WO2016056637A1 - 放熱基板及び該放熱基板の製造方法 - Google Patents
放熱基板及び該放熱基板の製造方法 Download PDFInfo
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- WO2016056637A1 WO2016056637A1 PCT/JP2015/078685 JP2015078685W WO2016056637A1 WO 2016056637 A1 WO2016056637 A1 WO 2016056637A1 JP 2015078685 W JP2015078685 W JP 2015078685W WO 2016056637 A1 WO2016056637 A1 WO 2016056637A1
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- Prior art keywords
- metal
- heat dissipation
- alloy composite
- metal layer
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Images
Classifications
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- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
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- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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Definitions
- the present invention is mounted on a package of a high performance semiconductor module (hereinafter abbreviated as PKG), has a metal layer with few defects on the surface, and has a linear expansion coefficient suitable for the semiconductor module and a large thermal conductivity.
- PKG high performance semiconductor module
- the present invention relates to an inexpensive metal diamond-based heat dissipation substrate and a manufacturing method thereof.
- Semiconductor modules have applications such as LSIs, IGBTs, power semiconductors, semiconductors for radio waves and optical communications, lasers, LEDs, sensors, etc., and the structures vary depending on the performance required for these.
- the semiconductor module is a highly sophisticated precision instrument composed of materials made of materials with different linear expansion coefficients and thermal conductivities, and the heat dissipation board used in the PKG has many proposals for various composite materials and shapes. Has been.
- the heat dissipation board of the semiconductor module must have a suitable linear expansion coefficient in order to ensure performance and life in the manufacture of PKG and soldering of semiconductor devices. Also for the thermal conductivity, a high value is required to dissipate and cool the heat of the semiconductor device to ensure performance and life. In addition, in order to join various members and semiconductor devices, it is also very important that good plating is easily performed.
- Patent Document 1 As a countermeasure, CuW and CuMo (Patent Document 1), which can change and adjust the linear expansion coefficient and can cope with the linear expansion coefficient of high-performance semiconductor modules, have been developed. Moreover, AlSiC (patent document 2) was developed as a response
- the quality of plating is important for heat dissipation boards.
- a semiconductor module manufacturer joins a semiconductor device or an insulating plate with solder, if there are many voids at the bonding interface, the heat flow is interrupted, and the semiconductor device or the insulating plate is peeled off or broken. For this reason, a heat dissipation substrate having a surface layer with few defects that can be subjected to final Ni-based plating capable of good soldering is required.
- the final Ni-based plating has various forms to ensure quality. In order to correspond to these forms, there is a case where plating is performed by a heat sink substrate manufacturer and a case where plating is performed by a PKG manufacturer. Therefore, various Ni-based plating, solder materials, soldering conditions, etc. have been developed. In these developments, in order to ensure the quality of the final Ni-based plating, it is extremely important that the surface layer of the heat dissipation substrate has few defects, and various heat dissipation substrates have been developed to realize this.
- the Cu heat dissipation board has few surface layer defects, so it is easy to apply a good final Ni plating.
- CuW and CuMo machined products and polished products are prone to surface defect problems when the relative density is low, and it is said that the relative density must be 99% or more of the true density for practical use.
- the surface layer formed above and below them is a Cu layer, so problems in applying the final Ni plating can be avoided.
- AlSiC has a problem that it is difficult to plate ceramic SiC even if the relative density is 99% or more of the true density.
- the composite material has defects such as pinholes (fine holes on the surface) or SiC that is difficult to plate, a pure Al foil or an infiltrated metal Al layer is provided on the surface of the composite material.
- the final Ni-based plating can be satisfactorily applied.
- a metal diamond heat dissipation substrate As a heat dissipation substrate for high-performance semiconductor modules, a metal diamond heat dissipation substrate is promising because there is a possibility that high thermal conductivity can be obtained, and various research and development have been conducted and reported so far.
- Patent Document 4 There is a report (Patent Document 4) that, by sintering a green compact in which a main metal, an additive metal, and a diamond powder are sintered, a carbide of the additive metal is formed on the diamond surface and high thermal conductivity is obtained.
- the alloy composite obtained by such a sintering method is unstable and a high true density cannot be obtained, there are many pinholes on the surface of the alloy composite and the quality of the final Ni-based plating is good. There is a problem that it cannot be secured. For this reason, an alloy composite that can be used as a heat dissipation substrate has not been obtained.
- Patent Document 5 There is a report (Patent Document 5) that a high thermal conductivity can be obtained by using a manufacturing method in which metal is infiltrated into a skeleton in which a carbide film of an additive metal is formed on the surface layer of diamond powder.
- this manufacturing method can obtain a higher true density and thermal conductivity than the sintering method, there is a problem that the composition of the skeleton varies due to the unstable structure of the skeleton.
- the final Ni plating having the quality required for the heat dissipation substrate cannot be applied. Therefore, the composite material could not be used as a heat dissipation substrate.
- Patent Document 6 a green powder obtained by sintering a Cu-plated powder on diamond powder is sintered by a SPS (Spark Plasma Sintering) method to obtain high thermal conductivity.
- SPS Spark Plasma Sintering
- Cu plating on diamond powder is expensive, and in addition, in order to obtain high thermal conductivity by the SPS current sintering method, there is a problem that long-time sintering is required and productivity is low. Further, there is a problem that diamond may be exposed on the surface layer, and the quality of the final Ni-based plating capable of good soldering cannot be ensured.
- Patent Document 7 As a result of forming an infiltrated metal film on the surface layer with high thermal conductivity by pressure infiltrating Al / Si / Mg alloy into a skeleton with SiC ceramic coating on diamond powder (Patent Document 7), There are reports that the quality of the final Ni plating is satisfactory. However, a thin heat dissipation board is not suitable for a heat dissipation board because the surface layer has an infiltrated metal layer having a low thermal conductivity. Further, it is not economical to provide an infiltrated metal layer on the surface layer using a precise jig because the manufacturing difficulty is high and a composite material cannot be produced at low cost. In addition, the surface infiltrated metal film is not necessarily suitable for the final Ni-based plating.
- this production method can be applied only to Al alloys, and the composition range is limited to 60% or less for Al alloys in order to ensure the stability of the skeleton. For this reason, the range which can be used as a heat dissipation board has a limit, and the use was limited.
- Patent Document 8 a PKG (Patent Document 8) was manufactured by silver brazing a pure Cu plate to a composite material in which Cu was infiltrated into a green compact with diamond powder coated with metal or ceramic.
- the cost of applying metal or ceramic coating to diamond powder is high, and in addition, it is necessary to grind and remove excess infiltrated metal on the outer periphery with a diamond grindstone. Not much economic.
- a pure Cu plate is silver brazed to a metal diamond heat dissipation substrate, Cu and the silver brazing material react to form an alloy to form a layer having a low thermal conductivity.
- the composite material which can be used as a heat dissipation board has not been commercialized yet.
- the linear expansion coefficient can be changed and adjusted by changing the ratio of metal to diamond, increasing the ratio of diamond and using large particles of diamond By doing so, it has been reported that a heat dissipation substrate having a large thermal conductivity exceeding the thermal conductivity of Cu or Ag can be obtained.
- the heat dissipation substrate of the present invention is mainly composed of metal and diamond powder as main components, and a metal layer is formed by plating on the surface of an alloy composite made by various manufacturing methods.
- a metal layer is formed by plating on the surface of an alloy composite made by various manufacturing methods.
- the surface layer has a metal layer with few defects, and has a linear expansion coefficient suitable for semiconductor modules and high thermal conductivity.
- a metal diamond-based heat dissipation substrate is obtained.
- the manufacturing method of the heat dissipation board according to the present invention is as follows.
- a metal layer is formed by plating the surface of the alloy composite mainly composed of metal and diamond powder,
- the defect of the metal layer is repaired by heating and pressing the alloy composite formed with the metal layer below the melting point of the metal layer and below the melting point of the alloy composite.
- the “alloy composite” means a powder mixture having a certain self-supporting shape.
- the alloy composite according to the present invention can be obtained, for example, by embossing a mixed powder of metal and diamond, but is preferably produced by liquid phase sintering after embossing. Moreover, you may produce an alloy composite by other methods, such as an infiltration method. Moreover, “below the melting point of the metal layer and below the melting point of the alloy composite” means that the melting point of the metal layer and the alloy composite is lower than the lower temperature.
- the heating and pressurizing treatment is also referred to as solid phase sintering for the sake of convenience.
- the treatment mainly has the purpose of repairing defects in the metal layer, and it is preferable but not essential to reconstruct the internal structure of the alloy composite.
- a metal layer is formed by plating on an alloy composite obtained by a method such as liquid phase sintering after embossing a mixed powder of main metal, additive metal, and diamond, and then heated and pressurized under the above conditions.
- a heat dissipation substrate for a semiconductor module having a metal layer with few defects on the surface layer, a linear expansion coefficient in the range of 6.5 to 15 ppm / K, and a thermal conductivity of 420 W / m ⁇ K or more is obtained.
- the alloy composite mainly composed of a main metal, an additive metal different from the main metal, and a diamond powder.
- the main metal may be at least one of Ag, Cu, Al, and alloys thereof.
- the additive metal may be at least one of Ti, Cr, Co, Mn, Ni, Fe, B, Y, Si, Mg, and Zn, and the amount of addition is the entire alloy composite. It is preferable to be 1 vol% or more and 15 vol% or less.
- the powder metallurgy sintering method is the most accurate method for manufacturing various products at the lowest cost, and it is highly possible that small and medium-sized products can be manufactured in near net shape. With this technology, various semiconductor components have been developed. It has been put into practical use.
- alloy composites obtained by liquid-phase sintering of mixed powders of mixed powders of main metal, additive metal, and diamond may be unstable due to low relative density. Therefore, even if the metal layer is formed by plating, a large defect is hardly generated. However, it cannot be said that the carbide of the added metal and the main metal are necessarily easily plated. In addition, since the sinterability is poor, voids are easily generated at the interface between the alloy composite and the metal layer. For these reasons, there is a problem that the quality of the final Ni-based plating cannot be ensured. Further, when the thickness of the metal layer is increased, the adhesiveness is lowered, and many voids are generated inside. Moreover, when the surface layer particles are large, irregularities may be formed and fall off.
- an alloy composite is used as a method of performing the final Ni-based plating that can be soldered well even with an alloy composite obtained by liquid phase sintering of a mixed powder of main metal, additive metal, and diamond.
- an alloy composite is used.
- the adhesion of the metal layer can be improved, and defects such as internal voids, pinholes, and roughness of the metal layer can be repaired.
- the alloy composite can be further densified, and the characteristics can be improved and stabilized.
- the quality of the heat dissipation board of high performance modules has been confirmed by the solder void ratio when the final Ni plating is applied to the heat dissipation board and soldered to a semiconductor device or insulating board. Therefore, by measuring the solder void ratio, it is confirmed that if a metal layer with few defects is formed on the surface layer, the final Ni-based plating quality can be secured on the heat dissipation substrate, and good soldering that passes strict standards can be achieved. did.
- the heat dissipation board according to the present invention is: An alloy composite mainly composed of a main metal, a different type of additive metal from the main metal, and diamond powder, and a metal layer formed on the surface of the alloy composite;
- the linear expansion coefficient is 6.5 ppm / K or more and 15 ppm / K or less, the thermal conductivity is 420 W / m ⁇ K or more, and the ratio of defects on the surface of the metal layer is 5% or less.
- the defects on the surface are so-called pinholes, and the ratio of the area occupied by such pinholes can be evaluated by, for example, the above-described solder void ratio.
- alloy composite means a mixture of powders having a certain self-supporting shape, similar to the “alloy composite” in the method of manufacturing a heat dissipation board according to the present invention.
- the alloy composite may be a stamped body of a mixed powder of a main metal, an additive metal, and diamond, but is preferably a product obtained by liquid phase sintering of the stamped body.
- the melting point of the metal layer and the alloy composite is below the melting point in an atmosphere that is difficult to oxidize such as in a vacuum.
- the thermal radiation board which can ensure the final Ni-type plating quality which can be soldered favorable. It is also possible to improve the relative density and thermal conductivity by densifying the alloy composite.
- the main metal When heat resistance is required for the heat dissipation substrate, the main metal may be Ag or Cu, or an alloy thereof, and when weight reduction is required, the main metal may be Al or an Al alloy.
- the range of the linear expansion coefficient comparable to that of the heat dissipation substrate of CuW, CuMo, and AlSiC can be covered, and an alloy composite with good soldering and high thermal conductivity can be produced.
- the shape of the heat dissipation board is also submount (several millimeters square x thickness 0.1 to 1 mm), flat plate (10 to 250 mm square x thickness 0.8 to 5 mm), screwed flat plate (10 -250mm square x thickness 0.8-5mm), flat plate, three-dimensional shape (size 10-50mm x thickness 1-5mm), etc.
- the heat dissipation substrate according to the present invention diamond chipping or grain separation on the surface of the alloy composite by grinding with a diamond grindstone, particularly the surface of the alloy composite Even if the interface between the exposed diamond and the metal layer peels off and metal deposition is performed, a good final Ni-based plating may not be achieved.
- the metal layer such as Ti, Cr, Au, and Pt is deposited on the alloy composite, and then the metal layer is formed by plating, and then the heating and pressurizing are performed, thereby eliminating the above problem. As a result, a good final Ni-based plating can be secured.
- an alloy composite produced by liquid phase sintering or the like is used at a high temperature just below the melting point at a high pressure. After pressurization, a metal layer may be formed by plating, and the alloy composite formed with the metal layer may be heated and pressurized.
- the heating and pressurization can be performed in an atmosphere of vacuum, reduced pressure, non-oxidation, reduction, inert gas, etc., but the apparatus becomes large and requires time for sintering.
- the heat dissipation substrate according to the present invention can be manufactured easily and inexpensively.
- this manufacturing method does not require processing such as slicing, grinding, and cutting, a large-diameter diamond particle can be used to obtain a near net shape heat dissipation substrate with high thermal conductivity.
- the present invention is a technology that can easily provide a metal layer with few defects that can be applied to a metal diamond alloy composite by applying existing technology. Further, one embodiment of the present invention is a technique that enables a near-net shape manufacturing of a heat dissipation substrate using a metal / additive / diamond alloy composite by a new technique of heating and pressurizing in water. Furthermore, the relative density and thermal conductivity of the alloy composite can be improved and stabilized by heating and pressing after plating.
- the present invention can produce a high-performance heat dissipation substrate using a metal / addition metal / diamond alloy composite in a near net shape that could not be produced by CuW, CuMo, AlSiC, or the like.
- the main metal, the additive metal, and the diamond powder are mixed and embossed, and then liquid phase sintering is performed to produce an alloy composite, and the metal composite is formed on the alloy composite.
- the surface layer has a metal layer with few defects, and the coefficient of linear expansion is 6.5 ppm / K to 15 ppm / K, and the thermal conductivity is 420 W / m It is possible to obtain a heat sink substrate for a semiconductor module with a new idea that is K or more and low in price.
- the coefficient of linear expansion is 6.5 ppm / K to 15 ppm / by mixing the additive metal and diamond powder optimally and performing liquid phase sintering after embossing.
- a heat dissipation substrate with a thermal conductivity of 420 W / m ⁇ K or higher in a range of K or lower.
- the thermal conductivity varies greatly and the thermal conductivity is stable.
- a metal layer is formed by plating on the surface of an alloy composite mainly composed of metal and diamond powder, and then heated and pressed below the melting point of the metal phase and the alloy composite.
- the heat treatment and pressure treatment are also referred to as “solid-phase sintering” for convenience, and a metal layer with few defects is formed on the surface layer to improve and stabilize the thermal conductivity.
- the “alloy composite” means one produced in a lump shape.
- the alloy composite can be obtained by, for example, embossing a mixed powder of metal and diamond, but it is preferable to produce a high-density alloy composite by performing liquid phase sintering after embossing. Moreover, you may produce an alloy composite by other methods, such as an infiltration method.
- heat resistance it is desirable to use Ag, Cu, or an alloy thereof as the main metal.
- Al or an Al alloy it is desirable to use Al or an Al alloy as the main metal.
- the additive metal is not particularly specified as long as it is an element that can form a carbide with diamond or alloy with the main metal, but Ti, Cr, Co, Mn, Ni, Fe, B, Y, Si, Mg, Zn or the like, the amount of which is 1 vol% or more and 15 vol% or less of the whole alloy composite, and there is no problem if it is effective even with a plurality of types. It should be noted that the thermal conductivity does not exceed 420 W / m ⁇ K even if the amount of the added metal is less than 1 vol% or exceeds 15 vol%.
- the main metal is Ag, Cu, or any of these alloys, for example, Ti, Cr, Co, Mn, Ni, Fe, B can be used as the additive metal, and the amount added is an alloy composite. It is desirable to set it to 1 vol% or more and 5 vol% or less of the whole body. Even if the addition amount is less than 1 vol% or exceeds 5 vol%, the thermal conductivity does not exceed 420 W / m ⁇ K. Further, when the main metal is Al or an Al alloy, for example, Si can be used as the additive metal, and the addition amount is desirably 5 vol% or more and 15 vol% or less of the entire alloy composite. Even if the addition amount is less than 5 vol% or exceeds 15 vol%, the thermal conductivity does not exceed 420 W / m ⁇ K. Further, the addition of 1.0 vol% Mg has an effect of stabilizing liquid phase sintering described later.
- the diamond powder desirably has a value of 95% or more in the range of 10 ⁇ m or more and 1000 ⁇ m or less in order to ensure the value of thermal conductivity.
- thermal conductivity 420 W / m ⁇ K or more cannot be obtained. If it is 1000 ⁇ m or more, the effect of improving the thermal conductivity is small, the workability such as cutting is remarkably lowered, and the powder price is significantly increased. Further, even if a mixture of large and small diamond powders inside and outside the above range is used, there is no problem if the amount of diamond powder having a size within the above range is 95% or more.
- Liquid phase sintering Sintering after embossing the mixed powder of main metal, additive metal, and diamond is the temperature at which the main metal liquid phase appears in vacuum, reduced pressure, pressurization, non-oxidation, reducing gas, and inert gas (melting point) ) Liquid phase sintering as described above is preferable.
- the added metal and diamond react with the surface layer of diamond particles to form carbide.
- an alloy layer in which carbide, additive metal, and main metal react can be formed, and an alloy composite mainly composed of metal, additive, and diamond powder can be obtained.
- the metal layer is formed by coating the alloy composite after liquid phase sintering or its abrasive product with plating, and is made of Ag, Cu, Ni, or an alloy thereof, and has a thickness of 5 ⁇ m to 200 ⁇ m. For example, there is no problem on the entire surface of the alloy composite, on the top and bottom, or only on the portion where the semiconductor device is mounted. Particularly, an Ag or Cu metal layer that is soft and has a high thermal conductivity is suitable, and the plating of Ni or an alloy thereof is effective for a large and thick heat dissipation substrate of Al-based diamond. Further, Ag, Cu, Ni, or an alloy thereof may be plated in multiple layers as the metal layer.
- the thickness of the metal layer is 5 ⁇ m or less, it is difficult to provide a metal layer with few defects necessary for the heat dissipation substrate even when heated and pressurized. On the other hand, when the thickness is 200 ⁇ m or more, the metal layer tends to be very unstable, and the cost for plating increases.
- Solid phase sintering after plating can be performed in an atmosphere such as vacuum, reduced pressure, pressurization, non-oxidation, inert gas, flame retardant liquid, non-flammable liquid, etc. It can be manufactured with a near net shape and is advantageous in terms of cost. Defects in the metal layer plated on the surface of the alloy composite can be obtained by heating and pressing under the conditions below the melting point of the metal layer and the alloy composite and between 50 MPa and 500 MPa (conditions equivalent to solid phase sintering). It is possible to restore and further improve and stabilize the thermal conductivity of the alloy composite itself. Its manufacture is possible by hot pressing (hereinafter abbreviated as HP), forging, electric current sintering and the like.
- HP hot pressing
- a thin sheet or wafer When a thin sheet or wafer is solid-phase sintered, it can be manufactured in multiple stages by using HP, which is effective. Also, current sintering is suitable for the near net shape. Furthermore, thermal conductivity can be improved and stabilized by applying temperature and pressure. Since plating of Ag, Cu, Ni and their alloys softens at high temperatures, it is preferable to perform sintering at a temperature of 400 ° C. or higher and a melting point or lower and a pressure of 50 MPa or higher and 500 MPa or lower. When the temperature is 400 ° C. or lower, sufficient repair is difficult. When the temperature is 600 ° C. or higher, large burrs start to appear between the jig and the electrode, and the life of the jig is significantly reduced.
- Al and Al alloys have a low melting point, 500 ° C. or lower is desirable.
- the pressure is preferably 50 MPa or more, and below that, it is difficult to sufficiently repair the metal layer.
- pressure cannot be applied unless a large apparatus is used at 500 MPa or more, it is not economical, and a general jig or electrode may break. For this reason, it is important to select solid-state sintering conditions (temperature and pressure), jigs, and electrodes suitable for the type of alloy composite or metal layer.
- Solid-phase sintering in vacuum or gas requires a long time for heating and pressurization due to the large size of the equipment and is difficult to automate.
- the effect of improving the plating of the metal layer can be obtained in the same way by solid phase sintering in water.
- an alloy composite with a metal layer formed on the surface is sandwiched between metal electrodes in water and subjected to current sintering, so that solid-phase sintering can be achieved in a few tens of seconds and automation Is also possible.
- the effect of improving the plating of the metal layer is improved by repeatedly turning the current on and off while being sandwiched between the metal electrodes.
- the surface roughness of the jig or electrode is transferred to the surface, so it is cut into a predetermined shape with a water jet, high power laser, wire cut, etc. to produce a product. If even higher accuracy is required, the metal layer is polished with abrasive paper or buff to finish to a specified surface roughness, then cut into a specified shape with water jet, high power laser, wire cut, etc. It is also possible to do. Further, when an alloy composite is produced with a near net shape, shape processing is not required, which is advantageous in terms of cost.
- the final plating is performed for the purpose of joining various members, insulating plates, semiconductor devices, etc. to the heat dissipation board by silver brazing or soldering.
- a defect occurs in the system plating, and there arises a problem that good silver brazing and soldering cannot be performed. Even if Ni-based plating becomes multi-layered, defects are transferred one after another, so the problem is not solved.
- the Ni-based plating means Ni or Ni alloy plating.
- solder bonding of a semiconductor device to a heat dissipation board is most important, and a very low void ratio is required.
- various solder materials and technologies have been developed, but SnAgCu (melting point: 218 ° C) is mainly used for Pb-free and high temperature, and it is also used for evaluation.
- Cu Ni heat dissipation substrates have been made of electrolytic Ni, electroless Ni-P, and electroless Ni-B.
- the final plating of the CuW or CuMo-based heat dissipation substrate is performed by electrolytic Ni + electroless Ni-P, electroless Ni-P + electroless Ni-B, and electroless Cu + electroless Ni-P.
- AlSiC is electroless Ni-P + electroless Ni-B.
- the evaluation of the void quality with solder when the final plating is 3 ⁇ m Ni-B is performed.
- the metal layer on the surface of the alloy composite is the first. Since it plays the role of a layer, it is only necessary to apply a Ni-based plating treatment to the final surface layer.
- the plated metal layer is Ni-plated electrolytic Ni, electroless Ni-P, or electroless Ni-B, the final Ni-based plating process itself can be omitted.
- solder quality was evaluated with a standard of 80% or more solder spread according to JIS Z3197 (corresponding international standard ISO94455), but the standard is too loose to match the actual situation, so the standard with a void area of 5% or less Are beginning to be used.
- a laser flash method is used to cut a test piece of ⁇ 10mm x thickness 2mm to 2.5mm from a 25mm x 25mm x 2 to 2.5mm sample (alloy composite with a metal layer on the surface) after solid-phase sintering using a WEDM or power laser.
- the thermal conductivity of RT 25 ° C. was measured using a thermal conductivity meter (TC-7000, ULVAC-RIKO).
- Example 1 Ag-Ti-diamond heat dissipation substrate sample, sample No. 9
- Example 1 Ag-Ti-diamond heat dissipation substrate sample, sample No. 9
- Example 1 Ag-Ti-diamond heat dissipation substrate sample, sample No. 9
- the liquid phase is in vacuum at a temperature of 1100 ° C for 60 minutes.
- Sintering to produce an alloy composite 5 ⁇ m Ag plating treatment was applied to the alloy composite as a metal layer, and then solid phase sintering was performed with HP at a temperature of 400 ° C., a pressure of 50 MPa, and maintained for 30 minutes.
- a blister test was performed, and then 3 ⁇ m Ni ⁇ B plating was performed to evaluate the void quality with solder.
- Table 1 Ag-Ti-diamond heat dissipation substrate sample, sample No. 9
- Example 2 Cu—Cr—Diamond Heat Dissipation Board Sample, Sample No. 15 After mixing 35vol% Ag, 5vol% Cr, 60vol% 100 ⁇ m diamond powder and pressing with a pressure of 500MPa using a 25mm x 25mm mold, the liquid phase is in hydrogen at a temperature of 1200 °C for 60 minutes.
- Example 3 Ag-Ti-Diamond-Residual Cu heat dissipation substrate, Sample No. 24
- 10 vol% Ag, 37 vol% Cu, and 3 vol% Ti After mixing 10 vol% Ag, 37 vol% Cu, and 3 vol% Ti with 30 vol% 100 ⁇ m diamond powder and 20 vol% 30 ⁇ m diamond powder, using a 25 mm ⁇ 25 mm mold, press-molding at a pressure of 500 MPa, Liquid phase sintering is performed in vacuum at a temperature of 1000 ° C. for 60 minutes to prepare an alloy composite. After the alloy composite is subjected to 100 ⁇ m Cu plating as a metal layer, the plated alloy composite 1 is 1 is placed in the ceramic jig 4 of FIG. 1 using a resistance welder, while holding the current at 500 ° C.
- Example 4 Al-Si-Mg-diamond heat dissipation substrate, sample No. 27
- 29vol% Al, 10vol% Si, 1vol% Mg, 60vol% 50 ⁇ m diamond powder was mixed and pressed with a pressure of 500MPa using a 25mm x 25mm mold, then in nitrogen at a temperature of 600 ° C for 60 minutes.
- An alloy composite is prepared by performing phase sintering, the surface layer of the alloy composite is ground, Ti and Ni are combined, and 0.3 ⁇ m is deposited. Solid-state sintering was performed under the conditions of vacuum, temperature 450 ° C, pressure 100 MPa, holding for 10 minutes. After deburring, a fret test was performed, and then 3 ⁇ m Ni ⁇ B plating was performed to evaluate the void quality with solder. The results are shown in Table 2.
- Example 5 Evaluation of a semiconductor module in which a semiconductor device is mounted on a PKG heat dissipation board
- the material such as ceramic and Kovar to hydrogen radiator (temperature expansion coefficient 8.3ppm / K and thermal conductivity 555W / m ⁇ K) in Example 3 in hydrogen at a temperature of 750 ° C
- there is no peeling or cracking make a PKG after confirming that the metal electrode of Si device of 10mm ⁇ 10mm ⁇ 0.7mm is bonded to high temperature AuSn (melting point 280 ° C) solder at 300 ° C, and the void area is less than 3% by ultrasonic.
- a semiconductor module was confirmed, and a heat cycle test ( ⁇ 40 to 125 ° C., 3000 times) was performed on the semiconductor module.
- the same PKG is formed on a 20 wt% CuW heat dissipation board with the same thermal expansion coefficient of 8.3 ppm / K as in Example 3 and the thermal conductivity of 200 W / m ⁇ K.
- a heat cycle test ( ⁇ 40 to 125 ° C., 3000 times) was performed. As a result, no problem such as peeling or cracking occurred in any of the samples.
- this invention is not limited to the present form, The form in the range which can achieve the objective of this invention is included in this invention.
- the specific structure, form, etc. when carrying out the present invention may be other structures as long as the object of the present invention can be achieved.
- the present invention can also be applied to ensure the plating quality of a heat-radiating substrate made of metal diamond by another manufacturing method.
- the heat dissipation substrate according to the present invention has high thermal conductivity and a linear expansion coefficient of 6.5 ppm / K or more and 15 ppm / K or less. Therefore, it can be suitably used as a heat dissipation board on which a high-performance semiconductor module having a linear expansion coefficient of 6.5 ppm / K or more and 15 ppm / K or less, which is widely used in recent years, is mounted.
- a package equipped with these high-performance semiconductor modules can be used for memories, ICs, LSIs, power semiconductors, communication semiconductors, optical devices, lasers, LEDs, sensors, and the like.
- SYMBOLS 1 Material which formed the metal layer in the alloy composite which consists of a metal, an addition metal, and diamond 2 ... Up-and-down upper electrode 3 ... Lower electrode 4 ... Ceramic jig 5 ... Welding machine power supply 6 ... Water 7 ... Diamond 8 ... Metal layer 9... Enlarged cross section of heat dissipation board
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Abstract
Description
金属とダイヤモンドの粉末を主成分とする合金複合体の表面にメッキ処理を行って金属層を形成し、
前記金属層が形成された前記合金複合体を、該金属層の融点以下かつ該合金複合体の融点以下で加熱及び加圧することにより前記金属層の欠陥を修復する
ことを特徴とする。
また、「該金属層の融点以下かつ該合金複合体の融点以下」とは、金属層と合金複合体の融点のうち、より低い温度以下であることを意味する。
上記のように、金属層及び合金複合体の温度以下で(即ち、金属層と合金複合体の固相を維持して)加熱及び加圧処理するという条件が固相焼結で用いられる条件と共通することから、本明細書では、上記の加熱及び加圧する処理を便宜的に固相焼結とも呼ぶ。ただし、その場合でも、当該処理は金属層の欠陥を修復することを主たる目的とするものあり、合金複合体の内部構造を再構成することは好ましいが必須ではない。
主金属、該主金属と異なる種類の添加金属、及びダイヤモンドの粉末を主成分とする前記合金複合体を作製する
ことが望ましい。
また、前記添加金属は、Ti、Cr、Co、Mn、Ni、Fe、B、Y、Si、Mg、及びZnのうちの少なくとも1種類とすることができ、その添加量は合金複合体の全体の1vol%以上15vol%以下とすることが好ましい。
主金属、該主金属と異なる種類の添加金属、及びダイヤモンドの粉末を主成分とする合金複合体と、該合金複合体の表面に形成された金属層を有し、
線膨張係数が6.5ppm/K以上15ppm/K以下であり、熱伝導率が420W/m・K以上であり、前記金属層の表面における欠陥の割合が5%以下である
ことを特徴とする。
既に、主金属がAg、Cu、Alやこれらの合金であれば、添加金属・ダイヤモンドの粉末を最適に混合し型押し後に液相焼結を行うことで線膨張係数6.5ppm/K以上15ppm/K以下の範囲、熱伝導率420W/m・K以上の放熱基板を製造することができるとの報告がある。しかし、添加金属を使用しても焼結が不安定で相対密度が低く、最終のNi系メッキの品質が確保できないという問題があり、また、熱伝導率のバラツキが大きく、熱伝導率が安定して420W/m・K以上にならないという問題等もあるため実用化に至っていない。
本発明は、金属とダイヤモンドの粉末を主成分とする合金複合体の表面に、メッキにより金属層を形成したのち、該金属相及び該合金複合体の融点以下で加熱し加圧する(以下、この加熱及び加圧処理を便宜的に「固相焼結」ともいう。)を行うことで、表層に欠陥の少ない金属層を形成して熱伝導率の向上と安定を図ったものである。ここで、「合金複合体」は塊状に作製されたものを意味する。合金複合体は、例えば、金属とダイヤモンドの混合粉末を型押しすることによって得ることが可能であるが、型押し後に液相焼結を行って高密度の合金複合体を作製することが好ましい。また、溶浸法等、他の方法により合金複合体を作成してもよい。
耐熱性が必要な場合には、主金属としてAg、Cu、またはこれらの合金を用いることが望ましい。大型の放熱基板で軽量化が必要な場合は、主金属としてAlやAl合金を用いることが望ましい。
主金属がAg、Cu、及びこれらの合金のうちのいずれかである場合、添加金属は、例えばTi、Cr、Co、Mn、Ni、Fe、Bを用いることができ、その添加量は合金複合体の全体の1vol%以上5vol%以下とすることが望ましい。添加量が1vol%未満でも5vol%を超えても熱伝導度率が420W/m・K以上にはならない。また、主金属がAlやAl合金の場合、添加金属には、例えばSiを用いることができ、その添加量は合金複合体の全体の5vol%以上15vol%以下とすることが望ましい。添加量が5vol%未満でも15vol%を超えても熱伝導度率が420W/m・K以上にはならない。また1.0vol%Mgを添加することで後述の液相焼結が安定する効果がある。
他に、ダイヤモンド粉末は高価であるため、ダイヤモンド粉末の一部を安価で低線膨張係数のSiC、W、Mo等の粉末で置換しても本発明に放熱基板の特性を満たせば問題ない。
主金属、添加金属、及びダイヤモンドの混合粉末を型押しした後の焼結は、真空、減圧、加圧、非酸化、還元ガス、不活性ガス中で主金属の液相が出現する温度(融点)以上での液相焼結であることが好ましい。液相焼結することでダイヤモンド粒子の表層に添加金属とダイヤモンドが反応して炭化物ができる。更に、炭化物と添加金属と主金属が反応した合金層ができ金属・添加物・ダイヤモンドの粉末を主成分とする合金複合体ができる。
金属層は液相焼結後の合金複合体やその研磨品にメッキを被覆して形成するものであり、Ag、Cu、Ni、あるいはそれらの合金等からなり、厚みが5μm以上200μm以下であれば、合金複合体の全面、上下、半導体デバイスを搭載する部分のみのいずれでも問題はない。特に、やわらかくて熱伝導度率の大きいAgやCuの金属層が好適であり、Niまたはこれらの合金のメッキはAl系ダイヤモンドの大型で寸法の厚い放熱基板に有効である。また金属層として、Ag、Cu、Niまたはこれらの合金を多層にメッキしてもよい。
金属層の厚みが5μm以下では加熱加圧しても放熱基板に必要な欠陥の少ない金属層を全体に設けることが難しい。また200μm以上では金属層が非常に不安定になりやすく、またメッキに係る費用が高くなる。
メッキ後の固相焼結は真空、減圧、加圧、非酸化、不活性ガス、難燃性液体、不燃性液等の雰囲気で行うことができるが、水中法で通電焼結を行うと、ニアネットシェイプで製作することが可能であり、またコスト的にも有利である。金属層及び合金複合体の融点以下、50MPa以上500MPa以下の条件(固相焼結に相当する条件)で加熱及び加圧を行うことにより、合金複合体の表面にメッキされた金属層の欠陥を修復し、更に合金複合体自体の熱伝導率の向上と安定化を図ることができる。その製造はホットプレス(以下HPと略記)、鍛造、通電焼結等により可能である。この固相焼結で金属とダイヤモンドからなる合金複合体の表面にメッキしたAg、Cu、Niや、それらの合金からなる金属層を、Cuの放熱基板の表層のような欠陥の少ない状態にできる。
圧力は50MPa以上とすることが好ましく、それ以下では金属層の十分な修復が難しい。また、500MPa以上では大型装置を用いなければ加圧できないので経済的でなく、また、一般的な治具や電極では破壊してしまうことがある。このため合金複合体や金属層の種類に適した固相焼結の条件(温度や圧力)、治具、及び電極を選択することが重要である。
薄いシートやウエハーの合金複合体では、治具や電極の面粗さが表面に転写されるので、ウォ―タージェット、高出力レーザー、ワイヤカット等で所定の形状に切断して製品化する。さらに高い精度が必要な場合には、金属層を研磨紙やバフで研磨し所定の表面粗さに仕上げ、ウォ―タージェット、高出力レーザー、ワイヤカット等で所定の形状に切断して製品化することも可能である。また、ニアネットシェイプで合金複合体を作製すると形状加工が不要でありコスト的に有利である。
最終のメッキは放熱基板に各種の部材、絶縁板、半導体デバイス等を銀ろう付やハンダ付等で接合することを目的として行われるが、放熱基板に欠陥があると、その影響で最終のNi系メッキに欠陥が発生し、良好な銀ろう付やハンダ付ができないという問題が発生する。Ni系メッキが多層になっても次々と欠陥が転写されていくので問題は解決しない。なお、Ni系メッキとは、NiやNi合金のメッキを意味する。
(線膨張係数の測定)
固相焼結後の25mm×25mm×2~2.5mmの試料(表面に金属層を施した合金複合体)からWEDMやパワーレーザーで10mm×5mm×厚み2~2.5mmの試験片を切り出し、熱膨張係数計(セイコー電子工業社製)でRT(25℃)の線膨張係数の測定を行った。
固相焼結後の25mm×25mm×2~2.5mmの試料(表面に金属層を施した合金複合体)からWEDMやパワーレーザーでφ10mm×厚み2mm~2.5mmの試験片を切り出し、レーザーフラッシュ法の熱伝導度計(アルバック理工製 TC-7000)でRT(25℃)の熱伝導率の測定を行った。
固相焼結後の25mm×25mm×2~2.5mmの試料(表面に金属層を施した合金複合体)を大気中に450℃に30分保持し、その外観を顕微鏡の10倍の倍率で目視観察し、金属層のメッキのフクレがない場合はOKであり、大小にかかわらずフクレが見つかった場合にはNGと判断した。
固相焼結後の25mm×25mmの試料(表面に金属層を施した合金複合体)をバリ取りしバフ研磨した後に、3μmNi-Bメッキした放熱基板に10mm×10mm×0.7mmのSiデバイスの金属電極付を高温SnAgCuハンダ(融点218℃)で接合し、超音波でボイドの面積を調べ5%以下のものを合格(OK)、5%よりも大きいものを不合格(NG)とした。なお、この評価は非常に厳しく、この測定でボイド率5%以下を合格すれば銀ろう付、他のハンダ付け、樹脂付等で問題が起こらない知見がある。
69vol%Ag、1vol%Ti、30vol%の30μmダイヤモンドの粉末を混合し、25mm×25mmの金型を使用して圧力500MPaでプレス型押しした後に、真空中・温度1100℃・60分で液相焼結を行って合金複合体を作製し、その合金複合体に金属層として5μmのAgメッキ処理を施した後、HPで温度400℃、圧力50MPa、30分保持という条件で固相焼結を行い、バリ取り後、フクレテストを行い、その後3μmNi・Bメッキを行い、ハンダ付のボイド品質の評価を行った。
結果を表1に示す。
35vol%Ag、5vol%Cr、60vol%の100μmダイヤモンドの粉末を混合し、25mm×25mmの金型を使用して圧力500MPaでプレス型押しした後に、水素中・温度1200℃・60分で液相焼結を行って合金複合体を作製し、その合金複合体に金属層として50μmのCuメッキ処理を施した後、セラミック治具に合金複合体を入れ通電焼結機で圧力300MPaがかかるように上下電極で加圧し、通電加熱で600℃、5分保持という条件で固相焼結を行い、バリ取り後、フクレテストを行い、その後3μmNi・Bメッキを行い、ハンダ付のボイド品質の評価を行った。
結果を表1に示す。
10vol%Ag、37vol%Cu、及び3vol%Tiと、30vol%の100μmダイヤモンドの粉末並びに20vol%の30μmダイヤモンド粉末を混合し、25mm×25mmの金型を用いて圧力500MPaでプレス型押しした後に、真空中・温度1000℃・60分で液相焼結を行って合金複合体を作製し、その合金複合体に金属層として100μmのCuメッキ処理を施した後、そのメッキ済合金複合体1を図1のセラミック治具4に入れ抵抗溶接機を用いて水中6で上下電極2、3により100MPa加圧しながら通電しつつ温度500℃で2秒保持し、さらにそれを加圧したままで500℃になる通電を3回繰り返すという条件で固相焼結を行い、バリ取り後、フクレテストし、その後3μmNi・Bメッキを行い、ハンダ付のボイド品質の評価を行った。
結果を表1に示す。
29vol%Al、10vol%Si、1vol%Mg 、60vol%の50μmダイヤモンド粉末を混合し、25mm×25mm金型を用いて圧力500MPaでプレス型押しした後に、窒素中・温度600℃・60分で液相焼結を行って合金複合体を作製し、その合金複合体の表層を研削してTiとNiを併せて0.3μm蒸着し、更に金属層として10μmのNiメッキ処理を施した後、HPで真空、温度450℃、圧力100MPa、10分保持という条件で固相焼結を行い、バリ取り後、フクレテストを行い、その後3μmNi・Bメッキを行い、ハンダ付のボイド品質の評価を行った。
結果を表2に示す。
実施例3の放熱基板(熱膨張係数8.3ppm/Kで熱伝導度555W/m・K)にセラミックとコバール等の部材を水素中・温度750℃で銀ろう付けした後、剥離や割れがないことを確認してPKGを作り、それに10mm×10mm×0.7mmのSiデバイスの金属電極を高温AuSn(融点280℃)ハンダを300℃で接合し、超音波でボイド面積が3%以下であることを確認した半導体モジュールを製作し、この半導体モジュールについてヒートサイクルテスト(-40~125℃、3000回)を行った。併せて、比較のために、同寸法の実施例3と同じ熱膨張係数8.3ppm/Kで、熱伝導度200W/m・Kの20wt%CuWの放熱基板で同じPKGを作りデバイスを搭載してヒートサイクルテスト(-40~125℃、3000回)を行った。
結果、いずれの試料も剥離や割れ等の問題は起こらなかった。
これにより将来的な高性能半導体モジュールに対応できる高性能放熱基板の要求を満たすことができる。
なお、本発明は現形態に限定されるものではなく本発明の目的を達成できる範囲での形態は本発明に含まれる。本発明を実施する際の具体的な構造や形態等は本発明の目的を達成できる範囲内で他の構造でもよい。例えば他の製法の金属ダイヤモンドの放熱基板のメッキ品質の確保にも本発明は応用できる。
今回開示された実施形態及び実施例はすべての点で例示であって制限的なものでないと考えられるべきである。上記した説明でなく特許請求範囲によって示される。
2…上下する上電極
3…下電極
4…セラミック治具
5…溶接機電源
6…水
7…ダイヤモンド
8…金属層
9…放熱基板の断面拡大写真
Claims (22)
- 金属とダイヤモンドの粉末を主成分とする合金複合体の表面にメッキ処理を行って金属層を形成し、
前記金属層が形成された前記合金複合体を、該金属層の融点以下かつ該合金複合体の融点以下で加熱及び加圧することにより前記金属層の欠陥を修復する
ことを特徴とする放熱基板の製造方法。 - 前記加熱及び加圧を行った後に、Ni系メッキ処理を行う
ことを特徴とする請求項1に記載の放熱基板の製造方法。 - 前記金属層が、Ag、Cu、Ni、及びこれらの合金のうちの少なくとも1種類からなり、該金属層の厚さが5μm以上200μm以下である
ことを特徴とする請求項1又は2に記載の放熱基板の製造方法。 - 前記金属層を形成する前に、
前記合金複合体を研削又は/及び研磨し、
前記研削又は/及び研磨した前記合金複合体の表面に、Ti、Cr、Au、Pt、及びこれらの合金のうちの少なくとも1種類を蒸着する
ことを特徴とする請求項1から3のいずれかに記載の放熱基板の製造方法。 - 主金属、該主金属と異なる種類の添加金属、及びダイヤモンドの混合粉末を型押し、該型押しした混合粉末を液相焼結して前記合金複合体を作成する
ことを特徴とする請求項1から4のいずれかに記載の放熱基板の製造方法。 - 前記ダイヤモンドの粉末のうちの95%以上が、粒径が10μm以上1000μm以下であるダイヤモンド粉末であり、
前記主金属が、Ag、Cu、Al、及びこれらの合金のうちの少なくとも1種類であり、
前記添加金属が、Ti、Cr、Co、Mn、Ni、Fe、B、Si、Mg、及びZnのうちの少なくとも1種類であり、その添加量が前記合金複合体の全体の1vol%以上15vol%以下である
ことを特徴とする請求項5に記載の放熱基板の製造方法。 - 前記ダイヤモンドの粉末のうちの95%以上が、粒径が10μm以上1000μm以下であるダイヤモンド粉末であり、
前記主金属がAg、Cu、及びこれらの合金のうちの少なくとも1種類であり、
前記添加金属が、Ti、Cr、Co、Mn、Ni、Fe、及びBのうちの少なくとも1種類であり、その添加量が前記合金複合体の全体の1vol%以上5vol%以下である
ことを特徴とする請求項5に記載の放熱基板の製造方法。 - 前記ダイヤモンドの粉末のうちの95%以上が、粒径が10μm以上1000μm以下であるダイヤモンド粉末であり、
前記主金属がAl及びAl合金のうちの少なくとも1種類であり、
前記添加金属がSiであり、その添加量が前記合金複合体の全体の5vol%以上15vol%以下である
ことを特徴とする請求項5に記載の放熱基板の製造方法。 - さらに、1.0vol%のMgが添加されている
ことを特徴とする請求項8に記載の放熱基板の製造方法。 - 真空雰囲気、減圧雰囲気、非酸化雰囲気、還元雰囲気、不活性ガス雰囲気、難燃性液体雰囲気、又は不燃性液体雰囲気において、前記主金属、及び前記主金属と前記添加金属の合金の融点以下の温度、50MPa以上500MPa以下の圧力で前記加熱及び加圧を行う
ことを特徴とする請求項5から9のいずれかに記載の放熱基板の製造方法。 - 水中において、前記主金属、及び前記主金属と前記添加金属の合金の融点以下の温度、50MPa以上500MPa以下の圧力で通電焼結することにより前記加熱及び加圧を行う
ことを特徴とする請求項5から9のいずれかに記載の放熱基板の製造方法。 - 主金属、該主金属と異なる種類の添加金属、及びダイヤモンドの粉末を主成分とする合金複合体と、該合金複合体の表面に形成された金属層を有し、
線膨張係数が6.5ppm/K以上15ppm/K以下であり、熱伝導率が420W/m・K以上であり、前記金属層の表面における欠陥の割合が5%以下である
ことを特徴とする放熱基板。 - 前記金属層の厚さが2μm以上である
ことを特徴とする請求項12に記載の放熱基板。 - 前記主金属が、Ag、Cu、Al、及びこれらの合金のうちの少なくとも1種類であり、
前記添加金属が、Ti、Cr、Co、Mn、Ni、Fe、B、Si、Mg、及びZnのうちの少なくとも1種類であり、その添加量が前記合金複合体の全体の1vol%以上15vol%以下である
ことを特徴とする請求項12又は13に記載の放熱基板。 - 前記主金属がAg、Cu、及びこれらの合金のうちの少なくとも1種類であり、
前記添加金属が、Ti、Cr、Co、Mn、Ni、Fe、及びBのうちの少なくとも1種類であり、その添加量が前記合金複合体の全体の1vol%以上5vol%以下である
ことを特徴とする請求項12又は13に記載の放熱基板。 - 前記主金属がAl及びAl合金のうちの少なくとも1種類であり、
前記添加金属がSiであり、その添加量が前記合金複合体の全体の5vol%以上15vol%以下である
ことを特徴とする請求項12又は13に記載の放熱基板。 - さらに、1.0vol%のMgが添加されている
ことを特徴とする請求項16に記載の放熱基板。 - 前記金属層が、Ag、Cu、Ni、及びこれらの合金のうちの少なくとも1種類からなり、その厚さが2μm以上である
ことを特徴とする請求項12から17のいずれかに記載の放熱基板。 - 前記合金複合体と前記金属層の間に、Ti、Cr、Au、及びPtのうちの少なくとも1種類からなる層が形成されている
ことを特徴とする請求項12から18のうちのいずれかに記載の放熱基板。 - 請求項12から19のいずれかに記載の放熱基板を備えることを特徴とする半導体用パッケージ。
- 請求項12から19のいずれかに記載の放熱基板を備えることを特徴とする半導体用モジュール。
- 前記金属層の表面にNi系メッキ及びハンダ付けが施されており、該ハンダ付けのボイド率が5%以下である
ことを特徴とする請求項21に記載の半導体用モジュール。
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JP2016504238A JP6028987B2 (ja) | 2014-10-09 | 2015-10-08 | 放熱基板及び該放熱基板の製造方法 |
US15/109,486 US10115655B2 (en) | 2014-10-09 | 2015-10-08 | Heat dissipation substrate and method for producing heat dissipation substrate |
EP15848453.5A EP3206227A4 (en) | 2014-10-09 | 2015-10-08 | Heat dissipation substrate and method for manufacturing said heat dissipation substrate |
CN201580054759.0A CN106796927B (zh) | 2014-10-09 | 2015-10-08 | 散热基板及该散热基板的制造方法 |
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EP (1) | EP3206227A4 (ja) |
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US11929294B2 (en) | 2020-09-30 | 2024-03-12 | Nichia Corporation | Composite substrate and method of producing the composite substrate, and semiconductor device comprising the composite substrate |
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CN106796927A (zh) | 2017-05-31 |
US20160336253A1 (en) | 2016-11-17 |
JP2016136549A (ja) | 2016-07-28 |
EP3206227A4 (en) | 2017-10-25 |
JP6028987B2 (ja) | 2016-11-24 |
JPWO2016056637A1 (ja) | 2017-04-27 |
CN106796927B (zh) | 2018-10-12 |
EP3206227A1 (en) | 2017-08-16 |
US10115655B2 (en) | 2018-10-30 |
JP5807935B1 (ja) | 2015-11-10 |
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