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 Al-Si alloy powder by mass percentage at 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
The melting in induction furnace of commercial-purity aluminium and HIGH-PURITY SILICON 8.8: 1.2 by mass percentage batching is warming up to 750 ℃, fully stirs, and covers 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 the about 200mm of nozzle 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 l.
Table 1 flouring technology parameter
Smelting temperature (℃) | Temperature retention time (h) | Nozzle bore (mm) | Atomization gas | Gas pressure (MPa) | The spray chamber type |
750 | 0.5 | 3.5 | Air | 0.6 | Circular seam type |
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; 100 o'clock coefficient of linear expansion (10
-6K
-1): 16.8; Tensile strength (MPa): 195; Bending strength (MPa): 242.
Embodiment 2:
A) powder is produced
The melting in induction furnace of commercial-purity aluminium and HIGH-PURITY SILICON 8: 2 by mass percentage batching is warming up to 900, fully stirs, and covers 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 the about 200mm of nozzle 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
Smelting temperature (℃) | Temperature retention time (h) | Nozzle bore (mm) | Atomization gas | Gas pressure (MPa) | The spray chamber type |
900 | 0.5 | 3.5 | Air | 0.6 | Circular seam type |
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
The melting in induction furnace of commercial-purity aluminium and HIGH-PURITY SILICON 7.4: 2.6 by mass percentage batching is warming up to 1050, fully stirs, and covers 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 the about 200mm of nozzle 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
Smelting temperature (℃) | Temperature retention time (h) | Nozzle bore (mm) | Atomization gas | Gas pressure (MPa) | The spray chamber type |
1050 | 1 | 3.5 | Air | 0.6 | Circular seam type |
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 ℃
-6K
-1): 15.7; Tensile strength (MPa): 285; Bending strength (MPa): 313.
Embodiment 4:
A) powder is produced
The melting in induction furnace of commercial-purity aluminium and HIGH-PURITY SILICON 6.7: 3.3 by mass percentage batching is warming up to 1200, fully stirs, and covers 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 the about 200mm of nozzle 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
Smelting temperature (℃) | Temperature retention time (h) | Nozzle bore (mm) | Atomization gas | Gas pressure (MPa) | The spray chamber type |
1200 | 1 | 3.5 | Air | 0.6 | Circular seam type |
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; 100 o'clock coefficient of linear expansion (10
-6K
-1): 14.7; Tensile strength (MPa): 245; Bending strength (MPa): 359.
Embodiment 5:
A) powder is produced
The melting in induction furnace of commercial-purity aluminium and HIGH-PURITY SILICON 6: 4 by mass percentage batching is warming up to 1350 ℃, fully stirs, and covers 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 the about 200mm of nozzle 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
Smelting temperature (℃) | Temperature retention time (h) | Nozzle bore (mm) | Atomization gas | Gas pressure (MPa) | The spray chamber type |
1350 | 1 | 3.5 | Air | 0.6 | Circular seam type |
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; Coefficient of linear expansion (10 in the time of 100 ℃
-6K
-1): 13.5; Tensile strength (MPa): 219; Bending strength (MPa): 325.