US3766634A - Method of direct bonding metals to non-metallic substrates - Google Patents

Method of direct bonding metals to non-metallic substrates Download PDF

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US3766634A
US3766634A US00245889A US3766634DA US3766634A US 3766634 A US3766634 A US 3766634A US 00245889 A US00245889 A US 00245889A US 3766634D A US3766634D A US 3766634DA US 3766634 A US3766634 A US 3766634A
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metallic
copper
eutectic
metallic member
reactive
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G Babcock
W Bryant
C Neugebauer
J Burgess
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General Electric Co
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General Electric Co
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    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
    • C04B37/021—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles in a direct manner, e.g. direct copper bonding [DCB]
    • H—ELECTRICITY
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    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
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Definitions

  • ABSTRACT A method for direct bonding of metallic members to non-metallic members at elevated temperatures in a controlled reactive atmosphere without resorting to the use of electroless plating, vacuum deposition or intermediate metals.
  • the method comprises placing a metal member such as copper, for example, in contact with a non-metallic substrate, such as alumina, heating the metal member and the substrate to a temperature slightly below the melting of the metal, e.g., between approximately 1,065C. and 1,080C. for copper, the heating being performed in a reactive atmosphere, such as an oxidizing atmosphere, for a sufficient time to create a copper-copper oxide eutectic melt which, upon cooling, bonds the copper to the substrate.
  • a reactive atmosphere such as an oxidizing atmosphere
  • the present invention relates to improved bonds and methods of bonding together non-metallic members to metal members and non-metallic members to other non-metallic'members.
  • This application relates to concurrently filed application Ser. No. 245,890 of common assignee, the entire disclosure of which is incorporated herein by reference thereto.
  • Another object of this invention is to provide a bond and a method of bonding non-metallic refractory materials together or to metal members in a simple heating step without the need for intermediate wetting agents.
  • Yet another object of this invention is to provide a tenacious bond and a method of forming this bond between a non-metallic refractory material and a metal which is useful in the formation of integrated circuit modules, and to provide high current carrying electrical conductors on insulating members with high thermal conductivity paths to a heat sink and to provide hermetic seals between two non-metallic refractory materials.
  • our invention relates to bonds and methods of bonding together non-metallic members to metallic members.
  • a bond between metallic and non-metallic members is formed by placing a metallic member in contact with a non-metallic member preferably exhibiting refractory characteristics and elevating the temperatures of the members in a reactive atmosphere of selected gases and at controlled partial pressures for a sufficient time to produce a eutectic composition which exhibits a eutectic melt.
  • This eutectic melt forms at a temperature below the melting point of the metallic member and wets the metallic member and the non-metallic refractory member so that upon cooling, a tenacious bond is formed between the metallic and non-metallic members.
  • Useful metallic materials include copper, nickel, cobalt and iron, for example.
  • Useful reactive gases include oxygen, phosphorusbearing compounds and sulfur-bearing compounds, for example. In general, the amount of reactive gas necessary to produce tenacious bonds is dependent, in part, upon the thickness of the metallic and non-metallic members and the times and temperatures required to form the eutectic melt.
  • FIG. 1 illustrates a typical bond between nonmetallic and metallic materials in accord with our invention
  • FIG. 2 is a series of schematic illustrations in the process of making a metal to non-metal bond in accord with one embodiment of our invention
  • FIG. 3 is a flow diagram illustrating the process steps in accord with the embodiment of FIG. 2;
  • FIGS. 4 and 5 illustrate still other bonds made in accord with our invention
  • FIG. 6 schematically illustrates a horizontal furnace useful in practising our invention.
  • FIG. 7 schematically illustrates a vertical furnace useful in practising our invention.
  • FIG. 1 illustrates, by way of example, a typical bond 11 between a non-metallic refractory member 12 and a metallic member 13.
  • the bond 11 comprises a eutectic composition formed with the metallic member and a reactive gas in accord with the novel aspects of our invention.
  • non-metallic material is intended to include refractory materials such as alumina (A1 0 beryllia (BeO), fused silica or other useful materials, such as titanates and spinnels, for example.
  • alumina and beryllia are particularly useful in the practice of our invention since they exhibit a high thermal conductivity which makes them particularly useful for semi-conductor integrated circuit applications or in high power electrical circuits.
  • other nonmetallic refractory materials may also be employed, if
  • the metallic member 13 may include such materials as copper, iron, nickel, cobalt, chromium and silver, for example. Also, alloys of these materials, such as copper-nickel, nickel-cobalt, copper-chromium, coppercobalt, iron-nickel, silver-gold, and ternary compositions of iron, nickel and cobalt, are useful in practising our invention. As will become more apparent from the following description, still other metallic materials, such as beryllium-copper, for example, may also be advantageoujsly employed, if desired.
  • FIG. 2 illustrates a non-metallic refractory material 12, such as alumina or beryllia, for example, with a metallic member 13 overlying the nonmetallic refractory substrate 12.
  • the substrate 12 and the metallic member 13 are placed in a suitable oven or furnace including a reactive atmosphere which at an elevated temperature forms a eutectic composition 11 on the surfaces of the metallic member 13.
  • eutectic or eutectic composition means a mixture of atoms of the metallic member and the reactive gas or compound formed between the metal and the reactive gas.
  • the eutectic is a mixture of copper and copper oxide.
  • the metal is nickel and the reactive gas is phosphorus, the eutectic is a mixture of nickel and nickel phosphide.
  • the metallic member is cobalt and the reactive gas is a sulfur-bearing gas,"the eutectic is formed between cobalt and cobalt sulfide.
  • Table I is'a representative listing of still other eutectics which are useful in practising our invention. These eutectics are formed by reacting the metallic member to be bonded with a reactive gas c'ontrollably introduced into the'oven or furnace.
  • the eutectic composition is believed to form with one of the elemental metals, generally the one with the lower melting point.
  • One factor which appears to affect the tenacity and uniformity of the bond is the relationship between the melting point of the metallic member and the eutectic approximately 30 to 50C. of the melting point of the metallic member, for example, the metallic member tends to plastically conform to the shape of the substrate member and thereby produce better bonds than those eutectics which become liquidus at temperatures greater than approximately 50C. below the melting point of the metallic member.
  • the uniformity of the bond therefore appears to be related to the creep of the metal which becomes considerable only near the melting point. From Table I, for example, it can be seen that the following eutectic compounds meet this requirement: copper-copper oxide, nickel-nickel oxide, cobalt-cobalt oxide, iron-iron oxide and copper-copper sulfide.
  • FIG. 4 illustrates an alternative embodiment of our invention wherein a non-metallic refractory material 12 has two metallic members 13 bonded to opposite surfaces thereof by bonds 1].
  • FIG. 5 illustrates still another embodiment of our invention wherein two non-metallic members 12, such as alumina or beryllia, for example, are bonded together by a metallic member 15.
  • the eutectic forms in substantially the same manner as described above but for the fact that bonding occurs on both surfaces of the metallic member 15.
  • This embodiment of our invention is particularly useful in forming hermetic seals between non-metallic refractory materials, for example, such as those employed in the fabrication of vacuum tubes, such as high frequency type tubes.
  • FIG. 6 illustrates a horizontal furnace comprising an elongated quartz tube 22,,for example, having a gas i nlet 23 at one end thereof and a gas'outlet 24 at the other end.
  • the quartz tube 22 also includes an opening or port 25 through which materials are placed into and removed from the furnace. The materials are placed on a holder 26 having a push rod-27 extending through one end of the furnace so that the holder and materials placed thereon may be introduced and removed from the furnace.
  • the furnace 21 is also provided with suitable heating elements, illustrated in FIG. 6 as electrical wires 28 which surround the quartz tube 22 in the region to be heated.
  • the electrical wires 28 may, for example, be
  • thermocouple 29 which extends through an opening in the quartz tube so that electrical connections can bemade thereto.
  • FIG. 6 also illustrates a substrate 12 such as a nonmetallic refractory material positioned on the holder 26 and a metallic material 13 overlying the substrate 12. These materials are introduced into the quartz tube through the opening 25 which is then sealed by suitable stopper means.
  • a substrate 12 such as a nonmetallic refractory material positioned on the holder 26 and a metallic material 13 overlying the substrate 12. These materials are introduced into the quartz tube through the opening 25 which is then sealed by suitable stopper means.
  • reactive gas flow or atmosphere means a mixture of an inert gas such as argon, helium or nitrogen, for example, with a controlled minor amount of a reactive gas, such as oxygen, a phosphorus-containing gas such as phosphine, for example, or a sulfur-containing gas such as hydrogen sulfide, for example.
  • a reactive gas such as oxygen, a phosphorus-containing gas such as phosphine, for example, or a sulfur-containing gas such as hydrogen sulfide, for example.
  • the amount of reactive gas in the total gas flow is dependent, in part, on the materials to be bonded and the thickness of the materials, in a manner more fully described below.
  • the partial pressure of the reactive gas must exceed the equilibrium partial pressure of the reactive gas in the metal at or above the eutectic temperature. For example, when bonding copper members to refractory members in a reactive atmosphere including oxygen, the partial pressure of oxygen must be above 1.5 X atmosphere at the eutectic temperature of 1,065C.
  • the furnace is then brought to a temperature sufficient to form a eutectic liquidus or melt at the metal-substrate interface.
  • a temperature sufficient to form a eutectic liquidus or melt at the metal-substrate interface.
  • the temperature of the furnace is brought to between approximately 1,065C. and 1,075C.
  • a copper-copper oxide eutectic forms on the copper member 13. This eutectic melt then wets the copper and the alumina to form a tenacious bond therebetween.
  • the times necessary to form this eutectic melt range between approximately 10 minutes for 1- mil-thick copper members and approximately 60 minutes for ZSO-mil-thick copper members.
  • a more detailed relationship between copper thickness and time at an elevated temperature of between 1,065 and l,075C. is presented below in Table II for a reactive atmosphere including oxygen.
  • Alumina 250 25 Mil, 96% 60 Alumina Table ll illustrates the relationship between copper thickness, non-metallic refractory material thickness and firing time in the furnace, i.e., the time at which the metal-non-metal materials remain in the furnace. From this table it is readily apparent that the firing time increases with the metal thickness, although there does not appear to be a linear relationship between the two.
  • FIG. 7 illustrates a vertical furnace 31 including a vertically positioned quartz tube 32, for example, with a carbon susceptor 33 positioned on a fused silica pedestal 34.
  • the quartz tube 32 is sur rounded with RF. heating coils 35 which are powered by an external R.F. generator, not shown.
  • FIG. 7 also illustrates a substrate 36 such as a nonmetallic refractory material resting on the susceptor 33 with a metal member 37 placed thereover.
  • inert and oxidizing gases are introduced through inlets 38 and 39, respectively.
  • the combined gas flows pass through conduit 40 onto the metallic and non-metallic members and exhaust through an exhaust outlet 41.
  • Flow meters 42 and 43 on each inlet monitor and control the rate of flow of the gases into the furnace.
  • the operation of the vertical furnace will be described with reference to the formation of a bond between a S-mil-thick copper member and an approximately -mil-thick beryllia member.
  • the flow meters 42 and 43 are adjusted so that pure argon is introduced at inlet 38 and argon containing 2 per cent oxygen is introduced at inlet 39.
  • the quartz tube is then flushed or purged for approximately 10 minutes with a flow rate of approximately 2 cubic feet per hour of argon and approximately 1 cubic foot per hour of the argon-containing oxygen gas produces a total oxygen content in the combined gases of approximately 0.04 molar per cent.
  • the temperature of the susceptor, beryllia and copper members is maintained at room temperature.
  • the RF. power is applied until the temperature of the copper member exceeds 1,065C., but is below l,083C. Typically, 2 to 5 minutes are required to produce this temperature which may, for example, be monitored optically.
  • Optical monitoring of temperature is well known in the art and as the copper member heats up from room temperature, a red-brown oxidation color typical of copper oxide appears on the surface. Above 600C., the copper surface emits light strongly. At a temperature of 1,065C., a liquid layer is observed around the copper member.
  • the liquid layer wets both the beryllia and copper members as evidenced by a drastic color change. Wetting first occurs at the outer edges of the copper member where a black color appears which then moves toward the center of the copper, until the entire copper member appears black to the eye. Under these conditions, the copper member retains its structural integrity and does not break up into separate liquid droplets. When the wetting process is completed over the entire surface area, the R.F. power is removed and the members permitted to cool. Upon removal of the copper and beryllia from the furnace, the copper is strongly bonded to the beryllia and bond strengths in excess of 20,000 pounds per square inch have been observed.
  • the shape of the bonded copper member is substantially the same as that of the original unbonded copper. However, there is some evidence of oxidation and precipitation of copper oxide in the bonded member. Also, some recrystallization of the grain structure within the copper member is discernible.
  • the tenacious bonds formed in accord with our invention result from the reaction of the metal with the reacting gas during the heating period prior to the formation of the eutectic melt. During this period, a small amount of the reacting gas dissolves into the metal, but most of it reacts with the metal to form a eutectic with the metal over its exposed surfaces. At'the eutectic temperature, 1,065C. for copper-oxide, for example, a liquid phase of or near the eutectic composition forms a skin around the metal. The thickness of this molten skin depends upon the partial pressure of the reacting gas and the length of time at the elevated temperature.
  • the eutectic Under conditions permitting the formation of the eutectic, the eutectic appears to wet the metal and the non' metallic refractory material in such a way that upon cooling, a strong bond forms between the two materials.A strong bond has also been observed between pure copper at its melting point of 1,08'3C., in theabsence of a reacting gas (or even in a reducing atmosphere), however,the copper member loses its structural integrity and forms liquid droplets which are bonded to the non-metallic refractory material.
  • the partial pressure of the reacting gas if the partial pressure of the reacting gas is too high, all the metal reacts with the reactive gas and forms, for example, an oxide, sulfide, phosphide, etc;, which prevents the formation of the eutectic melt.
  • an intermediate reacting gas partial pressure is required so that both the eutectic melt phase and the metallic phase are present simultaneously. Tests have illustrated that extremely strong bonds are achieved when both phases are present. Accordingly, in practising our invention the partial pressure of the reacting gas must be sufficiently great to permitthe formation of a eutectic with the metal butnot so great as to completely convert the metal to the oxide, sulfide, phosphide, etc. during the bonding time.
  • Table III illustrates ranges for partial pressures of the reactive gases at which good bonding occurs for other metals and gases. Only those eutectics which exhibit a eutectic temperature within 50C. of the melting point of the metal are listed.
  • useful bonds are formed with the aforementioned binary metallic composition such as coppernickel, nickel-cobalt, copper-chromium, coppercobalt, iron-nickel and beryllium-copper in a reactive atmosphere including oxygen.
  • binary metallic compositions such as coppernickel, nickel-cobalt, copper-chromium, coppercobalt, iron-nickel and beryllium-copper
  • Ternary compositions of iron, nickel and cobalt also form useful bonds in a reactive atmosphere of oxygen.
  • silver-gold compositions bond to non-metallic refractory members in a reactive atmosphere including a sulfur-bearing gas such as hydrogen sulfide, for example.
  • metallic members bonded to a non-metallic refractory material may be patterned by photolithographic masking and etching techniques to produce a desired pattern in the metallic member after forming the desired bond.
  • This method of forming patterned conductors is preferable in the fabrication of semiconductor integrated circuits, for example, where the size of the conductor if preformed before bonding would pose serious handling problems.
  • Microwave tests performed on electrical circuits formed by patterning copper bonded to alumina exhibit Qs comparable to those formed by thin film techniques. For example, Qs in excess of 450 have been observed.
  • the total gas flow rate may be varied over wide limits without materially affecting the bond and economic considerations will generally control the acceptable gas flow rate.
  • the partial pressure of the reactive gas in the inert gas also can be varied depending in part on the relative sizes of the materials-to be bonded, the gas flow rate, the presence of reactive elements in the flow system, such as carbon susceptors in the case of an oxygen system, the warm-up rate prior to bonding and the presence of residual oxygen or water in the bonding system and bonding time. Therefore, it is intended that the appended claims cover all such changes and modifications as fall within the true spirit and scope of our invention.
  • Av method of direct bonding a metallic member to a non-metallic refractory material substrate comprising the steps of:
  • said metallic member is selected from the group consisting of copper, nickel, cobalt, iron and chromium and the step of heating in a reactive atmosphere forms said eutectic with the selected metallic member.
  • said copper member is in the form of a sheet having a thickness of between approximately 1 and 250 milli-inches and said reactive atmosphere is argon, helium or nitrogen with approximately 0.01 to 0.5 per cent by volume of oxygen.
  • non-metallic material is selected from the group of alumina, beryllia and fused silica, titanates and spinnels.
  • said reactive atmosphere includes a partial pressure of a reactive gas in excess of the equilibrium partial pressure of the reactive gas in the metal at or above the eutectic temperature.
  • said metallic member is selected from the group of alloys consisting of copper-nickel, nickel-cobalt, copper-chromium, copper-cobalt, iron-nickel, silver-gold and berylliumcopper.
  • a method of bonding a metallic member to a non-metallic member comprising:
  • a metallic member selected from the group consisting of copper, nickel, cobalt, iron and chromium in contact with a non-metallic member; providing a reactive gas atmosphere which at an elevated temperature will react with the metal surface to form a eutectic;
  • step of forming a eutectic comprises:

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  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
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DE2319854A1 (de) 1973-10-25
GB1394322A (en) 1975-05-14
FR2181049A1 (fr) 1973-11-30
IT983841B (it) 1974-11-11
DE2319854C2 (de) 1983-12-29
FR2181049B1 (fr) 1980-04-11
JPS4917381A (fr) 1974-02-15
JPS5713515B2 (fr) 1982-03-17

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