CN106987741A - A kind of method for preparing powder metallurgy of metal-based compound electronics encapsulating material - Google Patents
A kind of method for preparing powder metallurgy of metal-based compound electronics encapsulating material Download PDFInfo
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- CN106987741A CN106987741A CN201710116032.1A CN201710116032A CN106987741A CN 106987741 A CN106987741 A CN 106987741A CN 201710116032 A CN201710116032 A CN 201710116032A CN 106987741 A CN106987741 A CN 106987741A
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- 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
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- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- 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
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- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of method for preparing powder metallurgy of metal-based compound electronics encapsulating material, this method uses and pressed compact made from Al W Si alloys and crystalline flake graphite mixed-powder is placed in graphite jig, it is placed in plasma sintering stove, close after fire door, vacuumize, be passed through inert gas pressurization, after the completion of pressurization, drain pressure after the completion of sintering, sintering is started to warm up, the demoulding is taken out.This method technique is simple; simple operation, the electronic package material prepared has higher consistency, so as to possess good heat conductivility; relatively low thermal coefficient of expansion and good mechanical strength is outer and radiation resistance, effectively can provide protection to electronic component.
Description
Technical field
The present invention relates to encapsulating material FIELD OF THE INVENTIONThe, more particularly to a kind of powder of metal-based compound electronics encapsulating material
Metallurgical preparation method.
Background technology
Electronic Packaging is to be sealed semiconductor element using fine interconnection technique, reliably electric with external circuit in realization
Connection is outer, additionally it is possible in terms of playing a part of effective heat transfer, machinery and insulation, so as to constitute a complete temperature solid knot
The technique of structure.Electronic package material has transmission electric energy and circuit signal, provides sinking path, protection structure and carrying applied force
Deng effect.Electronic package material, by more concern, is increasingly becoming electronic information along with integrated circuit, component development
The foundation stone of industry.
Electronic package material can be divided into ceramic-like, Plastic, diamond class and metal or metal-base composites class etc..
Ceramic-like encapsulating material has the advantages that thermal coefficient of expansion is small, thermal conductivity is high and good corrosion resistance, is mainly used in high density, gas
The Electronic Packaging of close property.Plastic encapsulating material realizes electronic product lightweight, miniaturization and cost degradation.Diamond is also
A kind of excellent electronic package material, but diamond prepares cost and processing cost is higher, and Aero-Space are still only limitted at present
Deng the encapsulation of highly sophisticated device.Metal material has excellent heat-conductive characteristic, can quickly conduct heat, but there is heat
The problems such as coefficient of expansion is high or expensive, should not be widely used in industrialized production.Metallic composite can both combine gold
The advantage of category, can possess the feature of other class materials so as to make up the defect of metal material, have become electronic package material again
One of research topic most popular in industry.
The performance of METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING mainly depends on the component ratio with reinforcement and matrix, selects suitable in addition
Preparation industry also have critical influence to the performance of material.The preparation method of Metal Substrate encapsulating material is according to gold when preparing
Category form difference can be divided into three classes：Solid state process, liquid phase process and spray deposition.Wherein solid state process can be divided into solid-state diffusion
Method and powder metallurgic method.Powder metallurgic method is a kind of ripe preparation method of technics comparing, and the advantage is that accurately to control
The volume proportion of substrate material particle processed and reinforcement particle, so as to realize the mesh of the thermophysical property of accurate control composite
's.But powder metallurgic method also having some limitations property, such as the consistency of its composite prepared is not high enough, herein side
Face still needs to improve.
Chinese patent CN201110422246.4 discloses a kind of powder metallurgy preparation side of high-thermal conductivity electronic packaging material
Method, raw material, the equivalent volume particle diameter of the two are used as using the enhanced thermal conduction body (R) and metallic matrix (M) powder of single particle size
(DR, DM), numbers of particles (NR, NM) are while meet certain relation to improve the thermal conductivity of material.The invention is increased based on heat conduction
Strong body and the matching of metallic matrix particle size, optimization design and the material ratio prepared do not carry out material during powder particle size matching
Expect that thermal conductivity improves 6~25%, and production cost does not increase.But, this method is improving the X-ray shield of encapsulating material
It could be improved in terms of effect.
The content of the invention
It is an object of the invention to provide a kind of method for preparing powder metallurgy of metal-based compound electronics encapsulating material, this method
Technique is simple, simple operation, and the electronic package material prepared has higher consistency, so as to possess good thermal conductivity
Can, relatively low thermal coefficient of expansion and good mechanical strength is outer and radiation resistance can be provided effectively electronic component
Protection.
To achieve the above object, the present invention uses following technical scheme：
A kind of method for preparing powder metallurgy of metal-based compound electronics encapsulating material, comprises the following steps：
(1) Al-W-Si alloy powders and crystalline flake graphite powder are prepared respectively using PREP method, by squama
Piece powdered graphite carries out chemical nickel plating processing, after being cleaned multiple times afterwards using deionized water and absolute ethyl alcohol, dries, and surface is made
The crystalline flake graphite powder of processing；
(2) the crystalline flake graphite powder prepared in the Al-W-Si alloy powders prepared in step (1) and step (2) is put into
In planetary ball mill, using positive and negative rotatable ball milling, ball milling speed is that 160-200 turns after/min, ball milling 3-5h, by two kinds of powder
It is sufficiently mixed uniform；
(3) mixed-powder is handled compressing using isostatic cool pressing, pressure is 200-300Mpa, and the dwell time is 8-
15min, is made pressed compact, pressed compact is placed in graphite jig, is placed in plasma sintering stove, closes after fire door, vacuumizes,
Inert gas pressurization is passed through, after the completion of pressurization, drain pressure after the completion of sintering, sintering is started to warm up, takes out the demoulding, is described
Metal-based compound electronics encapsulating material.
It is preferred that, in the Al-W-Si alloys, Al mass fractions are 55-60%, and W mass fractions are 15-24%, surplus
For Si.
It is preferred that, the nickel plating solution that the nickel process is used is nickel sulfate 30-50g/L, sodium hypophosphite 15-28g/
L, lactic acid 40-50g/L, sodium citrate 20-55g/L, succinic acid 18-32g/L, dodecyldimethylammonium hydroxide inner salt 1-2g/L.
It is preferred that, the crystalline flake graphite powder plating nickel on surface thickness degree is 2-7 μm.
It is preferred that, drying process is dried using vacuum drying chamber in the step (1), and temperature is 110 DEG C.
It is preferred that, the pressure in the sintering process is 60-80Mpa.
It is preferred that, in the heating sintering process：Below 600 DEG C, heating rate is 20 DEG C/min, after 600 DEG C
Heating rate is 65 DEG C/min, is risen to after 1400 DEG C, keeping temperature 10min, afterwards according to 30 DEG C/min rate reduction temperature
To normal temperature.
A kind of metal-based compound electronics encapsulating material, is prepared from by above method.
The invention has the advantages that, using material based on the excellent crystalline flake graphite of heat conductivility, improve envelope
The thermal conductivity of package material.And by carrying out Nickel Plating Treatment to graphite surface, the boundary moisture ability of graphite and alloy is improved,
So as to reduce the interface resistance of composite.Encapsulating material is allowd to possess radiation-resistant performance, Ke Yiti by adding tungsten
High material can play more efficient protection comprehensively to the safeguard function of hard X ray to electronic component.The preparation method is operated
Simply, technological process is short, is sintered using plasma sintering stove, more saves the energy, and production efficiency is high.
Embodiment
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solution
The present invention is released, any restriction will not be constituted to the present invention.
Embodiment 1
A kind of preparation method of the electronic package material with radiation-resisting functional, comprises the following steps：
(1) after being well mixed 20 parts of SiO 2 powder, 30 parts of aluminium powder, 30 parts of tungsten powder, as in stove, hydrogen is passed through,
It is 200 DEG C to adjust temperature, after roasting 1h, 5 parts of ground and mixeds of mixture and lime powder are uniform, sieving, and mesh number is 300
Mesh；
(2) mixture after sieving is placed in graphite jig, in advance in sleeve lining and upper push-down head pad carbon paper, afterwards
Graphite jig and mixture are put into baking oven together to dry under the conditions of 110 DEG C, it is compressing with 3Mpa pressure after the completion of drying；
(3) graphite jig that will be equipped with mixture is placed in plasma sintering stove, is closed after fire door, after vacuumizing,
Be passed through pressurized with hydrogen thereto, be forced into 60Mpa, after the completion of pressurization, start to warm up in sintering, sintering process, 600 DEG C with
Under, heating rate be 20 DEG C/min, more than 600 DEG C after heating rate be 65 DEG C/min, rise to after 1400 DEG C, keeping temperature
10min, afterwards according to 30 DEG C/min rate reduction temperature to normal temperature, drain pressure after the completion of sintering takes out the demoulding, as institute
State electronic package material.
Embodiment 2
A kind of preparation method of the electronic package material with radiation-resisting functional, comprises the following steps：
(1) after being well mixed 50 parts of SiO 2 powder, 60 parts of aluminium powder, 50 parts of tungsten powder, as in stove, hydrogen is passed through,
It is 300 DEG C to adjust temperature, after roasting 3h, 10 parts of ground and mixeds of mixture and lime powder are uniform, sieving, and mesh number is 400
Mesh；
(2) mixture after sieving is placed in graphite jig, in advance in sleeve lining and upper push-down head pad carbon paper, afterwards
Graphite jig and mixture are put into baking oven together to dry under the conditions of 130 DEG C, it is compressing with 4Mpa pressure after the completion of drying；
(3) graphite jig that will be equipped with mixture is placed in plasma sintering stove, is closed after fire door, after vacuumizing,
Be passed through pressurized with hydrogen thereto, be forced into 80Mpa, after the completion of pressurization, start to warm up in sintering, sintering process, 600 DEG C with
Under, heating rate be 20 DEG C/min, more than 600 DEG C after heating rate be 65 DEG C/min, rise to after 1400 DEG C, keeping temperature
10min, afterwards according to 30 DEG C/min rate reduction temperature to normal temperature, drain pressure after the completion of sintering takes out the demoulding, as institute
State electronic package material.
Embodiment 3
A kind of preparation method of the electronic package material with radiation-resisting functional, comprises the following steps：
(1) after being well mixed 20 parts of SiO 2 powder, 60 parts of aluminium powder, 30 parts of tungsten powder, as in stove, hydrogen is passed through,
It is 300 DEG C to adjust temperature, after roasting 1h, 10 parts of ground and mixeds of mixture and lime powder are uniform, sieving, and mesh number is 300
Mesh；
(2) mixture after sieving is placed in graphite jig, in advance in sleeve lining and upper push-down head pad carbon paper, afterwards
Graphite jig and mixture are put into baking oven together to dry under the conditions of 130 DEG C, it is compressing with 3Mpa pressure after the completion of drying；
(3) graphite jig that will be equipped with mixture is placed in plasma sintering stove, is closed after fire door, after vacuumizing,
Be passed through pressurized with hydrogen thereto, be forced into 80Mpa, after the completion of pressurization, start to warm up in sintering, sintering process, 600 DEG C with
Under, heating rate be 20 DEG C/min, more than 600 DEG C after heating rate be 65 DEG C/min, rise to after 1400 DEG C, keeping temperature
10min, afterwards according to 30 DEG C/min rate reduction temperature to normal temperature, drain pressure after the completion of sintering takes out the demoulding, as institute
State electronic package material.
Embodiment 4
A kind of preparation method of the electronic package material with radiation-resisting functional, comprises the following steps：
(1) after being well mixed 50 parts of SiO 2 powder, 30 parts of aluminium powder, 50 parts of tungsten powder, as in stove, hydrogen is passed through,
It is 200 DEG C to adjust temperature, after roasting 3h, 5 parts of ground and mixeds of mixture and lime powder are uniform, sieving, and mesh number is 400
Mesh；
(2) mixture after sieving is placed in graphite jig, in advance in sleeve lining and upper push-down head pad carbon paper, afterwards
Graphite jig and mixture are put into baking oven together to dry under the conditions of 110 DEG C, it is compressing with 4Mpa pressure after the completion of drying；
(3) graphite jig that will be equipped with mixture is placed in plasma sintering stove, is closed after fire door, after vacuumizing,
Be passed through pressurized with hydrogen thereto, be forced into 60Mpa, after the completion of pressurization, start to warm up in sintering, sintering process, 600 DEG C with
Under, heating rate be 20 DEG C/min, more than 600 DEG C after heating rate be 65 DEG C/min, rise to after 1400 DEG C, keeping temperature
10min, afterwards according to 30 DEG C/min rate reduction temperature to normal temperature, drain pressure after the completion of sintering takes out the demoulding, as institute
State electronic package material.
Embodiment 5
A kind of preparation method of the electronic package material with radiation-resisting functional, comprises the following steps：
(1) after being well mixed 30 parts of SiO 2 powder, 40 parts of aluminium powder, 40 parts of tungsten powder, as in stove, hydrogen is passed through,
It is 250 DEG C to adjust temperature, after roasting 2h, 8 parts of ground and mixeds of mixture and lime powder are uniform, sieving, and mesh number is 300
Mesh；
(2) mixture after sieving is placed in graphite jig, in advance in sleeve lining and upper push-down head pad carbon paper, afterwards
Graphite jig and mixture are put into baking oven together to dry under the conditions of 120 DEG C, it is compressing with 4Mpa pressure after the completion of drying；
(3) graphite jig that will be equipped with mixture is placed in plasma sintering stove, is closed after fire door, after vacuumizing,
Be passed through pressurized with hydrogen thereto, be forced into 70Mpa, after the completion of pressurization, start to warm up in sintering, sintering process, 600 DEG C with
Under, heating rate be 20 DEG C/min, more than 600 DEG C after heating rate be 65 DEG C/min, rise to after 1400 DEG C, keeping temperature
10min, afterwards according to 30 DEG C/min rate reduction temperature to normal temperature, drain pressure after the completion of sintering takes out the demoulding, as institute
State electronic package material.
Claims (8)
1. a kind of method for preparing powder metallurgy of metal-based compound electronics encapsulating material, it is characterised in that comprise the following steps：
(1) Al-W-Si alloy powders and crystalline flake graphite powder are prepared respectively using PREP method, by scale stone
Ink powder end carries out chemical nickel plating processing, after being cleaned multiple times afterwards using deionized water and absolute ethyl alcohol, dries, and surface treatment is made
Crystalline flake graphite powder；
(2) the crystalline flake graphite powder prepared in the Al-W-Si alloy powders prepared in step (1) and step (2) is put into planet
In formula ball mill, using positive and negative rotatable ball milling, ball milling speed is that 160-200 turns after/min, ball milling 3-5h, and two kinds of powder are abundant
It is well mixed；
(3) mixed-powder is handled compressing using isostatic cool pressing, pressure is 200-300Mpa, and the dwell time is 8-15min,
Pressed compact is made, pressed compact is placed in graphite jig, is placed in plasma sintering stove, closes after fire door, vacuumizes, be passed through lazy
Property gas pressurized, after the completion of pressurization, start to warm up drain pressure after the completion of sintering, sintering, take out the demoulding, as described Metal Substrate
Composite electron encapsulating material.
2. the method for preparing powder metallurgy of metal-based compound electronics encapsulating material according to claim 1, it is characterised in that：
In the Al-W-Si alloys, Al mass fractions are 55-60%, and W mass fractions are 15-24%, and surplus is Si.
3. the method for preparing powder metallurgy of metal-based compound electronics encapsulating material according to claim 1, it is characterised in that：
The nickel plating solution that the nickel process is used be nickel sulfate 30-50g/L, sodium hypophosphite 15-28g/L, lactic acid 40-50g/L,
Sodium citrate 20-55g/L, succinic acid 18-32g/L, dodecyldimethylammonium hydroxide inner salt 1-2g/L.
4. the method for preparing powder metallurgy of metal-based compound electronics encapsulating material according to claim 1, it is characterised in that：
The crystalline flake graphite powder plating nickel on surface thickness degree is 2-7 μm.
5. the method for preparing powder metallurgy of metal-based compound electronics encapsulating material according to claim 1, it is characterised in that：
Drying process is dried using vacuum drying chamber in the step (1), and temperature is 110 DEG C.
6. the method for preparing powder metallurgy of metal-based compound electronics encapsulating material according to claim 1, it is characterised in that：
Pressure in the sintering process is 60-80Mpa.
7. the method for preparing powder metallurgy of metal-based compound electronics encapsulating material according to claim 1, it is characterised in that：
In the heating sintering process：Below 600 DEG C, heating rate be 20 DEG C/min, more than 600 DEG C after heating rate be 65 DEG C/
Min, rises to after 1400 DEG C, keeping temperature 10min, afterwards according to 30 DEG C/min rate reduction temperature to normal temperature.
8. a kind of metal-based compound electronics encapsulating material, it is characterised in that：Prepared as the method described in claim any one of 1-7
Form.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108300925A (en) * | 2017-12-27 | 2018-07-20 | 柳州璞智科技有限公司 | A kind of METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING and preparation method thereof |
| CN109434124A (en) * | 2018-11-20 | 2019-03-08 | 许文强 | A kind of preparation method of the low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108300925A (en) * | 2017-12-27 | 2018-07-20 | 柳州璞智科技有限公司 | A kind of METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING and preparation method thereof |
| CN109434124A (en) * | 2018-11-20 | 2019-03-08 | 许文强 | A kind of preparation method of the low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene |
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