CN100435321C - Process for preparing silumin electronic package materials - Google Patents
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- CN100435321C CN100435321C CNB2006100319084A CN200610031908A CN100435321C CN 100435321 C CN100435321 C CN 100435321C CN B2006100319084 A CNB2006100319084 A CN B2006100319084A CN 200610031908 A CN200610031908 A CN 200610031908A CN 100435321 C CN100435321 C CN 100435321C
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Abstract
The present invention discloses preparation technology of high silumin electronic packing material. The present invention has the preparation technology: powder preparation, commercial pure aluminum and high pure silicon are prepared to Al-Si alloy powder according to the mass percent of 6-8.8: 4-1.2; powder air oxidation treatment technology, the Al-Si alloy powder is arranged in a resistance furnace and warmed up to 250 to 450DEG. C for thermal insulation oxidation for 8-32 hours, and the Al-Si alloy powder is naturally cooled in the air after taken out; hot extrusion technology, the oxidized alloy powder is filled in a pure aluminium wrap and extruded on a hydraulic press of 300 to 500 tons; the temperature of the Al-Si alloy powder is kept from 400 to 520DEG. C for 0.5 to 2 hours before extrusion; the extrusion ratio is from 10 to 21; various extrusion dies are fully preheated for thermal insulation at the temperature of 200 to 400DEG. C; the finished products are obtained after the extrusion. The present invention is the preparation technology of high silumin electronic packing material, which can obviously improve the heat conductivity, the air tightness and the tensile strength of material, keep the low thermal expansion coefficient of the material and greatly improve the processing and forming performance of the material.
Description
Technical field
The present invention relates to a kind of preparation technology of aluminium silicon electronic package material, relate in particular to a kind of preparation technology of silumin electronic package materials.
Background technology
Since 1958 first block semiconductor integrated circuits came out, up to the present, the MOORE law was followed in the development of IC chip integration substantially.The raising of chip integration must cause the rising of its heat generation rate, makes the working temperature of circuit constantly rise, thereby causes the increase of part failure rate.Meanwhile, Electronic Packaging is also constantly to miniaturization, the direction of lightweight and High Density Packagingization develops, since nineteen nineties, various High Density Packaging Technology, as chip size packages (CSP), continuing to bring out of multi-chip module (MCM) and one pole integrated package (SLIM) etc. further increased the heat generation rate of system unit volume.For satisfying developing rapidly of above-mentioned IC and encapsulation technology, require on the one hand the structure of encapsulation is reasonably designed; On the other hand, for fundamentally improving the performance of product, research and develop novel encapsulated material with all strength and seem particularly important with the high thermal conductance of low-density low bulk and good combination property.(density is less than 2.7gcm owing to have light weight with the electronic package material of silumin preparation
-3), thermal coefficient of expansion is low, heat-conductive characteristic is good and high strength and stiffness, can plate with gold, silver, copper, nickel, can weld with base material, be easy to accurate machine work, superior function such as nontoxic, meet the requirement that the Electronic Packaging technology develops towards miniaturization, lightweight, High Density Packaging direction.In addition, aluminium silicon content on earth is all quite abundant, the mature preparation process of silica flour, with low cost, so the alusil alloy material becomes a kind of potential electronic package material with broad prospect of application, but because alusil alloy materials processing shaping difficulty when silicone content is higher, a kind of process stabilizing is developed in expectation, cost is lower, the preparation technology of material high comprehensive performance.
Summary of the invention
Technical problem to be solved by this invention provides a kind of thermal conductivity, air-tightness and tensile strength that can significantly improve material, keep the lower thermal coefficient of expansion of material, improve the preparation technology of the silumin electronic package materials of materials processing forming property significantly, make aluminium silicon electronic package material have good comprehensive serviceability.
In order to solve the problems of the technologies described above, the preparation technology that the present invention adopts is:
A), powder is produced
Commercial-purity aluminium and HIGH-PURITY SILICON are prepared into the Al-Si alloy powder by quality ratio 6～8.8: 4～1.2;
B), the air oxidation treatment process of powder
The Al-Si alloy powder for preparing is placed in the resistance furnace, be warming up to 250～450 ℃, back natural cooling in air is taken out in insulation oxidation 8～32 hours;
C), hot extrusion technique
With the alloy powder after the oxidation just adorn, jolt ramming packs in the fine aluminium jacket, on 300～500 t hydraulic press, adopt the forward extrusion mode to push, before the extruding Al-Si alloy powder is adopted 400～520 ℃ of insulations 0.5～2 hour, extrusion ratio is 10～21, various extrusion dies are at first inserted in the heating furnace before the extruding, at 200～400 ℃ of abundant preheating insulations, be finished product after having pushed.
Adopt the preparation technology of the silumin electronic package materials of technique scheme, a kind of practicable process route has been proposed, the Al-Si alloy powder is incubated oxidation in air, adopt hot extrusion that powder is carried out follow-up densification again, make that matrix combines condition improvement with the interface of enhanced granule in the aluminum-silicon alloy composite, simultaneously, the oxidation particle disperse that the powder-processed afterreaction generates is distributed in the tissue of material, play the effect of dispersion-strengtherning and densification, improved the combination property of material.The present invention is on the basis of prior powder metallurgy prepared composite material, earlier alloy powder is carried out the air pre-oxidation treatment, make powder carry out abundant oxidation, adopt the fine aluminium jacket to carry out hot extrusion in the powder after the oxidation again and become a useful person, prepare the aluminium silicon composite electron encapsulating material of oxide dispersion intensifying.
The present invention adopts the high-temperature oxydation preliminary treatment to powder elder generation, makes the abundant oxidation of powder, again in conjunction with the densification process of jacket hot extrusion, has prepared the alusil alloy electronic package material with excellent comprehensive performances.
The performance index of material are as follows after the hot extrusion:
Air-tightness (10
-9Pam
3S
-1): 0.2～1.6; Thermal conductivity (WM
-1K
-1): 104.2～144.4; Coefficient of linear expansion (10 in the time of 100 ℃
-6K
-1): 13.5～16.8; Tensile strength (MPa): 195～285; Bending strength (MPa): 242～359.
Its integrated performance index obviously is better than the conditional electronic encapsulating material, can satisfy electronic package material fully to above-mentioned performance demands.
In sum, the present invention is a kind of thermal conductivity, air-tightness and tensile strength that can significantly improve material, keep the lower thermal coefficient of expansion of material, improve the preparation technology of the silumin electronic package materials of materials processing forming property significantly, make aluminium silicon electronic package material have good comprehensive serviceability.
Embodiment
Embodiment 1:
A) powder is produced
Commercial-purity aluminium and HIGH-PURITY SILICON are warming up to 750 ℃ by the melting in induction furnace of quality ratio 8.8: 1.2 batching, fully stir, and cover slag making with flux (30%NaCl+47%KCl+23% ice crystal), and with carbon trichloride (C
2Cl
6) degasification.Molten drop injects sprayer unit through leting slip a remark, directly sprayed in the High-Pressure Water apart from nozzle 200mm by the molten metal pearl after the high pressure nitrogen atomizing, after cooling, the current that contain the Al-Si alloy powder are crossed through screen cloth and are missed the drier that foreign material flow into high speed rotating and carry out processed, drying, sieving makes required Al-12Si alloy powder, its flouring technology parameter subordinate list 1.
Table 1 flouring technology parameter
B) the air oxidation treatment process of powder
The Al-12Si alloy powder for preparing is placed in the chamber type electric resistance furnace, be warming up to 250, insulation oxidization time 32 hours takes out back natural cooling in air.
C) hot extrusion technique
After the alloy powder oxidation, in just the fine aluminium jacket was packed in dress, jolt ramming into, its density can reach 70% of solid density, and the seam jacket at one end leaves a venthole.On 300 tons of hydraulic presses, adopt the forward extrusion mode to push.Before the extruding Al-12Si alloy powder is adopted 400 ℃ of insulations 0.5 hour, extrusion ratio is 21 (internal diameter of the container and the excellent diameter of extruding are respectively 60mm and 13mm), and recipient adopts the 45# steel to make, and its internal diameter is 60mm, the extrusion die internal diameter is 13mm, and the extruding cone angle is 90 °.Various extrusion dies are at first inserted in the heating furnace before pushing, and at 200 ℃ of abundant preheating insulations, evenly apply lubricant (75% graphite+25% machine oil) before the extruding in recipient.Be finished product after having pushed.
D) material property
Air-tightness (10
-9Pam
3S
-1): 0.2; Thermal conductivity (WM
-1K
-1): 144.4; Coefficient of linear expansion (10 in the time of 100 ℃
-6K
-1): 16.8; Tensile strength (MPa): 195; Bending strength (MPa): 242.
Embodiment 2:
A) powder is produced
Commercial-purity aluminium and HIGH-PURITY SILICON are warming up to 900 by the melting in induction furnace of quality ratio 8: 2 batching, fully stir, and cover slag making with flux (30%NaCl+47%KCl+23% ice crystal), and with carbon trichloride (C
2Cl
6) degasification.Molten drop injects sprayer unit through leting slip a remark, directly sprayed in the High-Pressure Water apart from nozzle 200mm by the molten metal pearl after the high pressure nitrogen atomizing, after cooling, the current that contain the Al-Si alloy powder are crossed through screen cloth and are missed the drier that foreign material flow into high speed rotating and carry out processed, drying, sieving makes required Al-20Si alloy powder, its flouring technology parameter subordinate list 2.
Table 2 flouring technology parameter
B) the air oxidation treatment process of powder
The Al-20Si alloy powder for preparing is placed in the chamber type electric resistance furnace, be warming up to 300 ℃, insulation oxidization time 24 hours takes out back natural cooling in air.
C) hot extrusion technique
After the alloy powder oxidation, in just the fine aluminium jacket was packed in dress, jolt ramming into, its density can reach 70% of solid density, and the seam jacket at one end leaves a venthole.On 350 t hydraulic press, adopt the forward extrusion mode to push.Before the extruding Al-20Si alloy powder is adopted 430 ℃ of insulations one hour, extrusion ratio is 16 (internal diameter of the container and the excellent diameter of extruding are respectively 40mm and 10mm), and recipient adopts the 45# steel to make, and its internal diameter is 40mm, the extrusion die internal diameter is 10mm, and the extruding cone angle is 90 °.Various extrusion dies are at first inserted in the heating furnace before pushing, and at 250 ℃ of abundant preheating insulations, evenly apply lubricant (75% graphite+25% machine oil) before the extruding in recipient.Be finished product after having pushed.
D) material property
Air-tightness (10
-9Pam
3S
-1): 0.4; Thermal conductivity (WM
-1K
-1): 136.5; 100 o'clock coefficient of linear expansion (10
-6K
-1): 15.2; Tensile strength (MPa): 268; Bending strength (MPa): 301.
Embodiment 3:
A) powder is produced
Commercial-purity aluminium and HIGH-PURITY SILICON are warming up to 1050 ℃ by the melting in induction furnace of quality ratio 7.4: 2.6 batching, fully stir, and cover slag making with flux (30%NaCl+47%KCl+23% ice crystal), and with carbon trichloride (C
2Cl
6) degasification.Molten drop injects sprayer unit through leting slip a remark, directly sprayed in the High-Pressure Water apart from nozzle 200mm by the molten metal pearl after the high pressure nitrogen atomizing, after cooling, the current that contain the Al-Si alloy powder are crossed through screen cloth and are missed the drier that foreign material flow into high speed rotating and carry out processed, drying, sieving makes required Al-26Si alloy powder, its flouring technology parameter subordinate list 3.
Table 3 flouring technology parameter
B) the air oxidation treatment process of powder
The Al-26Si alloy powder for preparing is placed in the chamber type electric resistance furnace, be warming up to 350 ℃, insulation oxidization time 24 hours takes out back natural cooling in air.
C) hot extrusion technique
After the alloy powder oxidation, in just the fine aluminium jacket was packed in dress, jolt ramming into, its density can reach 70% of solid density, and the seam jacket at one end leaves a venthole.On 400 t hydraulic press, adopt the forward extrusion mode to push.Before the extruding Al-26Si alloy powder is adopted 460 ℃ of insulations one hour, extrusion ratio is 14 (internal diameter of the container and the excellent diameter of extruding are respectively 40mm and 10.7mm), and recipient adopts the 45# steel to make, and its internal diameter is 40mm, the extrusion die internal diameter is 10.7mm, and the extruding cone angle is 90 °.Various extrusion dies are at first inserted in the heating furnace before pushing, and at 300 ℃ of abundant preheating insulations, evenly apply lubricant (75% graphite+25% machine oil) before the extruding in recipient.Be finished product after having pushed.
D) material property
Air-tightness (10
-9Pam
3S
-1): 0.5; Thermal conductivity (WM
-1K
-1): 124.6; Coefficient of linear expansion (10 in the time of 100 ℃
-5K
-1): 15.7; Tensile strength (MPa): 285; Bending strength (MPa): 313.
Embodiment 4:
A) powder is produced
Commercial-purity aluminium and HIGH-PURITY SILICON are warming up to 1200 ℃ by the melting in induction furnace of quality ratio 6.7: 3.3 batching, fully stir, and cover slag making with flux (30%NaCl+47%KCl+23% ice crystal), and with carbon trichloride (C
2Cl
6) degasification.Molten drop injects sprayer unit through leting slip a remark, directly sprayed in the High-Pressure Water apart from nozzle 200mm by the molten metal pearl after the high pressure nitrogen atomizing, after cooling, the current that contain the Al-Si alloy powder are crossed through screen cloth and are missed the drier that foreign material flow into high speed rotating and carry out processed, drying, sieving makes required Al-33Si alloy powder, its flouring technology parameter subordinate list 4.
Table 4 flouring technology parameter
B) the air oxidation treatment process of powder
The Al-33Si alloy powder for preparing is placed in the chamber type electric resistance furnace, be warming up to 400 ℃, insulation oxidization time 16 hours takes out back natural cooling in air.
C) hot extrusion technique
After the alloy powder oxidation, in just the fine aluminium jacket was packed in dress, jolt ramming into, its density can reach 70% of solid density, and the seam jacket at one end leaves a venthole.On 450 t hydraulic press, adopt the forward extrusion mode to push.Before the extruding Al-33Si alloy powder is adopted 490 ℃ of insulations 1.5 hours, extrusion ratio is 12 (internal diameter of the container and the excellent diameter of extruding are respectively 40mm and 11.5mm), and recipient adopts the 45# steel to make, and its internal diameter is 40mm, the extrusion die internal diameter is 11.5mm, and the extruding cone angle is 90 °.Various extrusion dies are at first inserted in the heating furnace before pushing, and at 350 ℃ of abundant preheating insulations, evenly apply lubricant (75% graphite+25% machine oil) before the extruding in recipient.Be finished product after having pushed.
D) material property
Air-tightness (10
-9Pam
3S
-1): 0.8; Thermal conductivity (WM
-1K
-1): 110.2; Coefficient of linear expansion (10 in the time of 100 ℃
-6K
-1): 14.7; Tensile strength (MPa): 245; Bending strength (MPa): 359.
Embodiment 5:
A) powder is produced
Commercial-purity aluminium and HIGH-PURITY SILICON are warming up to 1350 ℃ by the melting in induction furnace of quality ratio 6: 4 batching, fully stir, and cover slag making with flux (30%NaCl+47%KCl+23% ice crystal), and with carbon trichloride (C
2Cl
6) degasification.Molten drop injects sprayer unit through leting slip a remark, directly sprayed in the High-Pressure Water apart from nozzle 200mm by the molten metal pearl after the high pressure nitrogen atomizing, after cooling, the current that contain the Al-Si alloy powder are crossed through screen cloth and are missed the drier that foreign material flow into high speed rotating and carry out processed, drying, sieving makes required Al-40Si alloy powder, its flouring technology parameter subordinate list 5.
Table 5 flouring technology parameter
B) the air oxidation treatment process of powder
The Al-40Si alloy powder for preparing is placed in the chamber type electric resistance furnace, be warming up to 450 ℃, insulation oxidization time 8 hours takes out back natural cooling in air.
C) hot extrusion technique
After the alloy powder oxidation, in just the fine aluminium jacket was packed in dress, jolt ramming into, its density can reach 70% of solid density, and the seam jacket at one end leaves a venthole.On 500 t hydraulic press, adopt the forward extrusion mode to push.Before the extruding Al-40Si alloy powder is adopted 520 ℃ of insulations 2 hours, extrusion ratio is 10 (internal diameter of the container and the excellent diameter of extruding are respectively 40mm and 16mm), and recipient adopts the 45# steel to make, and its internal diameter is 40mm, the extrusion die internal diameter is 16mm, and the extruding cone angle is 90 °.Various extrusion dies are at first inserted in the heating furnace before pushing, and at 400 ℃ of abundant preheating insulations, evenly apply lubricant (75% graphite+25% machine oil) before the extruding in recipient.Be finished product after having pushed.
D) material property
Air-tightness (10
-9Pam
3S
-1): 1.6; Thermal conductivity (WM
-1K
-1): 104.2; 100 o'clock coefficient of linear expansion (10
-6K
-1): 13.5; Tensile strength (MPa): 219; Bending strength (MPa): 325.
Claims (2)
1, a kind of preparation technology of silumin electronic package materials, its processing step is as follows:
A), powder is produced
Commercial-purity aluminium and HIGH-PURITY SILICON are prepared into the Al-Si alloy powder by quality ratio 6～8.8: 4～1.2;
B), the air oxidation treatment process of powder
The Al-Si alloy powder for preparing is placed in the resistance furnace, be warming up to 250～450 ℃, back natural cooling in air is taken out in insulation oxidation 8～32 hours;
C), hot extrusion technique
With the alloy powder after the oxidation just adorn, jolt ramming packs in the fine aluminium jacket, on 300～500 t hydraulic press, adopt the forward extrusion mode to push, before the extruding Al-Si alloy powder is adopted 400～520 ℃ of insulations 0.5～2 hour, extrusion ratio is 10～21, various extrusion dies are at first inserted in the heating furnace before the extruding, at 200～400 ℃ of abundant preheating insulations, be finished product after having pushed.
2, the preparation technology of silumin electronic package materials according to claim 1, it is characterized in that: described powder reparation technology is: commercial-purity aluminium and HIGH-PURITY SILICON are by 6～8.8: 4～1.2 batching meltings in induction furnace of quality ratio, be warming up to 750～1200 ℃, fully stir, with the 30%NaCl+47%KCl+23% ice crystal is that flux covers slag making, and uses the carbon trichloride degasification; Molten drop injects sprayer unit through leting slip a remark, directly sprayed in the High-Pressure Water apart from nozzle 200mm by the molten metal pearl after the high pressure nitrogen atomizing, after cooling, the current that contain the Al-Si alloy powder are crossed through screen cloth and are missed the drier that foreign material flow into high speed rotating and carry out processed, and drying, sieving makes the Al-Si alloy powder.
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| CN100435321C true CN100435321C (en) | 2008-11-19 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103740956B (en) * | 2014-01-08 | 2015-12-30 | 镇江镨利玛新型材料科技有限公司 | The preparation method of silumin |
| CN104617276B (en) * | 2015-02-10 | 2018-03-30 | 南开大学 | Lithium rechargeable battery porous silicon/carbon compound cathode materials and preparation method thereof |
| CN106378458A (en) * | 2016-08-29 | 2017-02-08 | 河源富马硬质合金股份有限公司 | Method for preparing hard alloy in vacuum extrusion mode |
| CN106670467A (en) * | 2016-12-28 | 2017-05-17 | 北京有色金属研究总院 | Method for preparing high-silicon aluminum alloy by peeling and thermal extruding through rapid-solidified powder metallurgy |
| CN106967905B (en) * | 2017-03-14 | 2018-06-26 | 上海爱邦新型包装材料有限公司 | A kind of preparation method of low bulk high temperature aluminium alloys layered electronic encapsulating material |
| CN111036926A (en) * | 2019-12-18 | 2020-04-21 | 长沙新材料产业研究院有限公司 | High-silicon aluminum alloy material for additive manufacturing and preparation method thereof |
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| JP2003027109A (en) * | 2001-07-23 | 2003-01-29 | Sanyo Special Steel Co Ltd | Method for producing oxide dispersion type alloy |
| CN1531072A (en) * | 2003-03-14 | 2004-09-22 | 北京有色金属研究总院 | High-thermal conductivity silicon-aluminium alloy sealing material with low-density and expansion coefficient, preparing method thereof |
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2006
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Patent Citations (3)
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| JP2003027109A (en) * | 2001-07-23 | 2003-01-29 | Sanyo Special Steel Co Ltd | Method for producing oxide dispersion type alloy |
| CN1531072A (en) * | 2003-03-14 | 2004-09-22 | 北京有色金属研究总院 | High-thermal conductivity silicon-aluminium alloy sealing material with low-density and expansion coefficient, preparing method thereof |
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Non-Patent Citations (4)
| Title |
|---|
| 真空包套热挤压高硅铝合金粉末材料的研究. 甘卫平，陈招科，杨伏良.稀有金属与硬质合金，第32卷第3期. 2004 |
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Assignee: Hunan Jingang Aluminum Co., Ltd. Assignor: Central South University Contract record no.: 2010430000039 Denomination of invention: Process for preparing silumin electronic package materials Granted publication date: 20081119 License type: Exclusive License Open date: 20061213 Record date: 20100519 |
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Granted publication date: 20081119 Termination date: 20120630 |