GB2103250A - Silver-filled glass - Google Patents

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Publication number
GB2103250A
GB2103250A GB08222054A GB8222054A GB2103250A GB 2103250 A GB2103250 A GB 2103250A GB 08222054 A GB08222054 A GB 08222054A GB 8222054 A GB8222054 A GB 8222054A GB 2103250 A GB2103250 A GB 2103250A
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GB
United Kingdom
Prior art keywords
silver
glass
paste
replaced
metallizing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
GB08222054A
Other versions
GB2103250B (en
Inventor
Raymond L Dietz
Michael Featherby
Peter K Margetts
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Johnson Matthey Inc
Original Assignee
Johnson Matthey Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from US06/355,719 external-priority patent/US4401767A/en
Application filed by Johnson Matthey Inc filed Critical Johnson Matthey Inc
Publication of GB2103250A publication Critical patent/GB2103250A/en
Application granted granted Critical
Publication of GB2103250B publication Critical patent/GB2103250B/en
Expired legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
    • C04B41/5116—Ag or Au
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    • H01L2924/19041—Component type being a capacitor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/30—Technical effects
    • H01L2924/35—Mechanical effects
    • H01L2924/351—Thermal stress

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Abstract

A silver metallizing paste for attachment of silicon semi-conductive devices in lead-frame packages, specifically ceramic packages, which is less expensive than a gold preform but useable in hermetic packages, and provides better electrical and thermal conductivity, and higher bond strength, than silver polyimides. From 25 to 95% of silver is blended with a low-melting glass, preferably one having 95-96% PbO, and a paste or ink is formed with a suitable vehicle at 75-86% solids. Use of the paste follows conventional practice. Selection of Ag:glass ratio depends on the type of die bonding to be used. The paste is particularly useful in MOS technology, where low contact resistance is required, and also finds applications as a solder substitute and bonding chip capacitors. It is most advantageous in attachment of larger- area integrated circuits in that stress cracking associated with the gold silicon eutectic is avoided.

Description

SPECIFICATION Silver-filled glass The present invention relates generally to silver metallization and, more particularly, the invention relates to a silver-filled glass composition specifically adapted to bond silicon semiconductive devices to substrates.
Silver metallization compositions had their origins in decorative enamelling, but were adapted early on for use in thick film hybrid circuitry. The attention of early workers was, however, concentrated on designing compositions that would adhere strongly to the ceramic substrate The so-called "Scotch tape test" because an early standard of adhesion.
Knox, U.S. Pat. No. 2 385 580 disclosed high proportions of bismuth oxide in lead borosilicate glasses which was widely used with silver, but was not satisfactory with other noble metals.
Hoffman, U.S. Pat. No. 3 440 182 disclosed additions of vanadium and copper oxides as improving adhesion, solderability and conductivity of noble metal metallizing compositions generally. These compositions were used as conductors, rather than as a medium for attachment of devices such as silicon integrated circuits to the substrates.
In the latter category, gold-based inks or preforms have been the most common, taking advantage of the low-temperature gold-silicon eutectic to achieve a good bond. Even though very substantial efforts have been made to reduce the amount of gold used to make such bonds, its expense mitigates against its use wherever possible.
There has been a great deal of effort over the years to eliminate gold from hermetic packages in the electronics industry. One of the more difficult areas to eliminate gold has been in MOS technology, due to the necessity of having backside low resistance contact; as of now, gold is still the material of choice in this application.
Plastic packaging has nearly eliminated the necessity for gold, with the exceptions of gold bonding wire and gold evaporated on the backside of the wafer. The gold on the frame and gold preform have been eliminated by the use of epoxy and polyimides filled with silver flake in such packages.
Silver-filled polyimides have been used for die attachment in hermetic packages. Because of the problem of final cross linking of polyimides, and the generation of CO, and H20 during sealing, this has not achieved significant volume.
There are no low-temperature phases in the silver-gold system, which is a continuous series of solid solutions, and the silver-silicon system has a eutectic, but a high temperature one (over 8000C.), so systems based on silver must employ a fundamentally different bonding mechanism, indeed one where the silver per se plays little or no part.
Thus, where a gold preform is used to attach a silicon die to a silver metallized surface, the mechanism on one side is the gold-silicon eutectic and on the other it is a solid-liquid diffusion, with the glass playing the major role in terms of bond strength. Being less than a metallurgical bond, the thermal and electric conductivity are not as good as desired.
Pure glass bonds have also been used in this service, but without a conductive element both conductivities suffer, as would be expected.
Regarding silver polyimide compositions, the quantity of silver that can be incorporated is limited, and special processing is necessary (for high-volume manufacturing, uniformity of processing is an important cost consideration).
The biggest drawback of polyimides, or any organic bonding system, is that they can not be used in hermetic packages such as Cerdips, because they are moisture getters, can not be outgassed, and generally can not withstand high temperature used in assembling these packages.
The present invention provides a silver-filled glass that produces strong bonds between the silicon die and the substrate, whether or not the latter is metallized, with controllable thermal and electrical conductivity, and which may be used in hermetic packages.
According to one aspect the invention provides a silver-filled glass metallizing paste comprising: (a) about 75~85% of a solids component made up of: 20 to 95% of finely-divided silver; and 80 to 5% of a low-melting, finely-divided glass frit; (b) organic vehicle; with the privisos that: (i) up to 10% of said silver may be replaced by nickel; (ii) up to 60% of said silver may be replaced by tin; (iii) up to 20% of said silver may De replaced by copper; (iv) a portion of said silver may be replaced by a noble metal such as gold.
According to another aspect, the invention provides a silver-filled glass metallizing paste for bonding silicon semiconductive devices to ceramic substrates comprising: (a) 75~85% of a solids component made up of: 25 to 95% of finely-divided silver having a surface area of 0.7 to 1.0 m2/gm and a tap density of 2.25 to 2.75 g/cc; 75% to 5% of a finely-divided glass frit having a softening point in the range of 3250 to 42500.; and (b) an organic vehicle; with the provisos that: (i) up to 10% of said silver may be replaced by nickel; (ii) up to 60% of said silver may be replaced by tin; (iii) up to 20% of said silver may be replaced by copper; (iv) a portion of said silver may be replaced by a noble metal such as gold.
According to another aspect, the invention provides an electronic assembly comprising a ceramic substrate, and a silicon semiconductive device attached to said substrate by a bond, wherein said bond comprises a silver-filled glass.
According to a further aspect, the invention provides a method of bonding a silicon die to a ceramic substrate comprising: applying a silver-filled glass metallizing composition onto said substrate, said glass having a softening point in the range of 3250 42500 and having a silver:glass ratio in the range of 25:75 to 95:5; setting a silicon die into said metallizing composition with pressure to form an assembly; drying said assembly; firing said assembly at a peak temperature in the range of 425 0--52 5 OC.
Reference will hereinafter be made to the accompanying drawing, which shows by way of example a cross-sectional elevation of a silicon die bonded on a ceramic substrate in accordance with the invention.
Preferred embodiments of the invention will now be described.
In the selection of a silver powder for use with the invention, it has been determined that both spherical and flake powders function well, though the latter produces a shinier, more metalliclooking finish. It is of interest that some prior workers specified flake for silver conductives, but that was for a current-carrying "wire" rather than a bonding medium, where conductivity is through the thickness, rather than along the length.
Satisfactory silvers for the invention are those having a surface area in the range of 0.2 to 1 m2/gm, and a tap density of 2.2 to 2.8 g/cc.
The glass is the second key component, and it is essential that it be low-melting, so as to be molten at the die-attach temperature,425~ 45000. The preferred glass selected meets this requirement, has a softening temperature of 325 #C., and the following composition: PbO 95~96% SiO2 0.25-2.5% B203 remainder It has been found that small quantities of ZnO, under 0.5%, are not deleterious, but any sodium should be rigorously avoided, as it attacks silicon.
While bismuth oxide can also be incorporated in low-melting glasses, it is harder to mill than lead oxide, and will attack platinum used in formulation procedures. Thus, substitution of bismuth for lead is not advised.
The glass is fritted and ground in a high-purity alumina jar mill to meet the following specifications: surface area; 0.3-0.5 m2/gm tap density: 28-3.6 g/cc Generally, glasses having a softening point in the range of 3250 to 42500., and a coefficient of thermal expansion no higher than about 13 ppm/OC.. preferably in the range of 8-13 ppm/OC., may be used.
The softening point should be at least 32500.
to ensure that all organics are burned off. If the softening point is higher than 42500., the glass will not be sufficiently fluid at the die attach temperature. The glass is then mixed with the vehicle described hereinbelow (80% solids) and milled on a 3-roll mill to a particle size (F.O.G.) of 7-8 microns.
Those skilled in the art appreciate that the selection of vehicle is not critical, and a variety of appropriate vehicles are readily available. Of course, burn-out must be complete at the indicated temperatures. In this case the vehicle selected comprised: Ethyl methacrylate 12% Terpineol 88% The silver is then added to the glass paste in a desired silver:glass ratio as discussed below, but falling within the limits 25:75 to 95:5. The percent (total) solids is then adjusted to within the range of 75~86% by addition of more of the vehicle. Outside of this range, rheological problems are likely to be encountered; generally a solid content in the range of 8~83% is preferred.At this level, typically, the paste will have a viscosity of 20-22 Kcps, as measured on a Brookfield RVT Viscometer, with a TF spindle, at 20 RPM and 2500.
Use of the paste is essentially conventional.
Depending on use, a dot, square or screened area of the paste is applied on a metallized or bare film (ceramic) substrate, machine dispensing, screen printing of stamping techniques all being useable. If it is dotted, the size of the dot is about 25% larger than the die. The die is attached by placing the die in the center of the wet paste and "setting" it by applying pressure, so that the paste flows about half way up the side of the die and leaves a thin film under the die. Drying in an oven is carried out at 50#7500. for 20-40 minutes.Organic burnout is done on a cycle time of 1 5-20 minutes, with 2-3 minutes at a peak temperature in the range of 325--4500C. In the accompanying drawing, a substrate 10 is shown with a die 12 attached thereto with a layer of silver filled glass 14, which has flowed up around the edges during "setting". For test purposes, the package is subjected to a simulated (package) sealing cycle in the range of 4300 to 525 #C., with 1 5 minutes at 43000.
Alternatively, the die may be attached by known scrubbing techniques, or hot-stage vibratory bonding may be employed.
A surprising feature is that the mechanical strength of the bond is proportional to the silver content. Using a standard push test (Mil. Spec.
883B, method 2019.1), a range of 5 to 17 Ibs.
was recorded through the silver range of 30 to 95%. As would be expected, electrical conductivity also improves with silver content. At the low end, resistivity is comparable to the commercial epoxies (25-35 ohm. cm) for example EPO-TEK P-1 0, and this drops to 510 ohm. cm at high silver levels.
When the substrate has been metallized, acceptable bonds are achieved at Ag:glass ratios of 25:75 to 95:5. On bare alumina, it is preferred to keep the ratio between 50:50 and 90:10. Note that "acceptable" is here defined as well above the mil spec of 4.2 Ibs.
With both bond strength and conductivity rising with silver content a question could be raised as to utility of the low-silver, high-glass compositions. The answer, generally, depends on intended use. More particularly, when the die is to be attached by mechanical scrubbing means, very good bonds are achieved with silver in the 25 40% range. In situations where it is desired to have the die sink into the ink to a degree, the higher silver ratios are preferred. At the very high silver end (e.g. 75-96%), tests indicate that the ink can be applied to a bare substrate and the chip can be ultrasonically down-bonded with good results. One would not want to go much above 90% silver as adhesion will start to drop off.
There are thus a variety of possibilities, including elimination of certain processing steps, by, for example, attaching lead frames and dies at the same time.
It is possible to substitute certain base metals for a portion of the silver but generally, adhesion will drop and resistivity will rise with such substitution. Specifically, up to 10% Ni, up to 50% Sn and up to about 20% Cu were substituted and resulted in acceptable bond strengths, providing firing was carried out in air, not nitrogen, and at a combined metal:glass ratio of 80:20 (nitrogen firing reduces the lead oxide and destroys the glass).
An important aspect of the invention is its applicability to the larger integrated circuits now coming into use. More particularly, it is known that the gold-silicon eutectic is brittle intermetallic, and that any bonding material must accommodate the different thermal expansion rates of the die and the substrate. This is not a notable problem with small chips, but in the VLSIC range the sealing cycle temperature can cause both bond failure and chip cracking due to thermal stress. Because the composition of the present invention softens rather than melts, such thermal stresses are avoided, as has been shown by thermal shock test (mil spec standard 883 B, condition a).
Lastly, the question arises as to whether there might be applications of the invention where it would be desirable to substitute a noble metal, particularly gold, for a portion of the silver. It was found that no particular advantages accured by this expedient. More particularly, a standard gold paste was mixed with an 80:20 Ag:glass paste of the invention in proportions that ranged from Au:Ag ratio of 10/90 to 80/20. While the conductivity of bonds to chips showed some tendency to rise with higher gold, results were inconclusive and there was clearly no cost justification for such substitution. Moreover, the shear strength of the bonds tended to drop at higher gold, though it was acceptable at any level.
No gold-silicon eutectic was observed, presumably due to features of the Au-Ag-Si ternary phase diagram. There is thus no apparent reason to sacrifice the considerable economies of the invention by trading-off silver for gold.
A further important application of the invention is in bonding chip capacitors to substrates. For example, a 120x90x35 mil capacitor is "set" in a 5-7 mil pad of the silver-filled glass of the invention, dried and fired as noted above. Shear strength was 13.8 Ib., and a good electrical contact was made around the sides. In terms of hybrid circuit manufacture, this has important ramifications, to wit, circuit chips and capacitors can be attached, dried and fired in a single cycle, with good bonds. Moreover, subsequent processing or operation may be carried out at temperatures that would melt conventional solder pastes.
A further application for the invention is as a substitute for solder. More particularly, at the preferred 80:20 Ag:glass ratio, and the 80~85% solids content, the composition of the invention will "hold" the device to be soldered through the firing cycle, whereas solders will allow movement.
It will thus be seen that at least the preferred forms of the invention provide:~ (a) an improved medium for bonding silicon dies to substrates.
(b) a silver-filled glass adapted to make strong bonds between silicon dies and metallized or bare substrates under normal processing conditions.
(c) a silver-filled glass for bonding silicon dies to substrates that is lower in cost than gold-based systems, higher in conductivity and bond strength than other silver or non-metallic systems, and which is adapted for use in hermetic packages.
(d) a silver-filled glass usefule as a solder substitute and for bonding capacitor chips to substrates.
(e) a silver-filled glass for bonding silicon dies to alumina substrates that is as good as gold silicon eutectic bonds in terms of adhesion but which is lower in thermally induced stresses than eutectic bonds.
Various changes in the details, steps, materials and arrangements of parts which have been herein described and illustrated to explain the nature of the invention may be made by those skilled in the art within the principle and scope of the invention as defined in the appended claims.
Percentages and proportions in this specification are generally by weight.

Claims (20)

Claims
1. A silver-filled glass metallizing paste comprising: (a) about 75~85% of a solids component made up of: 20 to 95% of finely-divided silver; and 80 to 5% of a low-melting, finely-divided glass frit; (b) organic vehicle; with the provisos that: (i) up to 10% of said silver may be replaced by nickel; (ii) up to 60% of said silver may be replaced by tin; (iii) up to 20% of said silver may be replaced by copper; (iv) a portion of said silver may be replaced by a noble metal such as gold.
2. A metallizing paste as claimed in Claim 1, wherein said glass frit consists essentially of: PbO 95~96% SiO2 0.25-2.5% B203 remainder
3. A metallizing paste as claimed in Claim 1 or 2, wherein up to 10% of said silver is replaced by nickel.
4. A metallizing paste as claimed in Claim 1 or 2, wherein up to 60% of said silver is replaced by tin.
5. A metallizing paste as claimed in Claim 1 or 2, wherein up to 20% of said silver is replaced by copper.
6. A silver-filled glass metallizing paste for bonding silicon semiconductive devices to ceramic substrates comprising: (a) 75~85% of a solids component made up of 25 to 95% of finely-divided silver having a surface area of 0.7 to 1.0 m2/gm and a tap density of 2.25 to 2.75 g/cc; 75 to 5% of finely-divided glass frit having a softening point in the range of 3250 to 42500.; and (b) an organic vehicle; with the provisos that: (i) up to 10% of said silver may be replaced by nickel; (ii) up to 60% of said silver may be replaced by tin; (iii) up to 20% of said silver may be replaced by copper; (iv) a portion of said silver may be replaced by a noble metal such as gold.
7. An electronic assembly comprising a ceramic substrate, and a silicon semiconductive device attached to said substrate by a bond, wherein said bond comprises a silver-filled glass.
8. An electronic assembly as claimed in Claim 7, wherein said silver-filled glass has 25 to 95% silver (subject to the provisos specified in claim 1) and said glass has a softening point in the range of 325 425 C.
9. An electronic assembly as claimed in Claim 7 or 8, wherein said glass consists essentially of: PbO 95~96% SiO2 0.5-2.5% B203 remainder.
10. An electronic assembly as claimed in Claim 7, 8 or 9, and additionally comprising a conductive metallized layer between said substrate and said bond.
11. A method of bonding a silicon die to a ceramic substrate comprising: applying a silver-filled glass metallizing composition onto said substrate, said glass having a softening point in the range of 3250 42500 and having a silver:glass ratio in the range of25:75 to 95:5; setting a silicon die into said metallizing composition with pressure to form an assembly; drying said assembly; firing said assembly at a peak temperature in the range of 425o#5250C.
12. A method as claimed in Claim 11, wherein said metallizing composition has a solids content of 75-85%, the remainder being a suitable organic vehicle.
13. A method as claimed in Claim 11 or 12, wherein said glass comprises about 95% PbO.
14. A method as claimed in Claim 11, 12 or 13, wherein the silver:glass ratio in said metallizing composition is about 80:20.
15. A method as claimed in any one of Claims 11 to 14, wherein said glass consists essentially of: PbO 95~96% SiO2 0.5-2.5% B203 remainder.
16. A paste as claimed in Claim 1, substantially as hereinbefore described.
17. A paste as claimed in Claim 6, substantially as hereinbefore described.
18. An electronic assembly as claimed in Claim 7, substantially as hereinbefore described.
19. A method as claimed in Claim 11, substantially as hereinbefore described.
20. An electronic assembly as claimed in Claim 7, when made by a method as claimed in any one of Claims 11-1 5 or when made using a paste as claimed in any one of Claims 1 to 6.
GB08222054A 1981-08-03 1982-07-30 Silver-filled glass Expired GB2103250B (en)

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US06/355,719 US4401767A (en) 1981-08-03 1982-03-08 Silver-filled glass

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DE (1) DE3227815A1 (en)
FR (1) FR2513240B1 (en)
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0215462A2 (en) * 1985-09-16 1987-03-25 DEMETRON Gesellschaft für Elektronik-Werkstoffe m.b.H. Paste for bonding semi-conductors to ceramic underlayers
EP0323107A2 (en) * 1987-12-24 1989-07-05 Johnson Matthey Public Limited Company Bonding paste for electronic components
US4906596A (en) * 1987-11-25 1990-03-06 E. I. Du Pont De Nemours & Co. Die attach adhesive composition
US5180523A (en) * 1989-11-14 1993-01-19 Poly-Flex Circuits, Inc. Electrically conductive cement containing agglomerate, flake and powder metal fillers
US9224666B2 (en) 2012-04-18 2015-12-29 Rhode & Schwarz Gmbh & Co. Kg Circuit arrangement for a thermally conductive chip assembly and a manufacturing method
CN116018884A (en) * 2020-10-20 2023-04-25 株式会社东芝 Bonded body, ceramic circuit board using the same, and semiconductor device

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DE3414065A1 (en) * 1984-04-13 1985-12-12 Siemens AG, 1000 Berlin und 8000 München Configuration comprising at least one electronic component fixed on a substrate, and process for fabricating a configuration of this type
DE3837300A1 (en) * 1988-11-03 1990-05-23 Messerschmitt Boelkow Blohm Method for producing microelectronic circuits and hybrids
DE19816309B4 (en) * 1997-04-14 2008-04-03 CiS Institut für Mikrosensorik gGmbH Method for direct mounting of silicon sensors and sensors manufactured thereafter

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US2385580A (en) * 1944-07-01 1945-09-25 Du Pont Vitrifiable flux and bonding composition containing same
DE1646882B1 (en) * 1965-07-29 1970-11-19 Du Pont Precious metal mass to be burned onto ceramic carriers
SU391187A1 (en) * 1971-04-06 1973-07-25 PASTE FOR METALIZATION OF CERAMICS
US3824127A (en) * 1971-12-22 1974-07-16 Du Pont Disc capacitor silver compositions
JPS5116344A (en) * 1974-07-31 1976-02-09 Fujikura Kasei Kk Bodongarasuno netsusenyotoryo

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0215462A2 (en) * 1985-09-16 1987-03-25 DEMETRON Gesellschaft für Elektronik-Werkstoffe m.b.H. Paste for bonding semi-conductors to ceramic underlayers
EP0215462A3 (en) * 1985-09-16 1988-02-03 Demetron Gesellschaft Fur Elektronik-Werkstoffe M.B.H. Paste for bonding semi-conductors to ceramic underlayers
US4906596A (en) * 1987-11-25 1990-03-06 E. I. Du Pont De Nemours & Co. Die attach adhesive composition
EP0323107A2 (en) * 1987-12-24 1989-07-05 Johnson Matthey Public Limited Company Bonding paste for electronic components
EP0323107A3 (en) * 1987-12-24 1990-06-20 Johnson Matthey Public Limited Company Bonding paste for electronic components
US5180523A (en) * 1989-11-14 1993-01-19 Poly-Flex Circuits, Inc. Electrically conductive cement containing agglomerate, flake and powder metal fillers
US5326636A (en) * 1989-11-14 1994-07-05 Poly-Flex Circuits, Inc. Assembly using electrically conductive cement
US9224666B2 (en) 2012-04-18 2015-12-29 Rhode & Schwarz Gmbh & Co. Kg Circuit arrangement for a thermally conductive chip assembly and a manufacturing method
CN116018884A (en) * 2020-10-20 2023-04-25 株式会社东芝 Bonded body, ceramic circuit board using the same, and semiconductor device

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GB2103250B (en) 1986-02-26
FR2513240B1 (en) 1986-07-25
NL8203081A (en) 1983-03-01
CH652737A5 (en) 1985-11-29
IE821840L (en) 1983-02-03
DE3227815A1 (en) 1983-02-24
PH19754A (en) 1986-06-26
IE53305B1 (en) 1988-10-12
FR2513240A1 (en) 1983-03-25

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