EP1601631A1 - Verfahren zur herstellung eines verbundwerkstoffes - Google Patents

Verfahren zur herstellung eines verbundwerkstoffes

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Publication number
EP1601631A1
EP1601631A1 EP04703310A EP04703310A EP1601631A1 EP 1601631 A1 EP1601631 A1 EP 1601631A1 EP 04703310 A EP04703310 A EP 04703310A EP 04703310 A EP04703310 A EP 04703310A EP 1601631 A1 EP1601631 A1 EP 1601631A1
Authority
EP
European Patent Office
Prior art keywords
alloy
eutectic
diamond
infiltrate
group
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.)
Withdrawn
Application number
EP04703310A
Other languages
German (de)
English (en)
French (fr)
Inventor
Arndt LÜDTKE
Gerhard Leichtfried
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.)
Plansee SE
Original Assignee
Plansee SE
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
Application filed by Plansee SE filed Critical Plansee SE
Publication of EP1601631A1 publication Critical patent/EP1601631A1/de
Withdrawn legal-status Critical Current

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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/653—Processes involving a melting step
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
    • H01L23/3732—Diamonds
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3279—Nickel oxides, nickalates, or oxide-forming salts thereof
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/402—Aluminium
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/407—Copper
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/408—Noble metals
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
    • C04B2235/427—Diamond
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/428—Silicon
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/604—Pressing at temperatures other than sintering temperatures
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    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
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    • 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
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00

Definitions

  • the invention relates to a method for producing a diamond-containing composite material.
  • the thermal conductivity of diamond is 1,000 to 2,000 W / (m.K), with the content of nitrogen and boron atoms on lattice sites being the determining factor.
  • Heat sinks are widely used in the manufacture of electronic components.
  • the semiconductor components and a mechanically stable casing are the essential components of an electronic package.
  • substrate, heat spreader or carrier plate are often used for the heat sink.
  • the semiconductor component consists, for example, of single-crystal silicon or gallium arsenide. This is connected to the heat sink, and soldering methods are usually used as the joining technique.
  • the heat sink has the function of dissipating the heat generated during the operation of the semiconductor component.
  • Semiconductor components with particularly high heat development are, for example, LDMOS (laterally diffused metal oxide semi-conductor), laser diodes, CPU (central processing unit), MPU (microprocessor unit) or HFAD (high frequency amplify device).
  • LDMOS laterally diffused metal oxide semi-conductor
  • laser diodes laser diodes
  • CPU central processing unit
  • MPU microprocessor unit
  • HFAD high frequency amplify device
  • the geometric designs of the heat sink are application-specific and varied. Simple shapes are flat plates. However, complex substrates with recesses and steps are also used.
  • the heat sink itself is connected to a mechanically stable casing. The thermal expansion coefficient of the used
  • Semiconductor materials are low compared to other materials and are used in the literature for silicon with 2.1 x 10 "6 K “ 1 to 4.1 x 10 "6 K “ 1 and for gallium arsenide with 5, 6 x 10 "6 K “ 1 to 5.8 x 10 "6 K “ 1 specified.
  • Ceramic materials, composite materials or plastics are usually used for the encapsulation. Examples of ceramic materials are Al 2 0 3 with an expansion coefficient of 6.5 x 10 "6 K “ 1 or aluminum nitride with an expansion coefficient of 4.5 x 10 "6 K “ 1 .
  • Tensions can arise during the manufacture of the package, namely during the cooling phase from the soldering temperature to room temperature. However, temperature fluctuations also occur during operation of the package, which range, for example, from -50 ° C to 200 ° C and can lead to thermomechanical stresses in the package.
  • EP 0 521 405 describes a heat sink which has a polycrystalline diamond layer on the side facing the semiconductor chip.
  • the lack of plastic deformability of the diamond layer can lead to cracks in the diamond layer as soon as it cools down from the coating temperature.
  • US Pat. No. 5,273,790 describes a diamond composite material with a thermal conductivity> 1,700 W / (mK), in which loose, shaped diamond particles are converted from the gas phase into a stable shaped body by means of subsequent diamond deposition.
  • the diamond composite produced in this way is too expensive for commercial use in mass parts.
  • WO 99/12866 describes a method for producing a diamond-silicon carbide composite material. It is manufactured by infiltrating a diamond skeleton with silicon or a silicon alloy. Due to the high melting point of silicon and the resulting high infiltration temperature, diamond is partly converted into carbon or subsequently into silicon carbide. Due to the high brittleness, the mechanical workability of this material is extremely problematic and complex, so that this composite material has not yet been used for heat sinks.
  • US 4 902 652 describes a method for producing a sintered diamond material.
  • An element from the group of transition metals from groups 4a, 5a and 6a, boron and silicon is deposited on diamond powder by means of physical coating processes.
  • the coated diamond grains are then connected to one another by means of a solid phase sintering process. It is disadvantageous that the resulting product has a high porosity and a coefficient of thermal expansion that is too low for many applications.
  • Diamond grains with a size of 1 to 50 microns is a metallic matrix consisting of aluminum, magnesium, copper, silver or their alloys.
  • the disadvantage here is that the metallic matrix is poorly bonded to the diamond grains, so that the thermal conductivity and mechanical integrity are insufficient.
  • the metal carbides are the carbides of the metals of the 4a to 6a groups of the periodic table.
  • TiC, ZrC and HfC are particularly emphasized.
  • Ag, Cu, Au and Al are mentioned as particularly advantageous filler metals.
  • the metal carbides have a low thermal conductivity, which is in the range from 10 to 65 W / (mK) for TiC, ZrC, HfC, VC, NbC and TaC.
  • Another disadvantage is that the metals of the 4a to 6a groups of the periodic table have a solubility in the filler metal, such as silver, whereby the thermal conductivity of the metal phase is greatly reduced.
  • EP 0898 310 describes a heat sink which consists of diamond grains, a metal or a metal alloy of high thermal conductivity from the group Cu, Ag, Au, Al, Mg and Zn and a metal carbide of the metals of groups 4a, 5a and Cr, the Metal carbides cover at least 25% of the surface of the diamond grains.
  • EP 0 898 310 also describes process techniques, for example an infiltration process, for producing a heat sink. Alloys are used which consist of a metal with high thermal conductivity and a carbide-forming metal from the group of elements from groups 5a, 6a and Cr. For two-component alloys made from these components, however, infiltration temperatures of over 1000 ° C are required, which leads to an impermissibly high conversion of diamond into graphite.
  • the liquidus temperature of a eutectic Ag-Cu alloy (Ag-30% by weight Cu) is 780 ° C, while the Cu-Ag-Ti alloys mentioned in EP 0 898 310 have a liquidus temperature of 830 to 870 ° C.
  • the method according to the invention comprises a shaping step of an intermediate material which is carried out without pressure or with the aid of pressure.
  • the intermediate material consists of diamond powder with an average grain size of the diamond grains of 5 to 300 ⁇ m. A preferred grain size range is 60 to 250 ⁇ m. Fine diamond grains and thus a large interface with neighboring phases reduce the thermal conductivity.
  • Pressure-free processes are, for example, pouring processes, vibrating processes or slip casting. In the case of pressure-supported process technologies, die pressing, isostatic pressing and powder injection molding are examples. Depending on the process technology chosen, the proportion of diamond based on the total volume is 40 to 90% after the shaping process. The remaining part consists of pores and / or binders and / or metallic parts with high thermal conductivity.
  • An added binder enables the green compact density to be increased or the matrix friction to be reduced.
  • diamond powder and binder are mixed in conventional mixers or mills.
  • suitable binders are those based on polymer and wax.
  • Favorable binder proportions are 1 to 20% by weight. It is advantageous to pass the binder through a chemical before the infiltration step or at least partially remove thermal process. In the case of a thermal process, it can be advantageous to conduct the process in such a way that residual portions of the pyrolyzed carbon remain on the diamond surface, which react with portions of the infiltrate in a carbide.
  • Thermal debinding can also be integrated in the infiltration process. Cu, Al, Au and their alloys can be mentioned as metallic components of high thermal conductivity.
  • the infiltration process can be pressure-free or pressure-supported. The latter is commonly referred to as squezze casting.
  • the infiltrate alloy has a eutectic or near-eutectic composition. Near-eutectic alloys include compositions that have a liquidus temperature below 950 ° C.
  • the infiltrate alloy comprises at least one metallic component with high thermal conductivity, consisting of an element or an alloy from the group Cu, Ag, Au and at least one element from the group Si, Y, Sc, rare earth metals. It has been shown 'that the use of inventive Infiltratlegleiteren leads to a very good wetting of the diamond grains and a high interfacial strength between the diamond grains and the surrounding phase regions.
  • the infiltrate alloys according to the invention have the advantage that their solidus temperatures are significantly lower than those of Cu, Au or Ag alloys with the metals of the 4a / 5a groups of the periodic table or Cr, as is also shown in Table 1. This enables the use of two-component alloys instead of multi-component alloys, which has a favorable effect on the thermal conductivity.
  • the solidus temperatures of the infiltrate alloys according to the invention are below 870 ° C. This ensures that during the
  • Table 1 This implementation can be reduced even further by using multi-component alloys in accordance with the composition ranges specified in the claim. These multi-component alloys are particularly advantageous if the infiltration times are long due to the process. However, the use of multi-component alloys leads to a reduced thermal conductivity.
  • Table 1 also shows that the infiltrate alloys according to the invention have a very low solubility at the eutectic temperature or at 400 ° C. for Y, Si and rare earth metals.
  • This has the advantage that the Cu, Ag, or Au-rich phase resulting from the eutectic conversion has a very high purity and thus thermal conductivity.
  • Alloys of Ag or Au with Cu or up to 3 at.% Ni also have a sufficiently high thermal conductivity, which is impaired to a not unacceptably high degree by low, undissolved Si, Y, Sc or rare earth metal fractions. Portions of graphite also deteriorate the thermal conductivity to a not unacceptably high extent.
  • the wetting behavior can be further improved by adding Ni, Cr, Ti, V, Mo, W, Nb, Ta, Co and / or Fe, but the total content of these elements must not exceed 3 at.%, Otherwise an impermissible one high reduction in thermal conductivity is associated.
  • the advantages of the infiltrate alloy according to the invention also come into play when hot pressing is used as the compression process.
  • a die of a hot press which consists of graphite, for example, is filled with the intermediate material.
  • the intermediate substance is subsequently brought to a temperature below 1000 ° C., for example by conductive heating of the die to a temperature above the solidus temperature of the infiltrate alloy, the pressure being applied by means of a stamp movement.
  • This heat treatment can also have a beneficial effect on the interfacial strength between the diamond particles and the surrounding components.
  • This heat treatment step can also be integrated in the cooling process of the infiltration step.
  • diamond-containing composite materials produced according to the invention have a sufficiently good machinability.
  • the diamond content can be reduced by the high thermal conductivity of the Ag, Au or Cu-rich structural components.
  • the diamond and metal phase content By varying the diamond and metal phase content, it is possible to produce tailor-made heat sinks for a wide range of requirements with regard to thermal conductivity and thermal expansion. Further structural constituents do not deteriorate the properties to an inadmissible extent as long as their content does not exceed 5% by volume. Unbound proportions of Si, C, Y, Sc and rare earth metals should be mentioned. Although these structural components slightly impair the thermal conductivity, they have a favorable effect on the coefficient of thermal expansion in the case of C and Si by reducing it. In addition, some of them can only be completely avoided in terms of manufacturing technology with relatively great effort.
  • the composite material according to the invention can also be used as a heat sink in other areas of application, for example in the field of aerospace or engine construction.
  • the invention is explained in more detail below by means of production examples.
  • Natural diamond powder of quality IIA (Micron + SND from Element Six GmbH) with an average grain fraction of 80 - 150 ⁇ m was filled into a graphite mold with dimensions of 35 mm x 35 mm x 5 mm.
  • the bulk density was determined by mechanical shaking at 65 vol.%. set.
  • the diamond powder was covered with a film made of an eutectic Ag-Si alloy, the Si content being 11 at.% And heated to a temperature of 860 ° C. in a furnace under vacuum for infiltration, the holding time being 15 Minutes.
  • the subsequent gas pressure infiltration using helium was carried out at 1 bar for 15 minutes. After cooling to room temperature with a break point at 400 ° C.
  • Silicon carbide phase can not be determined.
  • the structure consists of an Ag-rich phase with embedded Si precipitates, which have formed through the eutectic conversion.
  • the volume fraction of the Ag-rich phase was approximately 12%, that of Si approximately 1%.
  • no other constituents could be detected by means of EDX, so that, based on the detection limit, it can be assumed that the Ag content is greater than 99 at.%.
  • the plate was processed by laser and eroding. An average value of 500 W / (mK) was measured for the thermal conductivity at room temperature. The determination of the coefficient of thermal expansion gave an average value of 8.5 10 "6 K " 1 .
  • Example 3 synthetic diamond powder of Micron + MDA quality from Element Six GmbH and an average grain size of 40 - 80 ⁇ m was processed. Processing was carried out as described in Example 1. The average thermal conductivity at room temperature of the composite material produced in this way was 410 W / (mK), the average coefficient of thermal expansion 9.0 10 "6 K " 1 .
  • Example 3 The average thermal conductivity at room temperature of the composite material produced in this way was 410 W / (mK), the average coefficient of thermal expansion 9.0 10 "6 K " 1 .
  • Hot-work steel was preheated to 150 ° C at a gas pressure of approx.
  • the temperature of the Ag-Si melt was approximately 880 ° C.
  • Composite material was 480 W / (m.K), the middle one
  • Example 4 Synthetic diamond powder of the Micron + MDA quality from Element Six GmbH with an average grain fraction of 40-80 ⁇ m was processed in accordance with Example 3, but without a holding phase being carried out at about 400 ° C. for 15 minutes while cooling from the infiltration temperature.
  • the average thermal conductivity at room temperature of the composite material produced in this way was 440 W / (mK), the average coefficient of thermal expansion 8.5 10 "6 K " 1 .
  • Natural diamond powder of quality IIA (Micron + SND from Element Six GmbH) with an average grain size of 40 - 80 ⁇ m was mixed with 7% by volume of a binder based on epoxy resin.
  • the precursor or intermediate material thus produced was pressed by means of die presses at a pressure of 200 MPa to a plate measuring 35 mm ⁇ 35 mm ⁇ 5 mm.
  • the pore content of the plate was approximately 15% by volume. Subsequently, this plate was covered with a sheet of eutectic

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JP4880447B2 (ja) 2012-02-22
EP1601630A1 (de) 2005-12-07
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US20060157884A1 (en) 2006-07-20
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