (1), in order to select rational enhanced granule size to meet the high strength requirement of matrix material, preferred Si particle and the ratio of the particle size of AlN are greater than or close to 2, such as be more than or equal to 1.75, the median size (particle mean size) of AlN powder is 3 μm ~ 20 μm, and the median size of Si powder is 5 μm ~ 50 μm.
In above-mentioned steps (1); the size ratio of Al powder and Si powder and AlN powder must appropriately be selected; AlN powder particles and Si powder particles can be similar to be uniformly distributed in pure aluminium powder with monodispersed form, avoids the reunion that there is AlN powder particles or Si powder particles.The selection gist of this size ratio is: because the total content of AlN particle and Si particle is more than 50wt.%, in AlN-Si-Al mixed powder, the mean particle size of Al powder must be not more than the mean particle size of Si powder or the mean particle size of AlN powder, and the median size of Al powder is selected between 3 μm ~ 20 μm.
In above-mentioned steps (1), preferably, the purity of Al powder is the purity of more than 99.8wt.%, Si powder is more than 99.9wt.%.
In above-mentioned steps (2), pressure 100 ~ the 200MPa of described cold isostatic compaction, the time of cold isostatic compaction is 10 ~ 30 minutes, and isostatic cool pressing blank (base of the colding pressing) relative density that cold isostatic compaction obtains is 67% ~ 75% (relative density is the ratio of actual density and theoretical density).Mixed powder can be selected to be packaged in rubber jacket carry out cold isostatic compaction.
In above-mentioned steps (3), isostatic cool pressing blank is loaded in steel die and carries out vacuum hotpressing densification.
In above-mentioned steps (3), the blank of cold isostatic compaction is carried out vacuum hotpressing densification, the selection of densification temperature is most important for the complete densification of AlN-Si-Al hybrid composite.In order to form Al-Si and Al-AlN metallurgical interfaces, appropriate temperature must be selected on Al-Si aluminium alloy phase line used, the primary particle interface that pure Al powder and Si powder are contacted with each other produces a small amount of alloy liquid phase, liquid phase is fully filled starting powder particulate interspaces, has formed fully dense matrix material billet.
Described vacuum hotpressing densification is that isostatic cool pressing blank is carried out heat-insulation pressure keeping process at selected temperature and pressure; Described vacuum hotpressing densification temperature is selected within the scope of 575 DEG C ~ 600 DEG C, and hot pressing pressure is 75 ~ 120MPa, and the heat-insulation pressure keeping time is 3 hours.
In above-mentioned steps (3), vacuum tightness in the heat-insulation pressure keeping process of described vacuum hotpressing densification, in hot pressing furnace, must be kept not higher than 2 × 10
-2pa, to remove the entrap bubble in powder particle gap completely.
In above-mentioned step (4), any one or a few in the car that the mechanical workout used is routine, milling, brill, mill and spark cutting.
The present invention has the following advantages:
(1) adopt high-modulus, high rigidity, low-thermal-expansion AlN particle and hardness is moderate, the Si particle of low-gravity, low-thermal-expansion as strongthener, prepared AlN-Si-Al hybrid buildup matrix material has low-thermal-expansion, high strength and good process for machining performance.
(2) adopt powder metallurgical technique, can in whole composition range the content of accurate control Si and AlN, the thermal expansivity of accuracy controlling matrix material.
(3) by selecting fine powder to be directly mixed and made into mixed powder, Al powder, Si powder and AlN powder fully being mixed at micro-meter scale, fundamentally avoids particle agglomeration to occur.
(4) because AlN belongs to covalent linkage compound, its powder is difficult to carry out low-temperature sintering densification, therefore when there is part Si powder, select suitable consolidation technique, appropriately utilize Al-Si eutectic reaction feature, promote the metallurgical bonding interface forming Al-Si and Al-AlN, promote Si particle and AlN particle re-arrangement, made fully dense matrix material billet.
(5) technique that the present invention realizes is different from casting, liquid infiltration or in-situ method, can prepare the AlN-Si-Al hybrid composite with different size microtexture by simple powder size.
AlN-Si-Al hybrid composite of the present invention is expected to the equivalent material becoming high silicon content Si/Al and high SiC content SiC/Al packaged material.The powder metallurgic method being used for preparing AlN-Si-Al hybrid composite in the present invention is liquid process, there is very strong designability, possessing and realize the potentiality that through engineering approaches is produced and batch is applied, is one of technique developing AlN-Si-Al hybrid composite used for electronic packaging, high-performance, structure property are stable and other types height granule content aluminum matrix composite most competitive power.
The present invention is directed to the aluminum matrix composite used for electronic packaging with broad prospect of application, provide a kind of AlN particle and the enhancing of Si confusion, the aluminum matrix composite with low-thermal-expansion (thermal expansivity of 20 DEG C ~ 100 DEG C is 7.0 ~ 10.5ppm/K) and high strength (bending strength is 395MPa ~ 450MPa) and preparation method thereof.In low-thermal-expansion of the present invention, high strength AlN-Si-Al hybrid composite, AlN and Si is evenly distributed in continuous print aluminum substrate as strongthener all in granular form, forms the aluminum matrix composite of AlN particle and the enhancing of Si confusion.Matrix material microtexture evenly, completely fine and close and there is good process for machining performance.
Below by embodiment and accompanying drawing, the present invention will be further described, but do not mean that limiting the scope of the invention.
Accompanying drawing explanation
Fig. 1 is 10wt.%AlN-40wt.%Si-Al mixed powder stereoscan photograph.
Fig. 2 is 25wt.%AlN-45wt.%Si-Al mixed powder stereoscan photograph.
Embodiment
Embodiment 1
Hybrid composite prepared by the present embodiment is 10wt.%AlN-40wt.%Si-Al, and namely the content of AlN is the content of 10wt.%, Si be 40wt.%Si, Al content is 50wt.%.Its preparation method adopts following technical scheme:
By pure Al powder, AlN powder and the Si powder mass ratio 5: 1: 4 according to three kinds of powder, in taper mixing tank, Homogeneous phase mixing makes AlN-Si-Al mixed powder, the Granular composite feature of mixed powder as shown in Figure 1, to make the massfraction of AlN for 10wt.%, the massfraction of Si is 40wt.%, adopt φ 5mm Stainless Steel Ball as mixed powder medium, ratio of grinding media to material is 1: 1, and the mixed powder time is 14 hours; The median size (namely d0.5 is less than this size more than the powder diameter of 50wt.%) of described pure Al powder, AlN powder and Si powder is respectively 8.5 μm, 9 μm, 15 μm; Loaded by mixed powder and be of a size of cold isostatic compaction in the rubber jacket of φ 90mm × 260mm, pressure is 200MPa, pressurize 20 minutes, and billet relative density of colding pressing is 74%; It is carry out vacuum hotpressing densification in the steel die of φ 75mm × 220mm that the blank of cold isostatic compaction is loaded inner cavity size, has obtained fully dense matrix material billet; Vacuum hotpressing temperature is 575 DEG C, and pressure is 75MPa, heat-insulation pressure keeping 3 hours, to keep in stove vacuum tightness 5 × 10 between soak
-3pa ~ 2 × 10
-2between Pa.The density of hot pressing billet exceedes theoretical density, obtains the billet that physical dimension is φ 70mm × 160mm, any surface finish after simple machining.
After vacuum hotpressing densification, the actual density of 10wt.%AlN-40wt.%Si-Al is 2.60.g/cm
3, room temperature three-point bending strength and tensile strength are respectively 450MPa and 280MPa, and the thermal expansivity of 20 DEG C ~ 100 DEG C is 10.5ppm/K.
Embodiment 2
Hybrid composite prepared by the present embodiment is 25wt.%AlN-45wt.%Si-Al, and namely the content of AlN is the content of 25wt.%, Si be 45wt.%Si, Al content is 30wt.%.Its preparation method adopts following technical scheme:
By pure Al powder, AlN powder and the Si powder mass ratio 1.2: 1: 1.8 according to three kinds of powder, in taper mixing tank, Homogeneous phase mixing makes AlN-Si-Al mixed powder (the Granular composite feature of mixed powder as shown in Figure 2), to make the massfraction of AlN for 25wt.%, the massfraction of Si is 45wt.%, adopt φ 5mm Stainless Steel Ball as mixed powder medium, ratio of grinding media to material is 1: 1, and the mixed powder time is 20 hours; The median size of described pure Al powder, AlN powder and Si powder is respectively 3 μm, 4.5 μm, 9 μm; Loaded by mixed powder and be of a size of cold isostatic compaction in the rubber jacket of φ 84mm × 260mm, pressure is 200MPa, pressurize 20 minutes, and the relative density of isostatic cool pressing blank is 69%; It is carry out vacuum hotpressing densification in the steel die of φ 75mm × 220mm that the blank of cold isostatic compaction is loaded inner cavity size, has obtained fully dense matrix material billet; Vacuum hotpressing temperature is 600 DEG C, and pressure is 120MPa, heat-insulation pressure keeping 3 hours, to keep in stove vacuum tightness 5 × 10 between soak
-3pa ~ 2 × 10
-2between Pa.The density of hot pressing billet exceedes theoretical density, obtains the billet that physical dimension is φ 70mm × 150mm, any surface finish after simple machining.
After vacuum hotpressing densification, the actual density of 25wt.%AlN-45wt.%Si-Al is 2.65.g/cm
3, room temperature three-point bending strength and tensile strength are respectively 395MPa and 225MPa, and the thermal expansivity of 20 DEG C ~ 100 DEG C is 7.0ppm/K.
Can select in the present invention to adopt median size to be Al powder and the AlN powder of 3 μm ~ 20 μm, median size is the Si powder of 5 μm ~ 50 μm.The purity of Al powder can select more than 99.8wt.%, more than the purity 99.9wt.% of Si powder.The AlN-Si-Al hybrid composite prepared by the inventive method, the thermal expansivity of 20 DEG C ~ 100 DEG C is 7.0 ~ 10.5ppm/K, and bending strength is 395MPa ~ 450MPa, has the feature of low-thermal-expansion and high strength.
Claims (7)
1. a low-thermal-expansion and high strength AlN-Si-Al hybrid composite, it is characterized in that, its weight percent consists of: AlN:10wt.% ~ 25wt.%, Si:40wt.% ~ 45wt.%, Al:30wt.% ~ 50wt.%, wherein, the particle mean size of described AlN is 3 μm ~ 20 μm, the particle mean size of Si is 5 μm ~ 50 μm, and the ratio of the particle mean size of Si and AlN is more than or equal to 1.75, the particle mean size of described Al is 3 μm ~ 20 μm, and the particle mean size of Al is not more than the particle mean size of Si or AlN, AlN and Si as strongthener in granular form Dispersed precipitate in continuous print aluminum substrate, form the aluminum matrix composite of AlN particle and the enhancing of Si confusion.
2. low-thermal-expansion according to claim 1 and high strength AlN-Si-Al hybrid composite, is characterized in that: the weight percent sum of described AlN and Si is 50wt.% ~ 70wt.%.
3. the preparation method of the low-thermal-expansion described in claim 1 or 2 and high strength AlN-Si-Al hybrid composite, comprises the steps:
(1) by Al powder, AlN powder and Si powder according to weight percent batching and Homogeneous phase mixing make AlN-Si-Al mixed powder;
(2) gained mixed powder is carried out cold isostatic compaction and make isostatic cool pressing blank, the pressure of described cold isostatic compaction is 100 ~ 200MPa, the time of cold isostatic compaction is 10 ~ 30 minutes, and the relative density of described isostatic cool pressing blank is 67% ~ 75%;
(3) carry out vacuum hotpressing densification by isostatic cool pressing blank loading steel die, described vacuum hotpressing densification temperature is 575 DEG C ~ 600 DEG C, and hot pressing pressure is 75 ~ 120MPa, has obtained fully dense AlN-Si-Al hybrid composite billet;
(4) by the matrix material billet machined formation Electronic Packaging parts of vacuum hotpressing densification.
4. the preparation method of low-thermal-expansion according to claim 3 and high strength AlN-Si-Al hybrid composite, is characterized in that: the purity of described Al powder is the purity of more than 99.8wt.%, Si powder is more than 99.9wt.%.
5. the preparation method of low-thermal-expansion according to claim 3 and high strength AlN-Si-Al hybrid composite, is characterized in that: when carrying out vacuum hotpressing densification, and the heat-insulation pressure keeping time is 3 hours.
6. the preparation method of low-thermal-expansion according to claim 5 and high strength AlN-Si-Al hybrid composite, is characterized in that: in described heat-insulation pressure keeping process, keeps vacuum tightness not higher than 2 × 10
-2pa.
7. the preparation method of low-thermal-expansion according to claim 3 and high strength AlN-Si-Al hybrid composite, is characterized in that: described mechanical workout is any one or a few in car, milling, brill, mill and spark cutting.
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| CN1422970A (en) * | 2001-12-06 | 2003-06-11 | 北京有色金属研究总院 | Particle reinforced aluminium-based composite material and manufacture method thereof |
| CN1676644A (en) * | 2005-04-26 | 2005-10-05 | 河北工业大学 | Ceramic granule reinforced aluminium-base composite material and its preparing method |
| CN1718806A (en) * | 2005-07-28 | 2006-01-11 | 上海交通大学 | In situ mixed granula reinforced aluminium base composite material |
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| CN1422970A (en) * | 2001-12-06 | 2003-06-11 | 北京有色金属研究总院 | Particle reinforced aluminium-based composite material and manufacture method thereof |
| CN1676644A (en) * | 2005-04-26 | 2005-10-05 | 河北工业大学 | Ceramic granule reinforced aluminium-base composite material and its preparing method |
| CN1718806A (en) * | 2005-07-28 | 2006-01-11 | 上海交通大学 | In situ mixed granula reinforced aluminium base composite material |
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| 《金属/陶瓷复合材料的原位合成及其结构研究》;朱诚意等;《机械工程材料》;20060131;第30卷(第1期);第33-36页 * |
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