CN102701741A - Preparation method for improved electronic packaging material with high heat conductivity - Google Patents
Preparation method for improved electronic packaging material with high heat conductivity Download PDFInfo
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- CN102701741A CN102701741A CN2012101922835A CN201210192283A CN102701741A CN 102701741 A CN102701741 A CN 102701741A CN 2012101922835 A CN2012101922835 A CN 2012101922835A CN 201210192283 A CN201210192283 A CN 201210192283A CN 102701741 A CN102701741 A CN 102701741A
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Abstract
The invention relates to a preparation method for an improved electronic packaging material with high heat conductivity. The preparation method comprises the following steps of: (1) selecting diamonds and silicon powder as initial materials, and adding titanium powder and aluminium nitride as sintering accelerating agents; (2) fully and uniformly mixing the components; (3) selecting a graphite die with the diameter of 20mm, placing the mixture in a graphite container and placing the graphite container in a discharge plasma sintering furnace; (4) vacuumizing the discharge plasma sintering furnace, and starting rapid sintering when the vacuum degree is below 12-15Pa; (5) in the sintering process, setting the pressure to be 35-39Mpa, the temperature rising speed to be 80-120 DEG C/minute and the sintering temperature to be 1280-1320 DEG C, maintaining the sintering temperature for 4-5 minutes after reaching the sintering temperature, and sintering at a vacuum or inert gas environment; and (6) after ending sintering, carrying out furnace cooling on the product, and taking off the pressure at the temperature of 900-950 DEG C. The preparation method has the advantages that the equipment and technology are simple, the synthesis temperature is low, the density of the product is furthest increased, the microcracks of the product are reduced, and the combination property of the product is good.
Description
Technical field
The present invention relates to a kind of preparation method of electronic package material, relate in particular to a kind of preparation method of diamond-silicon composite.
Background technology
Development of modern science and technology improves the requirement of material day by day.In the Electronic Packaging field, along with the complicacy and the intensive of components and parts in electron device and the electronic installation improves day by day, the exploitation excellent performance, the electronic devices and components enclosed chip that can satisfy various requirement has become the task of top priority.
The Electronic Packaging substrate material is a kind of base electronic component, is used to carry electronic devices and components and phase interconnection line thereof, and the matrix with good electrical insulativity.Therefore enclosed chip must keep good coupling with components and parts placed on it aspect electrical properties, physical properties, chemical property.Usually, enclosed chip should possess following character: (1) heat conductivility is good.Thermal conductivity is one of main performance index of Electronic Packaging substrate material.To influence the life-span of electronics and operation conditions in addition if enclosed chip can not in time dispel the heat, temperature distributing disproportionation is even also can to cause electronic device noise to increase greatly; (2) linear expansivity coupling (main and Si and GaAs).If the two thermal expansivity differs bigger, the rapid thermal cycles during electron device work is prone to introduce thermal stresses and causes losing efficacy; (3) high frequency characteristics is good, promptly low specific inductivity and low dielectric loss.Because on high-speed transfer wiring lines circuit, be directly proportional with substrate material specific inductivity square root signal delay time.For satisfying requirement, require the enclosed chip material dielectric constant low as high-speed transfer speed device.In addition, the Electronic Packaging substrate also should have the mechanical property height, electrical insulation capability is good, chemical property is stable (Corrosion of Metallic Materials is used in electroplating processes liquid, wiring), be easy to characteristics such as processing.Certainly, in practical application and large-scale commercial prodn, price factor also is a very important aspect.
The kind of Electronic Packaging substrate material is a lot, and common used material comprises: pottery, metal and metal-base composites, diamond etc.Some material has been obtained comparatively sophisticated application on Electronic Packaging.But with regard to above-mentioned various performance requriementss, most materials all can not satisfy above-mentioned all requirements.
Stupalith is a kind of substrate material commonly used in the Electronic Packaging; Its major advantage is: high insulating property and excellent high frequency characteristics; Have the linear expansivity close with components and parts, very high chemicalstability and thermal conductivity (λ) preferably, in addition; Stupalith also has good comprehensive performances, is widely used in hybrid integrated circuit (HIC) and multicore sheet module (MCM) ceramic packing and often is multi-layered ceramic substrate (MLC).This technology starts from the casting technique patent of JL Park in 1961 invention, and the originator of ceramic packing is considered to Bernard Schwartz, because of research department's exploitation of his leader and have the encapsulation technology patents of many relevant MLC.From the sixties so far, lamination multi-layered ceramic substrate and packaged material and technology are studied and released in developed countries such as U.S.A, day in succession, ceramic substrate has been one of several kinds of high-performance ceramicss of widespread use in the world today.At present, the high heat-conducting ceramic substrate material that has been used for actual production and Application and Development mainly comprises Al2O3, AlN, SiC and BeO etc.
The metal-base composites that is used for enclosed chip is mainly Cu base and Al based composites.The Cu based composites adopts materials such as C fiber, B fiber etc., SiC particle to do the enhancing body, and the fibre-reinforced low bulk that obtains, high heat conduction Cu based composites have better comprehensive performance.For example the superficial expansivity of P130 graphite fibre Reinforced Cu-Base Composites is 6.5 * 10-6/K, and is keeping can also adding among the high thermal Cu W, Mo and low expansion alloy powder such as (like the FeNi alloys).When making W/Cu or Mo/Cu matrix material, Cu is penetrated in porous W, the Mo agglomerate, to keep the continuity of each phase.The linear expansivity of this material can be adjusted according to the variation of constituent element relative content, yet the copper body material exists that wettability is low, thermal expansivity and density is all than problems such as height.Aluminum matrix composite not only has characteristics such as specific tenacity, specific rigidity height; And good heat conductivity, linear expansivity is adjustable, density is lower; Selection as the Electronic Packaging components and parts; Enhancing body commonly used comprises C, B, carbide (like SiC, TiC), nitride (like Si3N4) and oxide compound (like Al2O3, SiO2), and matrix alloy then can be pure Al or alloy.Because the linear expansivity of duraluminum itself is bigger, for making semiconductor materials such as its linear expansivity and Si, Ge, GaAs close, usually has to adopt the enhancing body of high-volume fractional compound with it, addition even up to 70%.
Natural diamond has as semiconductor packages the most excellent necessary character, like high thermal conductivity (2000 W/mK, 25 ℃), low-k (5.5), high resistivity (1016 Ω cm) and breaking down field strength (1000 kV/ mm).From the 60's of this century; Microelectronics circle begins to utilize the effort of diamond as the semiconductor packages substrate; And with diamond as heat sink material, be used on microwave avalanche diode, Ge IMPATT and the laser apparatus, successfully improved their output rating.But the restriction of diamond synthesis fancy price and size under natural diamond or the HTHP makes this technology can't large-scale promotion.Comparatively ideal is to be equipped with matrix material with diamond particles as strengthening system; The HIGH-PURITY SILICON material has lower density, high heat-conducting property and lower thermal expansivity; Silicon and diamond wettability are good; Generate silit at silicon and diamond interface place in the sintering process, reduced interface resistance.Therefore, the diamond/carbon silicon composite becomes one of focus of electronic package material research at present.
Because diamond easy greying when high temperature; Prior art for preparing diamond-silicon carbide composite material by adopting be infiltration method, specifically be with diamond and silica flour layering assembling, and be pressurized to very high force value; At high temperature carry out sintering again; This method is high to production environment, production unit and operation technological requirement, and the finished product rate is low, and manufacturing cost is very high.
Summary of the invention
The object of the present invention is to provide a kind of improved high heat conductance electronic package material preparation method, this method prepared composite material interface contact is firm, and preparation technology is simple, and density and thermal property are significantly increased.
To achieve these goals, the technology side of the present invention's employing is: a kind of improved high heat conductance electronic package material preparation method is characterized in that this method comprises the steps:
1) selecting granularity is the diamond of 18～23 μ m, and granularity is 40～45 μ m, purity at 99. 99% silica flour as original material, and adds titanium valve and aluminium nitride AlN as sintering aids; The ratio of weight and number of diamond, silica flour, titanium valve, aluminium nitride AlN is 19.6～30.4:27.2～33.3:0.53～0.93:0.5 ~ 1.3;
2) with the said components thorough mixing evenly after;
3) select the graphite jig of φ 20 mm, with pack into crystal vessel and put into the discharge plasma sintering stove of said mixture;
4) at the discharge plasma sintering stove evacuation, when vacuum tightness reaches the Fast Sintering of beginning below 12 ~ 15Pa;
5) institute's stress is 35～39MPa in the sintering process, and heat-up rate is 80 ~ 120 ℃/minute, and sintering temperature is set at 1280～1320 ℃, reach after the sintering temperature to keep 4-5 minute, and under vacuum or inert gas environment sintering;
6) sintering finishes the back product is carried out furnace cooling and lays down pressure 900-950 ℃ the time.
Discharge plasma sintering (Spark Plasma Sintering; SPS) be a kind of novel Fast Sintering technology that development in recent years is got up; It melts plasma activation, hot pressing is one; Have that heat-up rate is fast, sintering time is short, cooling rapidly, impressed pressure and characteristics such as sintering atmosphere is controlled, energy-conserving and environment-protective; But discharging plasma sintering equipment is similar to hot-pressed sintering furnace, and different is to add the controllable pulse electric current to a pressure-bearing conductive die, through galvanic size control heat-up rate of regulating impulse and sintering temperature.Also do not see at present the report that discharge plasma sintering technique is used to prepare diamond-silicon composite.
The present invention specifically applies to the preparation of diamond-silicon composite with discharge plasma sintering, makes the silicon substrate particle under the silicon fusing point, in-situ chemical reaction take place in sintering process and diamond particles, generates the interface silicon carbide layer.And the present invention is through a large amount of tests, selected best set of dispense than and processing parameter, can effectively stop the diamond greying in utmost point chien shih sample densification in short-term.In addition, through adding titanium valve and aluminium nitride AlN as auxiliary agent, reduced the fusing point of silicon, improved sintered density thereby reduced sintering temperature, and compared with aluminium powder, used titanium valve can increase the thermal conductivity of product, aluminium nitride AlN stops the diamond greying simultaneously.
Beneficial effect of the present invention is; Equipment and technology are simple, synthesis temperature is low, and prepared matrix material density reaches more than 99%, and thermal conductivity is 480-510W/mK; Thereby farthest improve the product density, reduce the product tiny crack, The comprehensive performance is good.
Embodiment
Below set forth technical scheme of the present invention through specific embodiment; Wherein, The discharge plasma sintering stove (SPS) that Fast Sintering adopted among the present invention is the Dr Sinter that SUMITOMO CHEMICAL stone carbon mining industry Co., Ltd. produces, SPS-1050 discharge plasma sintering stove.
Embodiment 1:
1) selecting granularity is the diamond of 19 μ m, and granularity is 40 μ m, purity at 99. 99% silica flour as original material, and adds titanium valve and aluminium nitride AlN as sintering aids; The ratio of weight and number of diamond, silica flour, titanium valve, aluminium nitride AlN is 19.6:33.3:0.93:0.5;
2) with the said components thorough mixing evenly after;
3) select the graphite jig of φ 20 mm, with pack into crystal vessel and put into the discharge plasma sintering stove of said mixture;
4),, vacuum tightness begins Fast Sintering below the 12Pa when reaching at the discharge plasma sintering stove evacuation;
5) institute's stress is 35MPa in the sintering process, and heat-up rate is 120 ℃/minute, and sintering temperature is set at 1280 ℃, reach after the sintering temperature to keep 4 minutes, and under vacuum or inert gas environment sintering;
6) sintering finishes the back product is carried out furnace cooling and lays down pressure 950 ℃ the time.
Through test, the density of the product that obtains is more than 99.2%, and thermal conductivity is 529W/mK.
Embodiment 2:
1) selecting granularity is the diamond of 23 μ m, and granularity is 45 μ m, purity at 99. 99% silica flour as original material, and adds titanium valve and aluminium nitride AlN as sintering aids; The ratio of weight and number of diamond, silica flour, titanium valve, aluminium nitride AlN is 30.4:27.2:0.53:1.3;
2) with the said components thorough mixing evenly after;
3) select the graphite jig of φ 20 mm, with pack into crystal vessel and put into the discharge plasma sintering stove of said mixture;
4),, vacuum tightness begins Fast Sintering below the 15Pa when reaching at the discharge plasma sintering stove evacuation;
5) institute's stress is 35MPa in the sintering process, and heat-up rate is 80 ℃/minute, and sintering temperature is set at 1320 ℃, reach after the sintering temperature to keep 5 minutes, and under vacuum or inert gas environment sintering;
6) sintering finishes the back product is carried out furnace cooling and lays down pressure 900 ℃ the time.
Through test, its density is more than 99.3%, and thermal conductivity is 531W/mK.
Embodiment 3:
1) selecting granularity is the diamond of 21 μ m, and granularity is 43 μ m, purity at 99. 99% silica flour as original material, and adds titanium valve and aluminium nitride AlN as sintering aids; The ratio of weight and number of diamond, silica flour, titanium valve, aluminium nitride AlN is 21.1:30.2:0.7:0.9;
2) with the said components thorough mixing evenly after;
3) select the graphite jig of φ 20 mm, with pack into crystal vessel and put into the discharge plasma sintering stove of said mixture;
4),, vacuum tightness begins Fast Sintering below the 12Pa when reaching at the discharge plasma sintering stove evacuation;
5) institute's stress is 38MPa in the sintering process, and heat-up rate is 100 ℃/minute, and sintering temperature is set at 1300 ℃, reach after the sintering temperature to keep 5 minutes, and under vacuum or inert gas environment sintering;
6) sintering finishes the back product is carried out furnace cooling and lays down pressure 940 ℃ the time.
Through test, its density is more than 99.5%, and thermal conductivity is 523W/mK.
Claims (1)
1. an improved high heat conductance electronic package material preparation method is characterized in that this method comprises the steps:
1) selecting granularity is the diamond of 18～23 μ m, and granularity is 40～45 μ m, purity at 99. 99% silica flour as original material, and adds titanium valve and aluminium nitride AlN as sintering aids; The ratio of weight and number of diamond, silica flour, titanium valve, aluminium nitride AlN is 19.6～30.4:27.2～33.3:0.53～0.93:0.5 ~ 1.3;
2) with the said components thorough mixing evenly after;
3) select the graphite jig of φ 20 mm, with pack into crystal vessel and put into the discharge plasma sintering stove of said mixture;
4) at the discharge plasma sintering stove evacuation, when vacuum tightness reaches the Fast Sintering of beginning below 12 ~ 15Pa;
5) institute's stress is 35～39MPa in the sintering process, and heat-up rate is 80 ~ 120 ℃/minute, and sintering temperature is set at 1280～1320 ℃, reach after the sintering temperature to keep 4-5 minute, and under vacuum or inert gas environment sintering;
6) sintering finishes the back product is carried out furnace cooling and lays down pressure 900-950 ℃ the time, obtains product.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673656A (en) * | 2017-01-19 | 2017-05-17 | 北京科技大学 | Method for preparing diamond/silicon carbide composite material by using graphite as carbon source |
| CN110157999A (en) * | 2019-05-09 | 2019-08-23 | 李纳 | A kind of pantograph pan graphite fibre enhancing Cu-base composites |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102690120A (en) * | 2012-06-08 | 2012-09-26 | 黄凯敏 | Improved high-heat-conductance electronic packaging material |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102690120A (en) * | 2012-06-08 | 2012-09-26 | 黄凯敏 | Improved high-heat-conductance electronic packaging material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673656A (en) * | 2017-01-19 | 2017-05-17 | 北京科技大学 | Method for preparing diamond/silicon carbide composite material by using graphite as carbon source |
| CN110157999A (en) * | 2019-05-09 | 2019-08-23 | 李纳 | A kind of pantograph pan graphite fibre enhancing Cu-base composites |
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Application publication date: 20121003 |