WO2021015122A1 - 接合基板および接合基板の製造方法 - Google Patents

接合基板および接合基板の製造方法 Download PDF

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WO2021015122A1
WO2021015122A1 PCT/JP2020/027829 JP2020027829W WO2021015122A1 WO 2021015122 A1 WO2021015122 A1 WO 2021015122A1 JP 2020027829 W JP2020027829 W JP 2020027829W WO 2021015122 A1 WO2021015122 A1 WO 2021015122A1
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interface
layer
bonding
bonding layer
substrate
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French (fr)
Japanese (ja)
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隆 海老ヶ瀬
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NGK Insulators Ltd
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NGK Insulators Ltd
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Priority to JP2021534001A priority Critical patent/JP7197703B2/ja
Priority to EP20843472.0A priority patent/EP4006002A4/en
Publication of WO2021015122A1 publication Critical patent/WO2021015122A1/ja
Priority to US17/547,379 priority patent/US12165948B2/en
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Definitions

  • the present invention relates to a bonded substrate.
  • Silicon nitride ceramics have high thermal conductivity and high insulation properties. Therefore, a bonded substrate in which a copper plate is bonded to a silicon nitride ceramic substrate via a bonding layer is suitably used as an insulating heat-dissipating substrate on which a power semiconductor element is mounted.
  • the bonded substrate is produced by producing an intermediate product in which the brazing material layer is between the copper plate and the nitride ceramic substrate, and the produced intermediate product is heat-treated to change the brazing material layer into a bonding layer, and the copper plate is used. And manufactured by patterning the bonding layer (see, for example, Patent Document 1 and Patent Document 2).
  • the brazing layer often contains powders containing silver and copper, as well as titanium hydride powders.
  • the bonding layer contains titanium nitride, which is a reaction product of titanium derived from titanium hydride powder and nitrogen derived from a silicon nitride ceramic substrate, as a main component.
  • a copper metal plate is bonded to a silicon nitride substrate by a brazing method (paragraph 0016).
  • a brazing material an Ag—Cu alloy containing an active metal such as Ti, Zr or Hf is used (paragraph 0016).
  • TiN particles are sufficiently precipitated at the brazing material layer / silicon nitride interface in order to obtain a strong bonding strength (paragraph 0018).
  • Patent Document 2 describes an embodiment in which a copper plate is bonded to a nitride ceramic substrate such as a silicon nitride substrate or an aluminum nitride substrate using an Ag—Cu—Ti brazing material to obtain a bonded substrate having TiN as a bonding layer.
  • a nitride ceramic substrate such as a silicon nitride substrate or an aluminum nitride substrate using an Ag—Cu—Ti brazing material to obtain a bonded substrate having TiN as a bonding layer.
  • the obtained bonding substrate is shown in two types, one in which a void is formed between the copper plate and the bonding layer and the other in which an Ag-rich phase is posted instead of the void, and the latter is electrically used. It is said to be highly reliable even for various dielectric breakdowns.
  • the reliability for the thermal cycle is ensured by paying attention to the interface between the copper plate and the bonding layer, but at least the interface between the nitride ceramic substrate and the bonding layer. No attention has been paid to the relationship between the configuration in the vicinity and the adhesion strength between the two layers.
  • the interface is determined according to the bonding conditions. Voids are formed discretely, or Ag-rich phases are formed discretely in place of the voids. The formation of a void or Ag-rich phase at the interface between the copper plate and the bonding layer is not always desirable from the viewpoint of improving the adhesion strength between the copper plate and the bonding layer.
  • An object to be solved by the present invention is to improve the adhesion strength between the silicon nitride ceramic substrate and the bonding layer and the adhesion strength between the copper plate and the bonding layer to obtain a bonding substrate having high bonding strength.
  • the bonding substrate includes a silicon nitride ceramic substrate, a copper plate, and a bonding layer for bonding the copper plate to the silicon nitride ceramic substrate, and the bonding layer is the silicon nitride ceramic substrate. It has a first interface in contact with the copper plate and a second interface in contact with the copper plate, and contains a nitride and a siliconized product of an active metal which is at least one metal selected from the group consisting of titanium and zirconium.
  • the atomic fraction of nitrogen in the junction layer is maximum at the first interface and minimum at the second interface, and the sum of the atomic fraction of the active metal and the atomic fraction of silicon in the junction layer is It is characterized in that it is the smallest at the first interface and the largest at the second interface.
  • the atomic content of nitrogen forming a strong bond with silicon nitride of the bonding layer in contact with the silicon nitride ceramic substrate It is maximized at the first interface.
  • a bonded substrate having improved adhesion between the silicon nitride ceramic substrate and the bonded layer is realized as compared with the bonded substrate having no such nitrogen distribution.
  • the bonding layer of the bonding substrate formed by bonding the silicon nitride ceramic substrate and the copper plate the sum of the atomic fractions of the active metal forming the metal bond with copper and the atomic fraction of silicon is , Maximum at the second interface of the bonding layer in contact with the copper plate.
  • FIG. 13 It is sectional drawing which shows typically the intermediate product obtained in the process of patterning of a bonding layer 13 and a copper plate 12. It is sectional drawing which shows typically the intermediate product obtained in the process of patterning of a bonding layer 13 and a copper plate 12. It is a figure which shows the STEM image used for observing the sample for analysis in Example 1.
  • FIG. It is a partially enlarged image of the STEM image of FIG. It is a figure which shows the mapping result about oxygen, silicon, titanium, copper, and silver by energy dispersive X-ray analysis (EDX).
  • EDX energy dispersive X-ray analysis
  • HAADF-STEM image showing four extraction positions P1, P2, P3, and P4 that were the subject of quantitative analysis based on the measurement results by EDX. It is an enlarged HAADF-STEM image near the grain boundary triple point 191. It is a figure which shows the EDX spectrum in the grain boundary triple point 191 and the vicinity thereof. It is a BF-STEM image which shows 5 extraction positions P11, P12, P13, P14, and P15 which were the object of measurement of the selected area electron diffraction pattern. It is a figure which shows the measurement target region by electron energy loss spectroscopy (EELS), and the EELS intensity map which shows the distribution of each element in the region.
  • EELS electron energy loss spectroscopy
  • FIG. 1 is a cross-sectional view schematically showing a bonding substrate 1 according to an embodiment of the present invention.
  • the bonding substrate 1 includes a silicon nitride ceramic substrate (hereinafter referred to as a ceramic substrate) 11, a copper plate 12U, a bonding layer 13U, a copper plate 12L, and a bonding layer 13L.
  • the bonding substrate 1 may include elements other than these elements. Further, the arrangement of either the set of the copper plate 12U and the bonding layer 13U and the set of the copper plate 12L and the bonding layer 13L may be omitted.
  • the copper plate 12U and the bonding layer 13U are arranged on the main surface 101U of the ceramic substrate 11.
  • the copper plate 12L and the bonding layer 13L are arranged on the main surface 101L of the ceramic substrate 11.
  • the bonding layer 13U has the copper plate 12U bonded to the main surface 101U of the ceramic substrate 11, and the bonding layer 13L has the copper plate 12L bonded to the main surface 101L of the ceramic substrate 11.
  • the bonding substrate 1 may be used in any way, and is used, for example, as an insulated heat dissipation substrate on which a power semiconductor element is mounted.
  • FIG. 2 is an enlarged cross-sectional view schematically showing a part of the bonding substrate 1 according to the present embodiment.
  • the set of the main surface 101, the copper plate 12 and the bonding layer 13 of the ceramic substrate 11 shown in FIG. 2 is the set of the main surface 101U, the copper plate 12U and the bonding layer 13U of the ceramic substrate 11 and the main surface 101L and the copper plate 12L of the ceramic substrate 11. And the set of the bonding layer 13L.
  • the copper plate 12 is brazed to the ceramic substrate 11 by an active metal brazing method.
  • an intermediate in which a brazing material layer made of an active metal brazing material (hereinafter, simply referred to as a brazing material) is arranged between the ceramic substrate 11 and the copper plate 12 is pressurized and heated. Therefore, the brazing material layer is changed to the bonding layer 13.
  • the brazing material is a material containing silver (Ag) and active metal powder, and when forming the brazing material layer, a brazing material in the form of a paste containing a solvent or the like is arranged. Therefore, the bonding layer 13 contains silver and an active metal.
  • the active metal is at least one metal selected from the group consisting of titanium (Ti) and zirconium (Zr).
  • the thickness of the ceramic substrate 11 and the copper plate 12 is not particularly limited, but typically, the former has a thickness of about 0.2 mm to 0.4 mm, and the latter has a thickness of 0.3 mm to 1.2 mm. The one with a certain thickness is used.
  • the bonding layer 13 has a thickness corresponding to the thickness of the brazing material layer formed at the time of brazing, but is generally provided to a thickness of about submicron to several microns.
  • the bonding layer 13 contains nitrogen (N) and silicon (Si) supplied from the ceramic substrate 11 at the time of brazing. At least a portion of the supplied nitrogen or silicon forms a compound with the active metal. Therefore, the bonding layer 13 contains an active metal nitride and a siliconized product.
  • the bonding layer 13 further contains copper (Cu) supplied from the copper plate 12 during brazing. Copper is dissolved in the substance constituting the bonding layer 13.
  • the mode may be such that the copper contained in the brazing material and the copper supplied from the copper plate 12 are contained in the bonding layer 13.
  • the bonding layer 13 has a first interface 111 with the ceramic substrate 11 and a second interface 112 with the copper plate 12.
  • the bonding layer 13 includes a first interface layer 121, an intermediate layer 122, and a second interface layer 123.
  • the first interface layer 121 exists along the first interface 111.
  • the second interface layer 123 exists along the second interface 112.
  • the intermediate layer 122 exists apart from the first interface 111 and the second interface 112, and exists between the first interface layer 121 and the second interface layer 123.
  • the first interface layer 121, the intermediate layer 122, and the second interface layer 123 are made of polycrystals.
  • the bonding layer 13 further includes a nanoparticle layer 131 as shown in FIG.
  • the nanoparticle layer 131 is provided in the first interface layer 121 and exists along the first interface 111.
  • the nanoparticle layer 131 contains a plurality of nanoparticles 141.
  • the plurality of nanoparticles 141 have a particle size of 50 nm or less.
  • the nanoparticle layer 131 has a high surface tension. This contributes to the improvement of the adhesion strength between the ceramic substrate 11 and the bonding layer 13.
  • the nanoparticle layer 131 contains silver and copper at a larger atomic fraction than the portion of the first interface layer 121 other than the nanoparticle layer 131.
  • the silver present in the nanoparticle layer 131 remains in the bonding layer 13 without diffusing into the copper plate 12.
  • the nanoparticles 141 contain more silver than the surrounding nanoparticle layer 131.
  • the nanoparticle layer 131 has a lower Young's modulus than the other parts of the bonding layer 13.
  • FIG. 3 is a diagram schematically showing the microstructure of the bonding layer 13.
  • the bonding layer 13 includes a plurality of particles 151 and different phases 152.
  • the plurality of particles 151 form a grain boundary triple point.
  • the heterogeneous phase 152 exists at the formed grain boundary triple point.
  • the heterogeneous phase 152 contains silver.
  • the silver in the heterogeneous phase 152 also remains in the bonding layer 13 without diffusing into the copper plate 12. Due to the presence of the heterogeneous phase 152 in the bonding layer 13, even when stress is generated in the bonding layer 13, the generated stress is relaxed by the heterogeneous phase 152. This prevents cracks from propagating through the bonding layer 13.
  • the ceramic substrate 11 includes a layer 132 containing oxygen.
  • the oxygen-containing layer 132 exists along the first interface 111.
  • the bonding layer 13 in addition to the active metals (titanium, zirconium) contained in the brazing material, the bonding layer 13 also contains nitrogen and silicon contained in the ceramic substrate 11 and copper derived from the copper plate 12. Exists. On the other hand, most of the silver present in the brazing material is diffused into the copper plate 12.
  • the concentration distribution of these elements is the first interface layer 121, the intermediate layer 122, and the bonding layer 12 in the bonding layer 13.
  • the provision of the second interface layer 123 is related to the provision of the nanoparticle layer 131 in the first interface layer 121. As a result, it is related to ensuring the bonding strength between the ceramic substrate 11 and the copper plate 12 by the bonding layer 13 and other substrate characteristics.
  • the atomic fraction (concentration) of nitrogen derived from the ceramic substrate 11 in the bonding layer 13 is maximum at the first interface 111, and decreases as it moves away from the first interface 111 and approaches the second interface 112. , The smallest at the second interface 112. Therefore, the atomic fraction of nitrogen in the intermediate layer 122 is smaller than the atomic fraction of nitrogen in the first interface layer 121 and larger than the atomic fraction of nitrogen in the second interface layer 123.
  • the atomic fraction of nitrogen in the bonding layer 13 changes substantially continuously in the thickness direction.
  • the atomic fraction in the bonding layer 13 of silicon derived from the ceramic substrate 11 like nitrogen is the minimum at the first interface 111, and as it moves away from the first interface 111 and approaches the second interface 112, Tends to grow.
  • the atomic fraction of silicon in the bonding layer 13 changes discontinuously at the interface between the first interface layer 121 and the intermediate layer 122 and the interface between the intermediate layer 122 and the second interface layer 123.
  • the atomic fraction of the active metal in the bonding layer 13 is also the minimum at the first interface 111, and tends to increase as it moves away from the first interface 111 and approaches the second interface 112.
  • the atomic fraction of the active metal in the bonding layer 13 changes substantially continuously in the thickness direction.
  • the atomic fraction of nitrogen is maximum at the first interface 111 in contact with the ceramic substrate 11.
  • the bonding substrate 1 according to the present embodiment in which the atomic fraction of nitrogen in the bonding layer 13 is maximum at the first interface 111, is compared with the bonding substrate having no such nitrogen distribution. Therefore, the adhesion between the ceramic substrate 11 and the bonding layer 13 is high.
  • the atomic fractions of silicon and the active metal are maximum at the second interface 112 in contact with the copper plate 12.
  • the sum of the atomic fractions of silicon and the active metal is maximum at the second interface 112 in contact with the copper plate 12.
  • the bonding substrate 1 according to the present embodiment in which the atomic fraction of active metal and silicon in the bonding layer 13 is maximum at the second interface 112, has such a distribution of active metal and silicon.
  • the adhesion between the copper plate 12 and the bonding layer 13 is higher than that of a non-bonded substrate.
  • both the adhesion between the ceramic substrate 11 and the bonding layer 13 and the adhesion between the copper plate 12 and the bonding layer 13 are enhanced.
  • the first interface layer 121 contains the nitride of the active metal as the main component
  • the second interface layer 123 contains the siliconized product of the active metal as the main component
  • the intermediate layer 122 contains the nitride of the active metal. It contains a solid solution of nitride and silicon as the main component.
  • the nitride of the active metal contains titanium nitride having a composition represented by the composition formula TiN x .
  • the first interface layer 121 contains the titanium nitride as a main component.
  • the siliconized product of the active metal contains titanium siliconized having a composition represented by the composition formula Ti 5 Si 3 .
  • the second interface layer 123 contains the titanium siliconized as a main component.
  • the intermediate layer 122 contains a solid solution of titanium nitride and silicon having a composition represented by the composition formula TiN x as a main component.
  • the atomic fraction of copper in the bonding layer 13 is the largest in the intermediate layer 122, and is smaller than that in the intermediate layer 122 at the first interface 111 and the second interface 112.
  • the intermediate layer 122 is a layer having a smaller Young's modulus than the first interface layer 121 and the second interface layer 123, and therefore, the stress is easily relaxed as compared with those layers. It is a layer.
  • the atomic fraction of copper in the bonding layer 13 changes discontinuously at the interface between the first interface layer 121 and the intermediate layer 122 and the interface between the intermediate layer 122 and the second interface layer 123.
  • the atomic fraction of copper in the intermediate layer 122 is preferably 1 atomic% or more and 10 atomic% or less. When the atomic fraction of copper in the intermediate layer 122 is less than 1 atomic%, it tends to be difficult to relieve the stress generated in the intermediate layer 122. When the atomic fraction of copper in the intermediate layer 122 is larger than 10 atomic%, the copper dissolved in the intermediate layer 122 is likely to be dissolved and a depletion layer is easily formed in the intermediate layer 122 when the etching described below is performed. Tends to be.
  • FIG. 4 is a flowchart showing the flow of manufacturing of the bonding substrate 1 according to the present embodiment.
  • FIG. 6 and FIG. 7 are cross-sectional views schematically showing an intermediate product obtained in the process of manufacturing the bonding substrate 1.
  • the arrangement of any one of the set of the copper plate 12U and the bonding layer 13U and the set of the copper plate 12L and the bonding layer 13L may be omitted. In that case, in the procedure shown below, the process for the portion where the arrangement is omitted is appropriately omitted.
  • the steps S101 to S104 shown in FIG. 4 are sequentially executed.
  • step S101 as shown in FIG. 5, brazing material layers 13UA and 13LA are formed on the main surfaces 101U and 101L of the ceramic substrate 11, respectively.
  • a paste containing the brazing filler metal and a solvent is prepared.
  • the paste may further contain binders, dispersants, defoamers and the like.
  • the prepared paste is screen-printed on the main surfaces 101U and 101L of the ceramic substrate 11, and the first and second screen printing films are formed on the main surfaces 101U and 101L of the ceramic substrate 11, respectively.
  • organic components such as a solvent contained in the formed first and second screen printing films are volatilized.
  • the first and second screen printing films are changed to the brazing material layers 13UA and 13LA, respectively.
  • the brazing filler metal layers 13UA and 13LA may be formed by a method different from this method.
  • the brazing material contains metal powder and hydride powder of active metal.
  • the metal powder contains silver.
  • the metal powder may contain a metal other than silver.
  • the metal powder may contain copper (Cu), indium (In), tin (Sn) and the like.
  • the brazing material preferably consists of a powder having an average particle size of 0.1 ⁇ m or more and 10 ⁇ m or less.
  • a powder having such an average particle size as a brazing material, the brazing material layers 13UA and 13LA can be formed thinly.
  • the average particle size can be obtained by calculating D50 (median diameter) from the particle size distribution. Further, in the present embodiment, the particle size distribution of various powders is measured by a commercially available laser diffraction type particle size distribution measuring device.
  • the brazing filler metal layers 13UA and 13LA are preferably formed to a thickness of 0.1 ⁇ m or more and 10 ⁇ m or less, and more preferably 0.1 ⁇ m or more and 5 ⁇ m or less.
  • the silver powder contained in the brazing material one in which D50 in the particle size distribution is in the range of 0.5 ⁇ m to 1.5 ⁇ m and D95 is in the range of 2.0 ⁇ m to 3.5 ⁇ m is used.
  • the particle size distribution of the silver powder satisfying these conditions will be referred to as a specified particle size distribution.
  • the brazing material preferably contains 40% by weight or more and 80% by weight or less of silver.
  • step S102 as shown in FIG. 6, copper plates 12UA and 12LA are arranged on the formed brazing material layers 13UA and 13LA, respectively.
  • an intermediate product 1A including the ceramic substrate 11, the brazing material layer 13UA, the copper plate 12UA, the brazing material layer 13LA, and the copper plate 12LA can be obtained.
  • step S103 the obtained intermediate product 1A is pressure-heated.
  • the brazing material layers 13UA and 13LA are changed to the bonding layers 13UB and 13LB shown in FIG. 7, respectively, and an intermediate product 1B including the ceramic substrate 11, the bonding layer 13UB, the copper plate 12UA, the bonding layer 13LB and the copper plate 12LA is obtained. ..
  • the bonding layers 13UB and 13LB bond the copper plates 12UA and 12LA to the ceramic substrate 11, respectively.
  • the copper contained in the copper plates 12 (12UA and 12LA) is contained in the brazing material layer 13UA and the brazing material layer 13UA, respectively, on the side of the second interface 112 (FIG. 2). It is supplied to 13LA and diffuses into the brazing layers 13UA and 13LA. Further, the silver contained in the brazing filler metal layers 13UA and 13LA is sequentially diffused into the copper plate 12 from the vicinity of the second interface 112. As a result, in the brazing filler metal layers 13UA and 13LA, a concentration gradient is formed in which the atomic fraction of silver becomes relatively low and the atomic fraction of the active metal becomes relatively high toward the second interface 112. ..
  • nitride of the active metal reacts with the active metal contained in the brazing filler metal layers 13UA and 13LA to form a nitride of the active metal.
  • the nitride of the active metal is sequentially grown from the side of the ceramic substrate 11 (from the side of the first interface 111) in the thickness direction. At that time, in the vicinity of the first interface 111, a plurality of nanoparticles 141 containing a large amount of silver remaining without diffusing on the copper plate 12 are formed in the nitride of the active metal. As a result, the nanoparticle layer 131 is formed.
  • silicon which has a higher diffusion rate than nitrogen, diffuses significantly toward the second interface 112 side than nitrogen. Furthermore, it reacts with the active metal whose atomic fraction is relatively increased on the side of the second interface 112 to form a siliconized product of the active metal.
  • the atomic fraction distribution is preferably realized when the silver powder contained in the brazing material satisfies the above-mentioned specified particle size distribution.
  • the brazing material layer 13UA And in 13LA the proportion of silver particles with a large particle size (that is, volume) is relatively large. Therefore, the diffusion of silver to the copper plate 12 does not proceed sufficiently during the pressure heat treatment, and a large amount of silver remains in the bonding layer 13 (13UB and 13LB).
  • the silver copper plate 12 is used. Most of the silver in the brazing layer 13UA and 13LA diffuses into the copper plate 12 and in the vicinity of the first interface 111 without forming the concentration gradient as described above due to the rapid diffusion of silver. Almost never remains. Therefore, the atomic fraction of the active metal is relatively high also on the first interface 111 side, and the silicon supplied from the ceramic substrate 11 easily reacts with the active metal without going to the vicinity of the second interface 112. Become. In addition, nanoparticles 141 are not formed. In this case as well, a distribution of atomic fractions that improves the bonding strength cannot be obtained, which is not preferable.
  • the pressure heat treatment for the intermediate product 1A is preferably performed by hot pressing.
  • the intermediate product 1A is preferably heated in vacuum or in an inert gas according to a temperature profile having a maximum temperature of 800 ° C. or higher and 900 ° C. or lower, and the maximum surface pressure is increased.
  • the pressure is applied in the thickness direction of the ceramic substrate 11 according to the surface pressure profile of 5 MPa or more and 25 MPa or less.
  • step S104 the bonding layer 13UB, the copper plate 12UA, the bonding layer 13LB, and the copper plate 12LA are patterned.
  • the bonding layers 13UB and 13LB are changed to the patterned bonding layers 13U and 13L shown in FIG. 1, respectively.
  • the copper plates 12UA and 12LA are changed to the patterned copper plates 12U and 12L shown in FIG. 1, respectively.
  • FIG. 8 is a flowchart showing the flow of patterning of the bonding layer and the copper plate in the production of the bonding substrate 1 according to the present embodiment.
  • 9 and 10 are cross-sectional views schematically showing an intermediate product obtained in the process of patterning the bonding layer 13 and the copper plate 12.
  • step S111 the copper plates 12UA and 12LA are hard-etched.
  • the bonding layer 13UB includes a first portion 161U between the ceramic substrate 11 and the etched copper plate 12UC, and a second portion 162U not between the ceramic substrate 11 and the etched copper plate 12UC. Is formed.
  • the bonding layer 13LB includes a first portion 161L between the ceramic substrate 11 and the etched copper plate 12LC, and a second portion 162L not between the ceramic substrate 11 and the etched copper plate 12LC. Is formed.
  • an etching solution such as an iron chloride aqueous solution system or a copper chloride aqueous solution system can be used.
  • step S112 the second portions 162U and 162L are etched.
  • the second portions 162U and 162L are removed, leaving the first portions 161U and 161L as shown in FIG.
  • the remaining first portions 161U and 161L become the bonding layers 13U and 13L, respectively.
  • An etching solution such as an aqueous ammonium fluoride solution can be used for etching the second portions 162U and 162L.
  • step S113 the copper plates 12UC and 12LC are soft-etched. As a result, the ends of the copper plates 12UC and 12LC are removed, and the patterned copper plates 12U and 12L shown in FIG. 1 are obtained. Further, as shown in FIG. 1, the bonding layer 13U is formed with an inter-plate portion 171U between the ceramic substrate 11 and the copper plate 12U and a protruding portion 172U protruding from between the ceramic substrate 11 and the copper plate 12U. Will be done. Similarly, in the bonding layer 13L, an inter-plate portion 171L between the ceramic substrate 11 and the copper plate 12L and a protruding portion 172L protruding from between the ceramic substrate 11 and the copper plate 12L are formed. For the soft etching of the copper plates 12UC and 12LC, an etching solution such as an iron chloride aqueous solution system or a copper chloride aqueous solution system can be used.
  • an etching solution such as an iron chloride aqueous solution system or a copper
  • the bonding substrate 1 was manufactured according to the manufacturing method described above. Titanium was selected as the active metal. A ceramic substrate 11 having a thickness of 0.32 mm was prepared, and a copper plate 12 having a thickness of 0.8 mm was prepared. As the brazing material, a material containing 40 wt% of titanium and 60 wt% of silver was used. As the silver powder, one having a D50 of 1.0 ⁇ m and a D95 of 2.5 ⁇ m was used. The brazing filler metal layer was formed to a thickness of 4 ⁇ m. As a pressure heat treatment for forming the bonding layer 13, hot pressing was performed in vacuum using a temperature profile having a maximum temperature of 830 ° C. and a surface pressure profile having a maximum surface pressure of 15 MPa.
  • a sample for analysis was prepared by performing focused ion beam (FIB) processing or the like on the manufactured bonding substrate 1, and the cross section of the bonding substrate 1 was observed and analyzed for the sample.
  • FIB focused ion beam
  • FIG. 11 is a diagram showing a STEM image used for the observation
  • FIG. 12 is a diagram showing a partially enlarged image thereof.
  • 11 (a) and 12 (a) are bright field (BF) -STEM images
  • FIGS. 11 (b) and 12 (b) are high-angle scattering rings having the same field of view as the corresponding BF-STEM images, respectively.
  • Dark field (HAADF) -STEM image Note that FIGS. 12 (a) and 12 (b) are images in the vicinity of the first interface 111 in the portion A shown in FIG. 11 (a).
  • FIGS. 11 and 12 are images of a joint portion between the protruding portion 172U of the joint layer 13 and the ceramic substrate 11 without the joint between the copper plate 12 and the joint layer 13, and FIGS. 11A and 12A.
  • the layer 99 in the BF-STEM image and the HAADF-STEM image shown in FIG. 11B is a layer of a protective film for FIB processing.
  • the first interface layer 121, the intermediate layer 122, and the second interface layer 123 constituting the bonding layer 13 are polycrystalline. You can see that it consists of a body.
  • the visual field range of the STEM image in FIGS. 11 and the following figures does not include the copper plate 12, and therefore the interface between the copper plate 12 and the inter-plate portion 171U of the bonding layer 13 (13U).
  • the second interface 112 is not included, the properties of the protruding portion 172U continuous from the inter-plate portion 171U can be regarded as substantially the same as the inter-plate portion 171U, so that the field of view of the STEM image shown in FIG. It can be considered that the first interface layer 121, the intermediate layer 122, and the second interface layer 123 are present in the bonding layer 13 included in the range.
  • the first interface 111 can be clearly grasped from the difference in contrast. Moreover, in the latter, it was also confirmed that, in the bonding layer 13, nano-sized particles (nanoparticles) having a diameter remarkably brighter than the surroundings were scattered in the range within about 100 nm from the first interface 111. Will be done. In other words, it is confirmed that the nanoparticle layer 131 containing the plurality of nanoparticles 141 exists in the bonding layer 13 along the first interface 111.
  • FIG. 13 is a diagram showing mapping results for each element.
  • FIG. 14 is a partially enlarged image of each of the mapping images shown in FIG. 13 in the same field of view as the partially enlarged image of the STEM image shown in FIG. Specifically, FIGS. 13 (a), 13 (b), 13 (c), 13 (d), 13 (e), 13 (f), and 13 (g) are in this order. , Carbon, nitrogen, oxygen, silicon, titanium, copper and silver mapping images are shown. 14 (a), 14 (b), 14 (c), 14 (d), 14 (e), 14 (f), and 14 (g), respectively, in this order. Is shown.
  • the bonding layer 13 contains the image. It is confirmed that nitrogen is present in.
  • the nanoparticle layer 131 contains silver and copper. It is determined that the nanoparticle 141 contains more silver than the surrounding nanoparticle layer 131, and the nanoparticles 141 are determined to contain more silver than the surrounding nanoparticle layer 131.
  • FIG. 15 is a HAADF-STEM image for a partial range of the field of view of the STEM image shown in FIG. 11, showing the four extraction positions P1, P2, P3, and P4.
  • the extraction positions P1, P2, P3, and P4 are selected from the second interface layer 123, the intermediate layer 122, the first interface layer 121, and the nanoparticle layer 131, respectively.
  • Table 1 shows the concentrations (atomic fractions) of nitrogen, oxygen, silicon, titanium, copper and silver at the extraction positions P1, P2, P3 and P4.
  • the atomic fraction of nitrogen in the bonding layer 13 tends to be larger toward the first interface 111 and smaller toward the second interface 112. It is also confirmed that the atomic fractions of silicon and titanium in the bonding layer 13 tend to be smaller toward the first interface 111 and larger toward the second interface 112.
  • silver is present only in trace amounts in most of the junction layer 13
  • the nanoparticles layer 131 containing the plurality of nanoparticles 141 is more ubiquitous than the rest of the junction layer 13 and copper. It is also confirmed that although is unevenly distributed in the nanoparticle layer 131 like silver, the atomic fraction is the largest in the intermediate layer 122.
  • FIG. 16 is an enlarged HAADF-STEM image near the grain boundary triple point 191.
  • FIG. 17 is a diagram showing an EDX spectrum at and in the vicinity of the grain boundary triple point 191.
  • FIG. 17 (a) shows the EDX spectrum at the measurement position PA inside the grain boundary triple point 191 shown in FIG. 16, and
  • FIG. 17 (b) shows the measurement position PB outside the grain boundary triple point 191 shown in FIG. The EDX spectrum in is shown.
  • FIG. 18 is a BF-STEM image showing five extraction positions P11, P12, P13, P14, and P15 in a field of view substantially the same as in FIG. 11 (a).
  • the extraction position P11 is selected from the second interface layer 123.
  • the extraction positions P12 and P14 are selected from the intermediate layer 122.
  • the extraction position P13 is selected from the first interface layer 121 other than the nanoparticle layer 131.
  • the extraction position P15 is selected from the nanoparticle layer 131.
  • FIG. 19 is a diagram showing a measurement target region and an EELS intensity map showing the distribution of each element in the region.
  • FIG. 19 (a) is a diagram showing a rectangular measurement target region R in the same HAADF-STEM image as in FIG. 15, FIG. 19 (b), FIG. 19 (c), and FIG. 19 ( d) is an EELS intensity map showing the distribution of nitrogen, oxygen and titanium concentrations in region R, respectively. From FIGS. 19 (b), 19 (c), and 19 (d), it is confirmed that the oxygen-containing layer 132 exists along the first interface 111 of the ceramic substrate 11.
  • Example 2 In this example, a peel test of the copper plate 12 was performed on the bonding substrate 1 manufactured under the same conditions as in the first embodiment, and the adhesion of the copper plate 12 was evaluated.
  • a bonded substrate produced by the method disclosed in Patent Document 2 was prepared, and a peel test was conducted under the same conditions.
  • the bonding substrate according to the comparative example was formed so that the Ag-rich phase was discretely provided between the copper plate and the bonding layer, but no voids or Ag—Cu layers were present.
  • the peel test was performed by holding the end of the copper plate with a width of 2 mm in a state where the bonding substrate to be tested was placed and fixed horizontally, and applying a tensile force vertically upward to the holding portion. The tensile force was gradually increased until the copper plate was peeled off, and the magnitude of the tensile force per unit width when the copper plate was finally peeled off was defined as the bonding strength between the copper plate and the ceramic substrate in the bonding substrate.
  • the bonding strength of the bonding substrate 1 according to the embodiment was 40 kN / m.
  • the bonding strength of the bonding substrate according to the comparative example remained at 20 kN / m.

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WO2024166907A1 (ja) * 2023-02-07 2024-08-15 三菱マテリアル株式会社 金属／窒化物積層体、および、絶縁回路基板
WO2024176599A1 (ja) * 2023-02-24 2024-08-29 デンカ株式会社 回路基板の製造方法、回路基板、及びパワーモジュール

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