CN106906388A - A kind of preparation method of silumin - Google Patents
A kind of preparation method of silumin Download PDFInfo
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- CN106906388A CN106906388A CN201710220132.9A CN201710220132A CN106906388A CN 106906388 A CN106906388 A CN 106906388A CN 201710220132 A CN201710220132 A CN 201710220132A CN 106906388 A CN106906388 A CN 106906388A
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- silumin
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- 229910000551 Silumin Inorganic materials 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 45
- 238000001816 cooling Methods 0.000 claims abstract description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 23
- 239000010703 silicon Substances 0.000 claims abstract description 23
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 21
- 239000000956 alloy Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 17
- 239000004411 aluminium Substances 0.000 claims abstract description 17
- 238000003825 pressing Methods 0.000 claims abstract description 13
- 235000013312 flour Nutrition 0.000 claims abstract description 12
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 11
- 239000010439 graphite Substances 0.000 claims abstract description 11
- 229910000632 Alusil Inorganic materials 0.000 claims abstract description 10
- 238000007731 hot pressing Methods 0.000 claims abstract description 8
- 238000010792 warming Methods 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 239000011856 silicon-based particle Substances 0.000 claims abstract description 4
- 229920001296 polysiloxane Polymers 0.000 claims description 18
- 238000001125 extrusion Methods 0.000 claims description 9
- 239000000498 cooling water Substances 0.000 claims description 8
- 238000000280 densification Methods 0.000 claims description 8
- 239000011812 mixed powder Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 5
- TZHYBRCGYCPGBQ-UHFFFAOYSA-N [B].[N] Chemical compound [B].[N] TZHYBRCGYCPGBQ-UHFFFAOYSA-N 0.000 claims description 2
- 230000004888 barrier function Effects 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 230000006641 stabilisation Effects 0.000 claims description 2
- 238000011105 stabilization Methods 0.000 claims description 2
- 238000001192 hot extrusion Methods 0.000 description 14
- 238000000034 method Methods 0.000 description 12
- 239000007787 solid Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 9
- 239000012071 phase Substances 0.000 description 9
- 235000013339 cereals Nutrition 0.000 description 8
- 239000007788 liquid Substances 0.000 description 6
- KMWBBMXGHHLDKL-UHFFFAOYSA-N [AlH3].[Si] Chemical compound [AlH3].[Si] KMWBBMXGHHLDKL-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000005070 sampling Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000001540 jet deposition Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000009715 pressure infiltration Methods 0.000 description 4
- 229910000838 Al alloy Inorganic materials 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 238000009718 spray deposition Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
Classifications
-
- 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
-
- B22F1/0003—
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/16—Both compacting and sintering in successive or repeated steps
-
- 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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0408—Light metal alloys
- C22C1/0416—Aluminium-based alloys
-
- 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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- 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
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F2003/026—Mold wall lubrication or article surface lubrication
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of silumin, by silica flour, aluminium powder or alusil alloy powder, it is not less than after 30% metering ratio is well mixed by silicon weight content and is fitted into the graphite of sealing or alloy mold, imposes the axial compressive force pre-pressing of 5 ~ more than 10MPa；580 ~ 900 DEG C are warming up in the vacuum hotpressing stove that then device is put into bottom belt water cooling plant, vacuum is maintained at 10 ~ 100Pa in stove；The uniform after-applied axial compressive force for being not more than 10 MPa of mould internal and external temperature simultaneously pressurize 10 ~ 30 minutes are treated, is then lowered the temperature with 1 ~ 10 DEG C/min of speed；Water cooling plant continues water flowing and accelerates cooling mould from bottom in temperature-fall period；Treat that furnace temperature is down to operable temperature and can obtain high-compactness, even tissue, silicon particle size below 100 microns, the sial block alloy high of function admirable.
Description
Technical field
It is exactly a kind of preparation method of silumin the present invention relates to field of aluminum alloys.
Background technology
With the fast development of the core integrated circuit technique of microelectric technique, integrated level rapidly increases, the electric current for passing through
It is increasing, cause chip to generate heat rapidly and rise, have a strong impact on the reliability and service life of chip operation.Silumin is made
It is a kind of new light electronic packaging material, not only with light weight, heat conductivity be excellent, thermal coefficient of expansion is low, can be very well
Ground adapts to the heat management requirement of chip.Compared with other same type of material such as aluminium silicon carbide, silumin has more preferably solderable
Property and easy processing shape, have broad application prospects.
Preparation method mainly jet deposition+high temperature insostatic pressing (HIP), pressure infiltration, the powder metallurgy of silumin are prepared at present
Liquid phase/hot pressing sintering method, powder preform solid phase hot extrusion etc..Jet deposition+high temperature insostatic pressing (HIP) is to obtain high fine and close both at home and abroad
The main method of silumin is spent, the method can obtain that crystal grain is tiny, uniform, and silicon grain is preferable micro- without sharp corners
Structure, but spray deposition technology parameter is difficult to control to.It is tiny, uniform that the hot extrusion of powder preform solid phase can also obtain crystal grain,
And preferable microstructure of the silicon grain without sharp corners.Above two technical scheme is required for unit to put down during densification
The pressure of square cms ton, proposes high requirement, while all suffering from silicone content and material to pressurized equipment and matching die
The bottleneck of the hot densification that size increase brings difficulty all the more.Compared with aluminium silicon carbide encapsulating material, silumin is most obvious
Deficiency is low intensity, and fragility is bigger, this result in the material silicone content reach 70% or so and it is higher when machining it is easy
Spring side arrisdefect, causes percent defective high.Thick, thin silicon is typically used when preparing silumin using pressure infiltration and powder metallurgic method
Particle arranges in pairs or groups to improve the bulk density of silicon, and the thick silicon grain inside the silumin prepared all has more sharp rib
Angle, machinability is significantly lower than the silumin that spray deposition technology is obtained.
The content of the invention
It is an object of the invention to be directed to the respective advantage and disadvantage of above-mentioned technique, propose that one kind mixes Pressure Infiltration and powder smelting
Golden two kinds of advantages of technique, it is liquid-solid under vacuum（Liquid alusil alloy drop-solid-state silica flour mixture）Two-phase Isothermal Hot
Extruding scheme.Compared with jet deposition+high temperature insostatic pressing (HIP) and powder preform solid phase Hot-extrusion, the technology that the present invention is provided
Method institute hot densification pressure be only its 1/100~1/10, and technological process is short, and manufacturing cost is lower.
To realize purpose of the present invention, adopt the following technical scheme that：
A kind of preparation method of silumin, it is characterised in that comprise the following steps：
（1）By silica flour and aluminium powder or alusil alloy powder, it is not less than after 30% metering ratio is well mixed by silicon weight content and is loaded
In the graphite or alloy mold of sealing, the axial compressive force pre-pressing of 5~10MPa is imposed；
（2）580~900 DEG C are warming up in the vacuum hotpressing stove that then device is put into bottom belt water cooling plant, vacuum in stove
It is maintained at 10~100Pa；Treat 10~30 points of the uniform after-applied axial compressive force for being not more than 10 MPa of mould internal and external temperature and pressurize
Clock, is then lowered the temperature with 1~10 DEG C/min of speed；
（3）Water cooling plant continues water flowing and accelerates cooling mould from bottom in temperature-fall period；
（4）Treat furnace temperature be down to operable temperature can obtain high-compactness, even tissue, silicon particle size below 100 microns,
The sial block alloy high of function admirable.
The preparation method of described a kind of silumin, it is characterised in that operate according to the following steps：
The preparation of step one, powder.Silica flour and aluminium powder or alusil alloy powder are weighed by the proportioning of silicone content 30~70%, is carried out
Batch mixing；
The preparation of step 2, mould.In former inwall and the pressure end face spraying of upper and lower stamping or the obstruct of coating nitrogen boron
Agent；
Step 3, powder are die-filling.Bottom punch will be loaded after the vertical placement of former, flexible graphite paper compacting is then placed, then will be mixed
Even powder cavity space；Flexible graphite paper is subsequently placed into, and by upper punch from upper end press-in former, in axial direction finally
Compress upper and lower stamping；
Step 4, liquid aluminium alloy-solid-state silicon grain two-phase hot extrusion.By the mould of pre-pressing, including former, upper and lower stamping and
The powder loaded in former, is together put into the vacuum hotpressing stove of bottom belt water cooling plant and is warming up to 580~900 DEG C, true in stove
Reciprocal of duty cycle is maintained at 10~100Pa, applies to be not more than the axial compressive force of 10 MPa and protect with slow after mould internal and external temperature is uniform
Pressure 10~30 minutes；
Step 5, cooling and sampling.After pressurize terminates, vacuum furnace bottom water cooling plant is continually fed into cooling water immediately, from extruding
Cooling mould is accelerated in mould lower surface, controls furnace temperature to lower the temperature with 1~10 DEG C/min of speed while cooling water is passed through,
Squeeze pressure stabilization is maintained in temperature-fall period；Treat that temperature is down to less than 570 DEG C, shed pressure and stop heating, further cooling
To operable temperature, sample is together come out of the stove together with mould, and it is that can obtain densification that puffs of the top containing shrinkage cavity are removed after the demoulding
Silumin block.
The preparation method of described silumin, it is characterised in that in described step one, the silica flour for being used,
The particle diameter of aluminium powder or alusil alloy powder is not more than 20 microns.
The preparation method of described silumin, it is characterised in that in described step four, each silicone content interval
The corresponding extrusion temperature of mixed powder and pressure are respectively：Silicone content 30~55% is 580~700 DEG C and 0.1~4MPa, and silicon contains
Amount 55~65% is 650~800 DEG C and 1~8MPa, and silicone content is 700~900 DEG C and 2~10MPa more than 65%.
In described step one, the preferential purity of raw material powder silica flour high, aluminium powder or alusil alloy powder, to be conducive to improving
The thermal conductivity of material.No matter which kind of proportion scheme is used, various powder size maximum particle diameters will be controlled below 20 microns.Batch mixing
Mode also can first be added with ethanol, acetone and other organic solvent wet mixing using dry-mixed.
In described step two, mold materials can select alloy or graphite material, preferably graphite material；The nitrogen
The barrier of boron can be prepared voluntarily, also can directly purchase the various high temperature resistants for being commercially available for pack alloy and hot extrusion aluminium alloy
Demoulding lubricant finished product.
In described step three, the flexible graphite paper placed between powder and upper and lower stamping in mould seals,
Single or multiple lift graphite paper can be used, other high temperature resistants can be also used, be played the flexible material or powder body material of effective sealing.
In described step four, extrusion temperature is waited to increase with the increase of silicone content, the raw material of same silicone content
Powder, rising Silicon In Alloys granularity or grain size with extrusion temperature can increase, and preferably extrusion temperature is as follows：Each silicone content
The interval corresponding extrusion temperature of mixed powder and pressure is respectively：Silicone content 30~55% is 580~700 DEG C and 0.1~
4MPa, silicone content 55~65% is 650~800 DEG C and 1~8MPa, and silicone content is 700~900 DEG C and 2~10MPa more than 65%.
Nominal composition liquid-solid turn of the alusil alloy of correspondence of the extrusion temperature below mixed powder that the technical scheme that the present invention is provided is used
Become liquidus temperature, that is, at the extrusion temperatures with the extension of soaking time, even if aluminium element all melts in mixed powder, be
To the aluminium-silicon binary saturated solution molten drop for forming numerous Dispersed precipitates, whole extruded object is all or liquid（Aluminium alloy）Gu-（Silicon
Particle）Two-phase coexistent.Now, apply the pressure of below 10Mpa, these molten drops can be clamp-oned the solid of respective adjacent domain
In silicon grain, required pressure is only close 1/100~1/10 of all solid state thermic.With the increase of silicone content, although hot extrusion temperature
In raising, but in liquid-solid two-phase mixtures body, solid silicon granule content is also being continuously increased degree, and required hot extrusion pressure needs therewith
Increase.Another aspect pressure is crossed solid silicon aggregation of particles during conference causes extruded object and is grown up, and the final performance to alloy is unfavorable.
In described step five, matching for sample bottom water speed of cooling and whole vacuum drying oven cooling rate is controlled, protected
Card sample bottom water speed of cooling is faster than whole vacuum drying oven cooling rate, height of specimen direction is formed thermograde.It is common in aluminium silicon
Nearby cooling velocity is slow for fisheye temperature, i.e., cooling rate is preferably controlled in 1~2 DEG C/minute between 590~560 DEG C.
Principle of the invention is：
Mixed powder with thin silicon, aluminium or alusil alloy powder is nominal in al-si eutectic temperature aluminium silicon corresponding with mixed powder as raw material
Between composition solidus temperature after of short duration insulation, apply pressure close with Pressure Infiltration（Pressure is not more than 10 MPa）, will mix
The small aluminium molten drop of the liquid of Dispersed precipitate, the silicon dissolved together with it in powder, are slowly expressed to neighbouring solid silicon particulate interspaces, prepare
Go out silumin.Silumin preparation method provided by the present invention has technological process short, without high voltage equipment and resistance to
The matching die of HTHP, with lower manufacturing cost, and its microstructure is obtained with jet deposition+high temperature insostatic pressing (HIP)
Tissue be similar to, i.e., silicon crystal grain is tiny, be evenly distributed, and without sharp corners, is beneficial to machining.
The invention has the advantages that：
1st, technological process of the present invention is short, by batch mixing can carry out liquid-solid two-phase hot extrusion, also can use with finally into
Divide the directly liquid-solid two-phase hot extrusion of consistent silumin powder；
2nd, pressure needed for liquid-solid two-phase hot extrusion is only the 1/100~1/10 of conventional solid hot densification, will to equipment and mould
Ask not high, be readily available large-sized silumin；
3rd, silicon, mutually without obvious straight flange and sharp corner angle, is conducive to improving material in the silumin that the present invention is obtained
Toughness and machinability；
4th, the silumin that the present invention is obtained has good performance：Density is 2.4~2.6gcm-3, bending strength 110
~230MPa, room temperature thermal conductivity 110~170w ﹒ m-1·℃-1, thermal coefficient of expansion 7~17 × 10-6℃-1。
Brief description of the drawings
Fig. 1 is that the size that 10 microns of silica flours and 20 microns of aluminium powders are obtained under the conditions of 650 DEG C, 1MPa hot extrusions is Φ 62mm
The 50Si50Al samples of × 18mm；
Fig. 2 is the micro-organization chart of 50Si50Al samples described in Fig. 1；
Fig. 3 is that the 70Si30Al alloys that 20 microns of silica flours and 10 microns of aluminium powders are obtained under the conditions of 800 DEG C, 6MPa hot extrusions are micro-
Organization chart.
Specific embodiment
Embodiment 1
1st, the preparation of powder.By the proportioning that silicon weight content is 50% weigh 100 grams 10 microns silica flour and 100 grams 20 microns
Aluminium powder, dry-mixed 4 hours with small-sized drum-type batch mixer；
2nd, the preparation of mould.Commercially available good red board JD- is sprayed in the cylindrical shape former inwall of Φ 62mm and upper and lower stamping pressure end face
3028 boron nitride mould releases, and dry.
3rd, powder is die-filling.It is placed on former is vertical on levels operation platform, loads bottom punch, then places layer flexible stone
Black letterweight reality；Weighed from the compound acquired in step 1 and take 100 grams of powders and slowly pour into cavity space；It is subsequently placed into flexibility
Graphite paper, and upper punch is gently pressed into former from former upper end, finally in axial direction apply on small-sized hand-operated hydraulic press
The upper and lower stamping of pressure pre-pressing of 8Mpa.
4th, liquid aluminium alloy-solid-state silicon grain two-phase hot extrusion.By the mould of step 3 pre-pressing, including former, up and down
The powder loaded in stamping and former, is together put into the vacuum hotpressing stove of bottom belt water cooling plant and is warming up to 650 DEG C, interior vacuum
Degree is maintained between 10~20Pa.Insulation is slow after making within 30 minutes mould internal and external temperature uniform to apply axial compressive force, when pressure reaches
Start pressurize to 1 MPa, the dwell time is 30 minutes.
5th, cooling and sampling.Pressurize terminates, and vacuum furnace bottom water cooling plant is continually fed into cooling water immediately.It is being passed through cooling
Control furnace temperature to be cooled to 590 DEG C with 5 DEG C/min of speed cooling while water, be then cooled to 560 with 1 DEG C/minute of cooling rate
℃.Pressure is shed, stopping is heated and continues to be passed through cooling water, treat that furnace temperature is down to less than 100 DEG C, blow-on sampling.Small-sized hand-operated
On hydraulic press after the demoulding, the shrinkage cavity layer of removal sample top 4mm thickness obtains the silumin block of densification high.
Gained sample object is as shown in figure 1, its microscopic structure is as shown in Fig. 2 measured performance is as follows：Density is 2.49g
cm-3, 150~180MPa of bending strength, room temperature thermal diffusion coefficient 0.72cm2·s-1, thermal conductivity 146Wm-1·℃-1, room temperature is extremely
200 DEG C of mean thermal expansion coefficientses 11~12 × 10-6℃-1。
Embodiment 2
1st, the preparation of powder.140 grams 20 microns of silica flour and 60 grams 10 microns of aluminium is weighed by the proportioning that silicon weight content is 50%
Powder, dry-mixed 4 hours with small-sized drum-type batch mixer；
2nd, the preparation of mould.Commercially available good red board JD- is sprayed in the cylindrical shape former inwall of Φ 62mm and upper and lower stamping pressure end face
3028 boron nitride mould releases, and dry.
3rd, powder is die-filling.It is placed on former is vertical on levels operation platform, loads bottom punch, then places layer flexible stone
Black letterweight reality；Weighed from the compound acquired in step 1 and take 100 grams of powders and slowly pour into cavity space；It is subsequently placed into flexibility
Graphite paper, and upper punch is gently pressed into former from former upper end, finally in axial direction apply on small-sized hand-operated hydraulic press
The upper and lower stamping of pressure pre-pressing of 6Mpa.
4th, liquid aluminium alloy-solid-state silicon grain two-phase hot extrusion.By the mould of step 3 pre-pressing, including former, up and down
The powder loaded in stamping and former, is together put into the vacuum hotpressing stove of bottom belt water cooling plant and is warming up to 850 DEG C, true in stove
Reciprocal of duty cycle is maintained between 10~20Pa.Insulation is slow after making within 30 minutes mould internal and external temperature uniform to apply axial compressive force, works as pressure
Reach 6 MPa and start pressurize, the dwell time is 30 minutes.
5th, cooling and sampling.Pressurize terminates, and vacuum furnace bottom water cooling plant is continually fed into cooling water immediately.It is being passed through cooling
Control furnace temperature to be cooled to 590 DEG C with 5 DEG C/min of speed cooling while water, be then cooled to 560 with 1 DEG C/minute of cooling rate
℃.Pressure is shed, stopping is heated and continues to be passed through cooling water, treat that furnace temperature is down to less than 100 DEG C, blow-on sampling.Small-sized hand-operated
On hydraulic press after the demoulding, the shrinkage cavity layer of removal sample top 6mm thickness obtains the silumin block of densification high.
The microscopic structure of gained sample is as shown in figure 3, measured performance is as follows：Density is 2.392gcm-3, bending strength
110~132MPa, room temperature thermal diffusion coefficient 0.68cm2﹒ s-1, thermal conductivity 124Wm-1·℃-1, room temperature is swollen to 200 DEG C of evenly heats
Swollen coefficient 7.5~8.5 × 10-6℃-1。
Claims (3)
1. a kind of preparation method of silumin, it is characterised in that comprise the following steps：
(1) by silica flour and aluminium powder or alusil alloy powder, it is not less than after 30% metering ratio is well mixed by silicon weight content and is loaded
In the graphite or alloy mold of sealing, the axial compressive force pre-pressing of 5~10MPa is imposed；
(2) 580~900 DEG C are warming up in the vacuum hotpressing stove for and then by device putting bottom belt water cooling plant into, vacuum in stove
It is maintained at 10~100Pa；Treat 10~30 points of the uniform after-applied axial compressive force for being not more than 10 MPa of mould internal and external temperature and pressurize
Clock, is then lowered the temperature with 1~10 DEG C/min of speed；
(3) water cooling plant continues water flowing and accelerates cooling mould from bottom in temperature-fall period；
(4) treat furnace temperature be down to operable temperature can obtain high-compactness, even tissue, silicon particle size below 100 microns,
The sial block alloy high of function admirable.
2. the preparation method of a kind of silumin according to claim 1, it is characterised in that operate according to the following steps：
Step one, silica flour and aluminium powder or alusil alloy powder are weighed by the proportioning of silicone content 30~70%, carry out batch mixing；
The barrier of step 2, pressed in former inwall and upper and lower stamping end face spraying or coating nitrogen boron；
Step 3, bottom punch will be loaded after the vertical placement of former, then place flexible graphite paper compacting, then the powder that will be mixed is cloudy
Mould die cavity；Flexible graphite paper is subsequently placed into, and upper punch is finally in axial direction compressed upper and lower from upper end press-in former
Stamping；
The powder loaded in step 4, the mould by pre-pressing, including former, upper and lower stamping and former, is together put into bottom belt
580~900 DEG C are warming up in the vacuum hotpressing stove of water cooling plant, vacuum is maintained at 10~100Pa in stove, treat temperature inside and outside mould
With the slow axial compressive force for applying to be not more than 10 MPa and pressurize 10~30 minutes after degree is uniform；
After step 5, pressurize terminate, vacuum furnace bottom water cooling plant is continually fed into cooling water immediately, adds from extrusion die lower surface
Fast cooling mould, controls furnace temperature to lower the temperature with 1~10 DEG C/min of speed while cooling water is passed through, and is tieed up in temperature-fall period
Hold squeeze pressure stabilization；Treat that temperature is down to less than 570 DEG C, shed pressure and stop heating, be cooled further to operable temperature,
Sample is together come out of the stove together with mould, and it is the silumin block that can obtain densification that puffs of the top containing shrinkage cavity are removed after the demoulding
Body.
3. the preparation method of silumin according to claim 1, it is characterised in that in described step four, respectively
The interval corresponding extrusion temperature of mixed powder of silicone content and pressure are respectively：Silicone content 30~55% is 580~700 DEG C and 0.1
~4MPa, silicone content 55~65% is 650~800 DEG C and 1~8MPa, silicone content more than 65% for 700~900 DEG C and 2~
10MPa。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110423922A (en) * | 2019-08-26 | 2019-11-08 | 中国矿业大学 | A kind of silico-aluminum and its preparation method and application for Electronic Packaging |
| CN113692198A (en) * | 2021-08-26 | 2021-11-23 | 哈尔滨铸鼎工大新材料科技有限公司 | Silicon-aluminum alloy built-in cooling structure and forming method thereof |
| CN114293048A (en) * | 2021-12-28 | 2022-04-08 | 哈尔滨工业大学 | High-density and component-controllable high-silicon aluminum alloy material and preparation method thereof |
| CN115369275A (en) * | 2021-05-17 | 2022-11-22 | 哈尔滨工业大学 | Method for preparing Al-xwt.% Si alloy semi-solid blank based on element powder liquid-phase reaction sintering |
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| CN1393572A (en) * | 2001-06-22 | 2003-01-29 | 中国科学院金属研究所 | SiAl alloy with low expansibility and high thermal conductivity |
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| CN1144849A (en) * | 1995-09-07 | 1997-03-12 | 哈尔滨工业大学 | Simple and direct inter metallic compound preparation and forming method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110423922A (en) * | 2019-08-26 | 2019-11-08 | 中国矿业大学 | A kind of silico-aluminum and its preparation method and application for Electronic Packaging |
| CN115369275A (en) * | 2021-05-17 | 2022-11-22 | 哈尔滨工业大学 | Method for preparing Al-xwt.% Si alloy semi-solid blank based on element powder liquid-phase reaction sintering |
| CN113692198A (en) * | 2021-08-26 | 2021-11-23 | 哈尔滨铸鼎工大新材料科技有限公司 | Silicon-aluminum alloy built-in cooling structure and forming method thereof |
| CN114293048A (en) * | 2021-12-28 | 2022-04-08 | 哈尔滨工业大学 | High-density and component-controllable high-silicon aluminum alloy material and preparation method thereof |
| CN114293048B (en) * | 2021-12-28 | 2022-08-02 | 哈尔滨工业大学 | High-density and component-controllable high-silicon aluminum alloy material and preparation method thereof |
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