CN104046877A - Directional porous SiC-Cu composite material for electronic packaging and preparation method thereof - Google Patents
Directional porous SiC-Cu composite material for electronic packaging and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a directional porous SiC-Cu composite material for electronic packaging and a preparation method thereof. The composite material comprises the following components by volume fraction: 55-70% of SiC reinforcing phase and 30-45% of Cu matrix phase, wherein the matrix phase and the reinforcing phase are alternately continuous. According to the preparation method, a uniform and continuous metal tungsten layer is coated on the inner surface of the directional porous SiC ceramic by combining a vacuum sol-gel impregnation technology with a hydrogen gas reduction method, so that the problem of wettability of the SiC and the Cu is solved, spontaneous infiltration can be easily carried out, furthermore, the Cu gives full play to high thermal conductivity, and the thermophysical properties of the composite material can be improved remarkably. The preparation method is simple, has low cost and can be used for preparing composite materials of various complicated shapes.
Description
Technical field
The present invention relates to a kind of ceramic-metal composite material used for electronic packaging and preparation method.
Background technology
Along with the develop rapidly of unicircuit, require electronic package material to there is high thermal conductivity, low thermal expansivity and low density.Traditional electronic package material, as Cu/W, Cu/Mo, Invar/Cu etc. are difficult to take into account the requirement to above-mentioned various performances simultaneously, although this type of matrix material has high thermal conductivity and low thermal expansivity, but it is too large that shortcoming is density, not only increase package quality, and poor air-tightness, affect encapsulation performance.SiC/Cu matrix material can combine the characteristic of the high heat conduction of Cu and SiC low density, low thermal coefficient of expansion, as desirable structure-functions formed material, become one of focus of Electronic Packaging area research and application in recent years, there is very large commercial promise.
That at present research is more is SiC Particles Reinforced Cu-Base Composites (SiCp/Cu), as " preparing SiC particle reinforced composite material electronic package shell technique with semi-soild-state technology " (Chinese patent 200710119013.0), " a kind of high heat-conducting copper-based composite material and preparation method thereof " (Chinese patent 200710178844.5), " silicon carbide/copper metal ceramic high temperature electric contact composite material preparation method " (Chinese patent 03126354.2) etc.And it is fewer to the research of three-dimensional network SiC ceramic skeleton Reinforced Cu-Base Composites.Existing experimental study shows with model analysis result: in the time that wild phase volume fraction is identical, three-dimensional network SiC ceramic skeleton Reinforced Cu-Base Composites has higher thermal conductivity and lower thermal expansivity than SiCp/Cu matrix material.Particularly, if while being orienting stephanoporate structure as the porous SiC ceramics of wild phase, the performance of matrix material will show obvious anisotropy, there is the thermal expansivity matching and thering is higher thermal conductivity in vertical this plane with the in-plane at semiconducter device place, thereby be both conducive to reduce the thermal stresses between packaged material and semi-conductor, the heat that semi-conductor can be produced again passes to heat sink and loose removing in time, ensures the normal working efficiency of semi-conductor and work-ing life.Therefore, directional three-dimensional network SiC ceramic skeleton Reinforced Cu-Base Composites is more suitable for for Electronic Packaging.
Because the wettability between SiC and Cu is poor, therefore conventionally adopt pressure casting method to prepare SiC/Cu matrix material.As " a kind of properties of SiC foam ceramics strengthens Cu-base composites friction plate and preparation method " (Chinese patent 200610045647.1), " bi-continuous-phase composite friction material of foaming silicon carbide/metal and member thereof and preparation " (Chinese patent 200610046242.X) etc.Utilize pressure casting method to prepare matrix material and have following shortcoming: in (1) sample, understand lingering section pore, therefore can worsen the thermal characteristics of matrix material; (2) the complex-shaped property of part is restricted; (3) in pressure process, prefabricated component is easily destroyed; (4) having relatively high expectations to mould.With respect to squeeze casting method, pressureless infiltration is not owing to needing special die casting equipment and specific mould, and therefore preparation technology is simple, cost is low.The more important thing is, it can produce the large-sized composite material of various complicated shapes as a kind of near-net-shape preparation technology.But because the wettability between SiC and Cu is poor, be difficult to realize the quick spontaneous infiltration under passive state.In addition, SiC and the Cu generation cupro silicon that at high temperature easily reacts, this greatly reduces the thermal conductivity of copper metallographic phase, the heat physical properties of severe exacerbation matrix material.Therefore the reactivity of, how improving between wettability and inhibition SiC and the Cu between SiC and Cu has become the key issue that Spontaneous Melt Infiltration is prepared directional three-dimensional network SiC ceramic skeleton Reinforced Cu-Base Composites.
The method of improving the wettability between SiC and Cu mainly contains: (1) Cu matrix alloy, as " a kind of method of preparing high volume-fraction carborundum granule-reinforced copper-based composite material " (Chinese patent 200710177026.3), " a kind of silicon carbide/cupro silicon bicontinuous phase compound material and preparation method thereof " (Chinese patent 201210429043.2) etc.; (2) SiC ceramic surface metallization, as " SiC ceramic grain surface tangsten plating process " (Chinese patent 200510029906.7), " method of SiC particle surface plating tungsten " (Chinese patent 201210125165.2), " preparation method of tungsten-plated SiC particle reinforced copper-based composite material used for electronic packaging " (Chinese patent 200910055976.8) etc.After Cu matrix alloy, can greatly reduce the thermal conductivity of Cu, thereby reduce the heat physical properties of matrix material, be not therefore suitable for preparation SiC/Cu matrix material used for electronic packaging.Can give full play to the feature of the high heat conduction of Cu matrix for ceramic surface metal lining coating, metal W has the thermal expansivity close with SiC, contribute to form one deck dense coating at SiC ceramic surface, and wettability between W and Cu is good and be difficult for reacting, it is ideal porous SiC ceramics coating on inner surface material, but so far, at home and abroad there is no the open source literature report of being prepared by the ceramic porous internal surface metallizing of SiC W coating to three-dimensional network SiC ceramic skeleton Reinforced Cu-Base Composites.
Summary of the invention
The object of the invention is to, provide that a kind of in-plane and semiconducter device coefficient of thermal expansion match, vertical direction has high heat conductance, low-density directional hole three-dimensional network SiC ceramic skeleton Reinforced Cu-Base Composites used for electronic packaging; And prepare the method for this matrix material based on pressureless infiltration technique.
For reaching above object, the present invention takes following technical scheme to be achieved:
A kind of orienting stephanoporate SiC-Cu matrix material used for electronic packaging, it is characterized in that: by volume mark meter, SiC ceramic phase by 55～70% and 30～45% Cu metallographic phase form block, wherein SiC ceramic phase is porous skeleton structure, these holes are roughly arranged and are interconnected towards a direction, form three-dimensional network shape directed porosity, these directed porosity surfaces are with tungsten, and Cu metallographic phase infiltration is on tungsten and completely by the filling of three-dimensional network shape directed porosity.
The preparation method of above-mentioned orienting stephanoporate SiC-Cu matrix material used for electronic packaging, is characterized in that, comprises the steps:
The first step, prepares orienting stephanoporate SiC pottery
(1) press mass percent, by SiC powder 80～95%, Si
3n
4powder 5～20% ball millings mix rear dry, add account for mixture quality per-cent be 5% polyvinyl alcohol solution as binding agent, after mixing, sieve, compression molding, makes SiC green compact after dry at 80 DEG C;
(2) SiC green compact are placed in to intermediate frequency electromagnetic induction sintering furnace, under vacuum condition, are warming up to 1900～2200 DEG C, be incubated 3 hours, after furnace cooling, obtain having the porous SiC ceramics of three-dimensional network shape directed porosity.
Second step, at orienting stephanoporate SiC pottery three-dimensional network shape internal pore surface metallizing W layer
(1) orienting stephanoporate SiC pottery being put into massfraction is that 65% concentrated nitric acid carries out roughening treatment, after sonic oscillation, takes out, and rinses well with deionized water;
(2) by the orienting stephanoporate SiC pottery after alligatoring at WO
3after flooding 30min in colloidal sol, take out, repeatedly flood 3～6 times;
(3) by after dry the orienting stephanoporate SiC pottery after alligatoring dipping, under the hydrogen of 700～900 DEG C and argon gas mixed atmosphere, reduce 3h, after furnace cooling, take out, obtain three-dimensional network shape internal pore surface and be coated with the orienting stephanoporate SiC pottery of tungsten;
The 3rd step, adopts Spontaneous Melt Infiltration technique to make the compound of orienting stephanoporate SiC pottery and Cu metal
(1) mark by volume, is placed in 30～45% pure Cu and 55～70% second steps (3) gained orienting stephanoporate SiC pottery in high-temperature crucible, puts into vacuum oven;
(2) vacuum oven is evacuated to below 0.01Pa, is warming up to subsequently 1200～1400 DEG C, under vacuum tightness≤100Pa, insulation 3h carries out vacuum infiltration, and last furnace cooling, takes out crucible, obtains orienting stephanoporate SiC-Cu matrix material.
In above method, the particle size of the described SiC powder of the first step step (1) is 100 microns; Described Si
3n
4the particle size of powder is 3 microns.The mass concentration of the described polyvinyl alcohol solution of the first step step (1) is 10%.
The described WO of second step step (2)
3colloidal sol, preparation by the following method: the hydrogen peroxide that is 30% with the concentration of 800ml by the tungsten powder of 130g reacts 10 DEG C of left and right, after question response is complete, filter out resistates, add the Glacial acetic acid of 800ml to mix, the 24h that refluxes at 60 DEG C, obtains yellow solution, obtains solid state powder after vacuum-drying, this solid state powder of 20g is dissolved in 60ml ethanol, obtains WO
3colloidal sol.
The hydrogen that second step step (3) is described and the volume ratio of argon gas are 1:4.
The described dipping of second step step (2) is to carry out under vacuum condition.
Compared with prior art, tool of the present invention has the following advantages:
1. the orienting stephanoporate SiC-Cu matrix material that prepared by the present invention, not only there is high thermal conductivity and low thermal expansivity, and heat physical properties shows obvious anisotropy, there is the thermal expansivity matching and thering is higher thermal conductivity in vertical this plane with the in-plane at semiconducter device place, thereby be both conducive to reduce the thermal stresses between packaged material and semi-conductor, the heat that semi-conductor can be produced again passes to heat sink and loose removing in time, ensures the normal working efficiency of semi-conductor and work-ing life.Therefore more can meet the performance requriements of electronic package material.
2. the present invention adopts vacuum sol-gel dipping in conjunction with hydrogen reduction method even continuous metal tungsten layer in orienting stephanoporate SiC pottery three-dimensional network shape hole, can not only conveniently control the thickness of plating tungsten layer, easy to operate, with low cost, and be applicable to the processing of any complicated shape porous SiC ceramics internal surface plating tungsten.
3. the present invention is by improving the wettability and reactivity between SiC and Cu at orienting stephanoporate SiC pottery three-dimensional network shape directed porosity internal surface metallizing tungsten layer, make Spontaneous Melt Infiltration be easy to carry out on the one hand, can suppress on the other hand reacting between SiC and Cu, can give full play to the high heat conduction advantage of metal Cu, obviously improve the thermal conductivity of SiC/Cu matrix material.
4. Spontaneous Melt Infiltration technique of the present invention is as a kind of near-net-shape preparation technology, with respect to Extrution casting technique, owing to not needing special die casting equipment and specific mould, therefore preparation technology is simple, cost is low, can produce the matrix material of various complicated shapes.
Brief description of the drawings
Fig. 1 is the orienting stephanoporate SiC-Cu matrix material microstructure photograph of the embodiment of the present invention 1.Wherein a figure is micropore lateral cross section; B figure is micropore longitudinal cross-section.
Embodiment
Below by form (specific embodiment), the present invention is described in further detail by reference to the accompanying drawings.
A kind of orienting stephanoporate SiC-Cu matrix material used for electronic packaging, by volume mark meter, the SiC ceramic phase and the Cu metallographic phase that are made up of table 1 form block, wherein SiC ceramic phase is porous skeleton structure, these holes are roughly arranged and are interconnected towards a direction, form three-dimensional network shape directed porosity, these directed porosity surfaces are with tungsten, and Cu metallographic phase infiltration is on tungsten and completely by three-dimensional network shape directed porosity filling (referring to Fig. 1).
The preparation method of SiC-Cu matrix material of the present invention, comprises the steps:
The first step, prepare orienting stephanoporate SiC pottery:
Step 1: press mass percent, take particle size and be the SiC powder of 100 microns, particle size is the Si of 3 microns
3n
4powder (ratio is referring to table 1), after mixing, ball milling is dried 10 hours under the condition of 85 ± 5 DEG C, add that to account for mixture quality per-cent be that 5% the mass concentration polyvinyl alcohol solution that is 10% is as binding agent, be ground rear mistake 200 mesh sieves, under the condition that is 200MPa at pressure, be molded into growth footpath than the disk base substrate of 1:3, then dry 20h in 80 DEG C of baking ovens, makes SiC green compact;
Step 2: the SiC green compact in step 1 are placed in to intermediate frequency (2.5kHZ) electromagnetic induction sintering oven, furnace temperature is risen to the listed different sintering temperature of table 1 by temperature rise rate with 50 DEG C/min under vacuum condition, be incubated 3 hours, after furnace cooling, obtain thering is the porous SiC ceramics that aligns three-dimensional network shape hole.
Second step, at orienting stephanoporate SiC pottery three-dimensional network shape internal pore surface metallizing W layer, comprises the following steps:
Step 1: first orienting stephanoporate SiC pottery is put into massfraction and be 65% concentrated nitric acid and carry out roughening treatment, take out after sonic oscillation 10min, rinse well with deionized water;
Step 2: the orienting stephanoporate SiC pottery after alligatoring is immersed in to WO
3in colloidal sol, take out flood 30min under negative pressure of vacuum after, repeatedly repeatedly (specifically referring to table 1) of dipping.Wherein, WO
3the preparation method of colloidal sol is: the hydrogen peroxide that is 30% with the concentration of 800ml by the tungsten powder of 130g reacts 10 DEG C of left and right, after question response is complete, filter out resistates, add the Glacial acetic acid of 800ml to mix, 24h refluxes at 60 DEG C, obtain yellow solution, after vacuum-drying 6h, obtain solid state powder; 20g solid state powder is dissolved in the ethanol of 60ml, obtains WO
3colloidal sol.
Step 3: orienting stephanoporate SiC pottery after treatment step 2 is put into the dry 3h of loft drier of 350 DEG C, then reduced 3h (reduction temperature is referring to table 1) under hydrogen and argon gas mixed atmosphere, wherein the volume ratio of hydrogen and argon gas is 1:4.After furnace cooling, take out, obtain three-dimensional network shape internal pore surface and be coated with the orienting stephanoporate SiC pottery of metal W.
The 3rd step, makes in the three-dimensional network hole of the spontaneous infiltration orienting stephanoporate of Cu SiC pottery of melting, and concrete steps are as follows:
Step 1: by volume mark, the orienting stephanoporate SiC pottery after three-dimensional network shape internal pore surface metallizing tungsten is placed in to high-temperature crucible with pure Cu, then put into together vacuum oven, wherein, the volume ratio of orienting stephanoporate SiC pottery and pure Cu is referring to table 1.
Step 2: vacuum oven is evacuated to below 0.01Pa, be warming up to infiltrating temperature (referring to table 1) with the speed of 10 DEG C/min subsequently, under vacuum tightness≤100Pa, insulation 3h carries out Spontaneous Melt Infiltration, obtains orienting stephanoporate SiC-Cu matrix material after furnace cooling.
Table 1 forms and processing parameter
Claims (7)
1. an orienting stephanoporate SiC-Cu matrix material used for electronic packaging, it is characterized in that: by volume mark meter, SiC ceramic phase by 55～70% and 30～45% Cu metallographic phase form block, wherein SiC ceramic phase is porous skeleton structure, these holes are roughly arranged and are interconnected towards a direction, form three-dimensional network shape directed porosity, these directed porosity surfaces are with tungsten, and Cu metallographic phase infiltration is on tungsten and completely by the filling of three-dimensional network shape directed porosity.
2. a preparation method for orienting stephanoporate SiC-Cu matrix material used for electronic packaging, is characterized in that, comprises the steps:
The first step, prepares orienting stephanoporate SiC pottery
(1) press mass percent, by SiC powder 80～95%, Si
3n
4powder 5～20% ball millings mix rear dry, add account for mixture quality per-cent be 5% polyvinyl alcohol solution as binding agent, after mixing, sieve, compression molding, makes SiC green compact after dry at 80 DEG C;
(2) SiC green compact are placed in to intermediate frequency electromagnetic induction sintering furnace, under vacuum condition, are warming up to 1900～2200 DEG C, be incubated 3 hours, after furnace cooling, obtain having the porous SiC ceramics of three-dimensional network shape directed porosity;
Second step, at orienting stephanoporate SiC pottery three-dimensional network shape internal pore surface metallizing W layer
(1) orienting stephanoporate SiC pottery being put into massfraction is that 65% concentrated nitric acid carries out roughening treatment, after sonic oscillation, takes out, and rinses well with deionized water;
(2) by the orienting stephanoporate SiC pottery after alligatoring at WO
3after flooding 30min in colloidal sol, take out, repeatedly flood 3～6 times;
(3) by after dry the orienting stephanoporate SiC pottery after alligatoring dipping, under the hydrogen of 700～900 DEG C and argon gas mixed atmosphere, reduce 3h, after furnace cooling, take out, obtain three-dimensional network shape internal pore surface and be coated with the orienting stephanoporate SiC pottery of tungsten;
The 3rd step, adopts Spontaneous Melt Infiltration technique to make the compound of orienting stephanoporate SiC pottery and Cu metal
(1) mark by volume, is placed in 30～45% pure Cu and 55～70% second steps (3) gained orienting stephanoporate SiC pottery in high-temperature crucible, puts into vacuum oven;
(2) vacuum oven is evacuated to below 0.01Pa, is warming up to subsequently 1200～1400 DEG C, under vacuum tightness≤100Pa, insulation 3h carries out vacuum infiltration, and last furnace cooling, takes out sample, obtains orienting stephanoporate SiC-Cu matrix material.
3. the preparation method of orienting stephanoporate SiC-Cu matrix material used for electronic packaging as claimed in claim 2, is characterized in that, the particle size of the described SiC powder of the first step step (1) is 100 microns; Described Si
3n
4the particle size of powder is 3 microns.
4. the preparation method of orienting stephanoporate SiC-Cu matrix material used for electronic packaging as claimed in claim 2, is characterized in that, the mass concentration of the described polyvinyl alcohol solution of the first step step (1) is 10%.
5. the preparation method of orienting stephanoporate SiC-Cu matrix material used for electronic packaging as claimed in claim 2, is characterized in that, the described WO of second step step (2)
3colloidal sol, preparation by the following method: the hydrogen peroxide that is 30% with the concentration of 800ml by the tungsten powder of 130g reacts 10 DEG C of left and right, after question response is complete, filter out resistates, add the Glacial acetic acid of 800ml to mix, the 24h that refluxes at 60 DEG C, obtains yellow solution, obtains solid state powder after vacuum-drying, this solid state powder of 20g is dissolved in 60ml ethanol, obtains WO
3colloidal sol.
6. the preparation method of orienting stephanoporate SiC-Cu matrix material used for electronic packaging as claimed in claim 2, is characterized in that, the hydrogen that second step step (3) is described and the volume ratio of argon gas are 1:4.
7. the preparation method of orienting stephanoporate SiC-Cu matrix material used for electronic packaging as claimed in claim 2, is characterized in that, the described dipping of second step step (2) is to carry out under vacuum condition.
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| CN104962771A (en) * | 2015-05-25 | 2015-10-07 | 西安交通大学 | Directional porous SiC and diamond reinforced Al base composite material and preparation method thereof |
| CN108796267A (en) * | 2018-07-05 | 2018-11-13 | 西安航空学院 | A method of CuSiCp composite materials are prepared using differential pressure vacuum foundry engieering |
| CN108796262A (en) * | 2018-06-14 | 2018-11-13 | 中国科学院金属研究所 | SiC reinforcement metal-base composites and preparation method thereof with microcosmic oriented structure |
| CN111235421A (en) * | 2020-01-16 | 2020-06-05 | 长安大学 | Method for preparing SiC particle reinforced Cu-based composite material with high volume fraction by non-pressure infiltration |
| CN113548896A (en) * | 2020-04-23 | 2021-10-26 | 谢金龙 | Method for manufacturing ceramic composite material and product thereof |
| CN113755794A (en) * | 2021-09-16 | 2021-12-07 | 桂林理工大学 | Porous Cu-SiC composite membrane and preparation method thereof |
| CN113930634A (en) * | 2021-09-22 | 2022-01-14 | 郑州航空工业管理学院 | Cu/SiO2-Cu2O/SiC metal matrix composite material and preparation method thereof |
| CN114231812A (en) * | 2021-12-21 | 2022-03-25 | 合肥工业大学 | AlN-W-Cu composite material and preparation method thereof |
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| CN102962434A (en) * | 2012-10-31 | 2013-03-13 | 西安交通大学 | Silicon carbide/copper silicon alloy codual-continuous composite and preparation method thereof |
| CN103382534A (en) * | 2013-06-18 | 2013-11-06 | 武汉理工大学 | W-Cu-SiC ternary composite material and preparation method thereof |
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| CN102962434A (en) * | 2012-10-31 | 2013-03-13 | 西安交通大学 | Silicon carbide/copper silicon alloy codual-continuous composite and preparation method thereof |
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| CN104962771A (en) * | 2015-05-25 | 2015-10-07 | 西安交通大学 | Directional porous SiC and diamond reinforced Al base composite material and preparation method thereof |
| CN108796262A (en) * | 2018-06-14 | 2018-11-13 | 中国科学院金属研究所 | SiC reinforcement metal-base composites and preparation method thereof with microcosmic oriented structure |
| CN108796267A (en) * | 2018-07-05 | 2018-11-13 | 西安航空学院 | A method of CuSiCp composite materials are prepared using differential pressure vacuum foundry engieering |
| CN111235421A (en) * | 2020-01-16 | 2020-06-05 | 长安大学 | Method for preparing SiC particle reinforced Cu-based composite material with high volume fraction by non-pressure infiltration |
| CN113548896A (en) * | 2020-04-23 | 2021-10-26 | 谢金龙 | Method for manufacturing ceramic composite material and product thereof |
| CN113755794A (en) * | 2021-09-16 | 2021-12-07 | 桂林理工大学 | Porous Cu-SiC composite membrane and preparation method thereof |
| CN113755794B (en) * | 2021-09-16 | 2023-08-11 | 桂林理工大学 | Porous Cu-SiC composite film and preparation method thereof |
| CN113930634A (en) * | 2021-09-22 | 2022-01-14 | 郑州航空工业管理学院 | Cu/SiO2-Cu2O/SiC metal matrix composite material and preparation method thereof |
| CN113930634B (en) * | 2021-09-22 | 2022-08-12 | 郑州航空工业管理学院 | Cu/SiO 2 -Cu 2 O/SiC metal matrix composite material and preparation method thereof |
| CN114231812A (en) * | 2021-12-21 | 2022-03-25 | 合肥工业大学 | AlN-W-Cu composite material and preparation method thereof |
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