CN106987736A - A kind of preparation method of aluminium silicon-carbon alloy electronic package material - Google Patents

A kind of preparation method of aluminium silicon-carbon alloy electronic package material Download PDF

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Publication number
CN106987736A
CN106987736A CN201710246420.1A CN201710246420A CN106987736A CN 106987736 A CN106987736 A CN 106987736A CN 201710246420 A CN201710246420 A CN 201710246420A CN 106987736 A CN106987736 A CN 106987736A
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alloy
hours
solution
temperature
silicon
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不公告发明人
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Suzhou Nell Mstar Technology Ltd
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Suzhou Nell Mstar Technology Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D17/00—Pressure die casting or injection die casting, i.e. casting in which the metal is forced into a mould under high pressure
    • B22D17/007—Semi-solid pressure die casting
    • 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
    • C22C1/10—Alloys containing non-metals
    • C22C1/1005—Pretreatment of the non-metallic additives
    • 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
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent

Abstract

The invention discloses a kind of preparation method of aluminium silicon-carbon alloy electronic package material, the good combination of the invention by grapheme material and aluminium silicon, so that the total body density and intensity of the composite are adjusted, with good tensile strength and impact flexibility；In addition reduce alloy molten solution temperature by controlling the method for forming core and prepare semi solid slurry, make alloy molten solution by during forming core passage by strong stirring, primary silicon can effectively be suppressed to grow up, the features such as even tissue, consistency height, the low coefficient of expansion and high thermal conductivity, excellent combination property, is completely suitable for Electronic Packaging.

Description

A kind of preparation method of aluminium silicon-carbon alloy electronic package material
Technical field
The present invention relates to electronic product packaging material manufacture field, and in particular to a kind of aluminium silicon-carbon alloy electronic package material Preparation method.
Background technology
Alloy material can have a characteristic of different metal element due to there is Determination of multiple metal elements in the material, After the characteristic for possessing different metal element, expand the performance of alloy material and use scope.The use of albronze alloy Scope is very wide, can be used for light industry, heavy industry, electronics industry etc..For example be used to make spring, the metal part of electronic equipment, Hardware equipment, Medical Devices etc.
With the high speed development of microelectric technique, electronic component should have higher integrated level, the faster speed of service and more Big capacity, this allow in electronic device and electronic installation the complexity of component and and intensive increasingly improve, this certainty The raising of circuit caloric value, operating temperature can be caused to rise, and stability declines.Electronic Packaging is important as one for circuit Part plays circuit supporting, sealing, the connection of interior exterior point, radiating and shielding action, has to the Performance And Reliability of circuit Material impact.
Alusil alloy is as a kind of novel encapsulated material, due to the small (2.42-2.51cm of this alloy density3), thermal expansion Coefficient low (6.8 × 10-6-11 × 10-6/K), heat conductivity are good (120-149W/m K), and raw material resources enriches, and cost is low It is honest and clean, it is easy to machine-shaping and recycling, it is highly suitable for Electronic Packaging field and uses.
The content of the invention
The present invention provides a kind of preparation method of aluminium silicon-carbon alloy electronic package material, the present invention by grapheme material with The good combination of aluminium silicon, so as to adjust the total body density and intensity of the composite, with good tensile strength and Impact flexibility；In addition reduce alloy molten solution temperature by controlling the method for forming core and prepare semi solid slurry, make alloy molten solution By, by strong stirring, can effectively suppress primary silicon during forming core passage and grow up, even tissue, consistency are high, the coefficient of expansion is low And thermal conductivity it is high the features such as, excellent combination property is completely suitable for Electronic Packaging.
To achieve these goals, should the invention provides a kind of preparation method of aluminium silicon-carbon alloy electronic package material Method comprises the following steps：
（1）Prepare carbon particle aluminum alloy base material
The 5L nitration mixture constituted by 250g native graphites and by the 4.5L concentrated sulfuric acids and 0.5L concentrated phosphoric acids is mixed in reactor and electricity consumption Control magnetic stirrer uniform, 500g potassium permanganate is slowly added in the case of less than 20 DEG C；Afterwards, reactor is sealed simultaneously It is warming up to 85-90 DEG C to react 2-3 hours, product is taken out from reactor lower end, be diluted to 40L solution, adds 0.6L hydrogen peroxide Obtain glassy yellow graphite oxide solution；Then, washed with acid and water alternating centrifugal, to pH value of solution=5-6, remove foreign ion；Most Afterwards, ultrasonic disperse graphite oxide, configures certain density graphene oxide solution；
2L 0.5mg/mL graphene oxide solutions are transferred in reactor, under magnetic stirring add 12-36g iron powders and 0.8-1.8L concentrated hydrochloric acid, 75-90 DEG C is reacted 4-5 hours；Then stand, the iron powder of residual is removed with hydrochloric acid filtering and washing, then Wash suction filtration deacidification；Finally it is freeze-dried, grinds graphene particles of sieving to obtain；
It is matrix material by A357 aluminium alloys, is stirred under semisolid, described matrix material is that granular size is 14.2 μ Mixing time is 6 hours under m, semisolid；
After the completion of stirring semisolid slurry, graphene particles are added, continues to stir while heating, obtains liquid aluminium alloy material Material；
Liquid aluminium alloy material is cooled to liquid-solid two-phase section, is positioned in inert gas；Liquid is stirred in inert gas environment Liquid composite material is mixed, and temperature is progressively reduced to normal temperature, high-quality carbon particle aluminum alloy base material is can obtain；
（2）By material dispensing in proportion, wherein proportion scale is that the mass percent of silicon is 21%-35%, and surplus is above-mentioned carbon Particle aluminum alloy base material；
Above-mentioned dispensing is superheated to the 90-120 DEG C of refining of the liquidus temperature above；
By the alloy molten solution after refining pour into preheating after quantitative furnace and cover bell；
The valve of quantitative furnace tops is opened, while the valve of argon bottle is opened, untill the air in stove is drained completely, The valve and the valve of argon bottle finally closed at the top of bell；
Alloy molten solution in stove is superheated to 250-300 DEG C of the liquidus temperature above；
Alloy molten solution in stove is incubated 0.5-1 hours in the case of 250-300 DEG C of the liquidus temperature above；
The high temperature alloy liquation of overheat is delivered to by control forming core device by stalk with constant displacement pump, control forming core device closes high temperature Golden liquation is quickly cooled to semi-solid temperature area and completes semi solid slurry preparation；
By the direct rheo-diecasting of obtained semi solid slurry, and densification processing is done, obtain product.
It is preferred that, the densification processing is specially：Ingot blank is put into hot isostatic apparatus, ingot blank is densified Processing.Protective gas is nitrogen, and treatment temperature is 640 DEG C -700 DEG C, and pressure is 120MPa-180MPa, is incubated 5-6 hours.It is cold But resulting materials are the silicon aluminum carbon alloy material used for electronic packaging that consistency is more than 99% excellent combination property after.
It is an advantage of the current invention that by the good combination of grapheme material and aluminium silicon, so as to adjust the composite wood The total body density and intensity of material, with good tensile strength and impact flexibility；In addition by controlling the method for forming core to drop Low-alloy melt temperature simultaneously prepares semi solid slurry, makes alloy molten solution by, by strong stirring, can effectively press down during forming core passage Primary silicon processed is grown up, and even tissue, consistency are high, the low coefficient of expansion and the features such as high thermal conductivity, excellent combination property, completely Suitable for Electronic Packaging.
Embodiment
Embodiment one
The 5L nitration mixture constituted by 250g native graphites and by the 4.5L concentrated sulfuric acids and 0.5L concentrated phosphoric acids is mixed in reactor and electricity consumption Control magnetic stirrer uniform, 500g potassium permanganate is slowly added in the case of less than 20 DEG C；Afterwards, reactor is sealed simultaneously It is warming up to 85 DEG C to react 2 hours, product is taken out from reactor lower end, be diluted to 40L solution, adds 0.6L hydrogen peroxide and obtain bright orange Color graphite oxide solution；Then, washed with acid and water alternating centrifugal, to pH value of solution=5-6, remove foreign ion；Finally, it is ultrasonic Scattered graphite oxide, configures certain density graphene oxide solution.
2L 0.5mg/mL graphene oxide solutions are transferred in reactor, under magnetic stirring add 12g iron powders and 0.8L concentrated hydrochloric acid, 75 DEG C are reacted 4 hours；Then stand, the iron powder of residual is removed with hydrochloric acid filtering and washing, then wash suction filtration and remove Acid；Finally it is freeze-dried, grinds graphene particles of sieving to obtain.
It is matrix material by A357 aluminium alloys, is stirred under semisolid, described matrix material is that granular size is 14.2 μm, mixing time is 6 hours under semisolid.
After the completion of stirring semisolid slurry, graphene particles are added, continue to stir while heating, liquid aluminium conjunction is obtained Golden material.Liquid aluminium alloy material is cooled to liquid-solid two-phase section, is positioned in inert gas；The liquid in inert gas environment State stirs liquid composite material, and temperature progressively is reduced into normal temperature, can obtain high-quality carbon particle aluminum alloy base material.
By material dispensing in proportion, wherein proportion scale is that the mass percent of silicon is 21%, and surplus is above-mentioned carbon particle Aluminum alloy base material；Above-mentioned dispensing is superheated to more than liquidus temperature 90 DEG C of refinings；
By the alloy molten solution after refining pour into preheating after quantitative furnace and cover bell；The valve of quantitative furnace tops is opened, The valve of argon bottle, untill the air in stove is drained completely, the valve and argon gas finally closed at the top of bell are opened simultaneously The valve of bottle；Alloy molten solution in stove is superheated to more than liquidus temperature 250 DEG C；By alloy molten solution in stove in liquidus temperature 0.5 hour is incubated in the case of 250 DEG C of the above；The high temperature alloy liquation of overheat is delivered to by control by stalk with constant displacement pump High temperature alloy liquation is quickly cooled to semi-solid temperature area and completes semi solid slurry and prepared by forming core device, control forming core device.
By the direct rheo-diecasting of obtained semi solid slurry, ingot blank is subjected to densification processing, that is, obtains consistency and is more than 99% sial carbon alloy electronic package material.It is described densification processing be specially：Ingot blank is put into hot isostatic apparatus, Densification is carried out to ingot blank.Protective gas is nitrogen, and treatment temperature is 640 DEG C, and pressure is 120MPa, is incubated 5 hours.It is cold But resulting materials are the silicon aluminum carbon alloy material used for electronic packaging that consistency is more than 99% excellent combination property after.
Embodiment two
The 5L nitration mixture constituted by 250g native graphites and by the 4.5L concentrated sulfuric acids and 0.5L concentrated phosphoric acids is mixed in reactor and electricity consumption Control magnetic stirrer uniform, 500g potassium permanganate is slowly added in the case of less than 20 DEG C；Afterwards, reactor is sealed simultaneously It is warming up to 90 DEG C to react 3 hours, product is taken out from reactor lower end, be diluted to 40L solution, adds 0.6L hydrogen peroxide and obtain bright orange Color graphite oxide solution；Then, washed with acid and water alternating centrifugal, to pH value of solution=5-6, remove foreign ion；Finally, it is ultrasonic Scattered graphite oxide, configures certain density graphene oxide solution.
2L 0.5mg/mL graphene oxide solutions are transferred in reactor, under magnetic stirring add 36g iron powders and 1.8L concentrated hydrochloric acid, 90 DEG C are reacted 5 hours；Then stand, the iron powder of residual is removed with hydrochloric acid filtering and washing, then wash suction filtration Deacidification；Finally it is freeze-dried, grinds graphene particles of sieving to obtain.
It is matrix material by A357 aluminium alloys, is stirred under semisolid, described matrix material is that granular size is 14.2 μm, mixing time is 6 hours under semisolid.
After the completion of stirring semisolid slurry, graphene particles are added, continue to stir while heating, liquid aluminium conjunction is obtained Golden material.
Liquid aluminium alloy material is cooled to liquid-solid two-phase section, is positioned in inert gas；The liquid in inert gas environment State stirs liquid composite material, and temperature progressively is reduced into normal temperature, can obtain high-quality carbon particle aluminum alloy base material.
By material dispensing in proportion, wherein proportion scale is that the mass percent of silicon is 35%, and surplus is above-mentioned carbon particle Aluminum alloy base material；Above-mentioned dispensing is superheated to more than liquidus temperature 120 DEG C of refinings；
By the alloy molten solution after refining pour into preheating after quantitative furnace and cover bell；The valve of quantitative furnace tops is opened, The valve of argon bottle, untill the air in stove is drained completely, the valve and argon gas finally closed at the top of bell are opened simultaneously The valve of bottle；Alloy molten solution in stove is superheated to more than liquidus temperature 300 DEG C；By alloy molten solution in stove in liquidus temperature 1 hour is incubated in the case of 300 DEG C of the above；The high temperature alloy liquation of overheat is delivered to by control shape by stalk with constant displacement pump High temperature alloy liquation is quickly cooled to semi-solid temperature area and completes semi solid slurry and prepared by core device, control forming core device.
By the direct rheo-diecasting of obtained semi solid slurry, ingot blank is subjected to densification processing, that is, obtains consistency more than 99% Sial carbon alloy electronic package material.It is described densification processing be specially：Ingot blank is put into hot isostatic apparatus, to ingot Base carries out densification.Protective gas is nitrogen, and treatment temperature is 700 DEG C, and pressure is 180MPa, is incubated 6 hours.After cooling Resulting materials are the silicon aluminum carbon alloy material used for electronic packaging that consistency is more than 99% excellent combination property.

Claims (2)

1. a kind of preparation method of aluminium silicon-carbon alloy electronic package material, this method comprises the following steps：
（1）Prepare carbon particle aluminum alloy base material
The 5L nitration mixture constituted by 250g native graphites and by the 4.5L concentrated sulfuric acids and 0.5L concentrated phosphoric acids is mixed in reactor and electricity consumption Control magnetic stirrer uniform, 500g potassium permanganate is slowly added in the case of less than 20 DEG C；Afterwards, reactor is sealed simultaneously It is warming up to 85-90 DEG C to react 2-3 hours, product is taken out from reactor lower end, be diluted to 40L solution, adds 0.6L hydrogen peroxide Obtain glassy yellow graphite oxide solution；Then, washed with acid and water alternating centrifugal, to pH value of solution=5-6, remove foreign ion；Most Afterwards, ultrasonic disperse graphite oxide, configures certain density graphene oxide solution；
2L 0.5mg/mL graphene oxide solutions are transferred in reactor, under magnetic stirring add 12-36g iron powders and 0.8-1.8L concentrated hydrochloric acid, 75-90 DEG C is reacted 4-5 hours；Then stand, the iron powder of residual is removed with hydrochloric acid filtering and washing, then Wash suction filtration deacidification；Finally it is freeze-dried, grinds graphene particles of sieving to obtain；
It is matrix material by A357 aluminium alloys, is stirred under semisolid, described matrix material is that granular size is 14.2 μ Mixing time is 6 hours under m, semisolid；
After the completion of stirring semisolid slurry, graphene particles are added, continues to stir while heating, obtains liquid aluminium alloy material Material；
Liquid aluminium alloy material is cooled to liquid-solid two-phase section, is positioned in inert gas；Liquid is stirred in inert gas environment Liquid composite material is mixed, and temperature is progressively reduced to normal temperature, high-quality carbon particle aluminum alloy base material is can obtain；
（2）By material dispensing in proportion, wherein proportion scale is that the mass percent of silicon is 21%-35%, and surplus is above-mentioned carbon Particle aluminum alloy base material；
Above-mentioned dispensing is superheated to the 90-120 DEG C of refining of the liquidus temperature above；
By the alloy molten solution after refining pour into preheating after quantitative furnace and cover bell；
The valve of quantitative furnace tops is opened, while the valve of argon bottle is opened, untill the air in stove is drained completely, The valve and the valve of argon bottle finally closed at the top of bell；
Alloy molten solution in stove is superheated to 250-300 DEG C of the liquidus temperature above；
Alloy molten solution in stove is incubated 0.5-1 hours in the case of 250-300 DEG C of the liquidus temperature above；
The high temperature alloy liquation of overheat is delivered to by control forming core device by stalk with constant displacement pump, control forming core device closes high temperature Golden liquation is quickly cooled to semi-solid temperature area and completes semi solid slurry preparation；
By the direct rheo-diecasting of obtained semi solid slurry, and densification processing is done, obtain product.
2. the method as described in claim 1, it is characterised in that the densification, which is processed, is specially：Ingot blank is put into heat etc. quiet Press in equipment, densification is carried out to ingot blank, protective gas is nitrogen, and treatment temperature is 640 DEG C -700 DEG C, and pressure is 120MPa-180MPa, is incubated 5-6 hours, and resulting materials are the electronics that consistency is more than 99% excellent combination property after cooling Silicon aluminum carbon alloy material is used in encapsulation.
CN201710246420.1A 2017-04-15 2017-04-15 A kind of preparation method of aluminium silicon-carbon alloy electronic package material Pending CN106987736A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111408721A (en) * 2020-04-03 2020-07-14 北京机科国创轻量化科学研究院有限公司 Aluminum alloy semi-solid state melting three-dimensional direct-writing forming method

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Publication number Priority date Publication date Assignee Title
CA2815657A1 (en) * 2010-10-27 2012-05-03 Baker Hughes Incorporated Nanomatrix powder metal composite
WO2014178613A1 (en) * 2013-04-30 2014-11-06 동양피스톤 주식회사 Aluminium alloy composition for local strengthening of aluminium pistons, and aluminium piston formed so as to have local strengthening layer using said composition
CN104150470A (en) * 2014-07-31 2014-11-19 山东玉皇新能源科技有限公司 Metal-solution reduction method for preparing graphene
CN105750521A (en) * 2016-03-02 2016-07-13 慈溪阿尔特新材料有限公司 Semi-solid rheologic die-casting method capable of refining primary silicon of high-silicon aluminum alloy and device thereof
CN105986134A (en) * 2015-01-30 2016-10-05 中南大学 Method for preparing high silicon aluminum alloy electronic packaging material
CN106282614A (en) * 2015-06-05 2017-01-04 桂林市新业机械制造有限责任公司 A kind of particle enhanced aluminum-based composite material casting method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2815657A1 (en) * 2010-10-27 2012-05-03 Baker Hughes Incorporated Nanomatrix powder metal composite
WO2014178613A1 (en) * 2013-04-30 2014-11-06 동양피스톤 주식회사 Aluminium alloy composition for local strengthening of aluminium pistons, and aluminium piston formed so as to have local strengthening layer using said composition
CN104150470A (en) * 2014-07-31 2014-11-19 山东玉皇新能源科技有限公司 Metal-solution reduction method for preparing graphene
CN105986134A (en) * 2015-01-30 2016-10-05 中南大学 Method for preparing high silicon aluminum alloy electronic packaging material
CN106282614A (en) * 2015-06-05 2017-01-04 桂林市新业机械制造有限责任公司 A kind of particle enhanced aluminum-based composite material casting method
CN105750521A (en) * 2016-03-02 2016-07-13 慈溪阿尔特新材料有限公司 Semi-solid rheologic die-casting method capable of refining primary silicon of high-silicon aluminum alloy and device thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111408721A (en) * 2020-04-03 2020-07-14 北京机科国创轻量化科学研究院有限公司 Aluminum alloy semi-solid state melting three-dimensional direct-writing forming method

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