WO2013002407A1 - ろう材、ろう材ペースト、セラミックス回路基板、セラミックスマスター回路基板及びパワー半導体モジュール - Google Patents
ろう材、ろう材ペースト、セラミックス回路基板、セラミックスマスター回路基板及びパワー半導体モジュール Download PDFInfo
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- WO2013002407A1 WO2013002407A1 PCT/JP2012/066859 JP2012066859W WO2013002407A1 WO 2013002407 A1 WO2013002407 A1 WO 2013002407A1 JP 2012066859 W JP2012066859 W JP 2012066859W WO 2013002407 A1 WO2013002407 A1 WO 2013002407A1
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- brazing material
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- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
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Definitions
- the present invention relates to a brazing material for joining a ceramic substrate and a metal plate of a ceramic circuit substrate particularly used for a power semiconductor module or the like.
- a power semiconductor module capable of high voltage, large current operation is used as an inverter for an electric vehicle.
- IGBT module high power semiconductor module
- high power and high integration of power semiconductor modules are rapidly advancing, and ceramic substrates and metals against thermal stress at bonding and cooling and heating cycles at the time of use are more than ever on ceramic circuit substrates. Sufficient bonding strength with the plate is required.
- a substrate used for a power semiconductor module a ceramic circuit substrate in which a metal plate such as a copper plate or an aluminum plate is joined to a ceramic substrate made of aluminum nitride or silicon nitride is widely used.
- the ceramic circuit board is formed by bonding a circuit copper plate on which a semiconductor chip or the like is mounted on one surface of the ceramic substrate, and bonding a heat dissipation copper plate on the other surface.
- the above-mentioned copper plate for circuits usually has a circuit pattern which consists of a plurality of copper plates used as a circuit part by giving an etching treatment etc.
- a copper plate is demonstrated to an example as a metal plate, this invention is not limited only when using a copper plate as a metal plate.
- the following means are used. That is, there is a copper direct bonding method (DBC method: Direct Bonding Copper method) in which a copper plate is directly bonded on a ceramic substrate using a eutectic liquid phase such as Cu-Cu 2 O. There is also a refractory metal metallization method in which a refractory metal such as Mo or W is baked on a ceramic substrate to form the refractory metal.
- DBC method Direct Bonding Copper method
- a refractory metal metallization method in which a refractory metal such as Mo or W is baked on a ceramic substrate to form the refractory metal.
- a metal plate is placed on a ceramic substrate coated with a brazing material containing an active metal such as a Group 4A element or a Group 5A element, heated at an appropriate temperature while applying a pressing force, and formed of the brazing material
- an active metal method in which a copper plate is bonded to a ceramic substrate through a brazing material layer.
- the ceramic circuit substrates obtained by the DBC method and the active metal method all have advantages such as a simple structure and a small thermal resistance, and being compatible with a large current type or highly integrated type semiconductor chip.
- a circuit pattern of a circuit copper plate the following means are used. That is, there is a direct mounting method in which a circuit copper plate in which a circuit pattern is formed in advance by pressing or etching is bonded to a ceramic substrate through a brazing material layer. There is also a multistage etching method in which a brazing material layer is formed on almost the entire surface of the ceramic substrate and a copper plate is joined so as to cover it, and then the copper plate and the brazing material layer are etched together to form a circuit pattern.
- a brazing material layer is formed along the shape of the circuit pattern, and a copper plate is placed to cover the brazing material layer, and thereafter the copper plate is etched to form a circuit pattern as in the multistage etching method.
- a method in which the brazing material pattern printing and the etching method are used in combination hereinafter referred to as a pattern printing etching method).
- Patent Document 1 discloses a paste in which a mixed powder of an Ag-Cu-In alloy powder and a Ti powder is mixed with an organic solvent and a resin for the purpose of providing a brazing material having a strong and stable brazing strength and a low melting point.
- a specific composition of the brazing material is described that 30 to 60% of Ag, 20 to 45% of Cu, 20 to 40% of In, and 0.5 to 5% of Ti are preferable.
- the convex portion is an island-shaped Ag-In phase and a Cu-In phase
- the concave portion is a Ti-Cu phase.
- a large number of Ag-In phases and Cu-In phases, which are convex portions, and a large number of Ti-Cu phases, which are concave portions are distributed at the bonding interface between the brazing material layer and the ceramic substrate. It was found that the concave portions became voids, which lowered the bonding strength between the copper plate and the ceramic substrate.
- Patent Document 2 an alloy having an average particle diameter of 15 to 40 ⁇ m, which comprises 55 to 85% by mass of Ag, 5 to 25% by mass of In, 0.2 to 2.0% by mass of Ti, the balance Cu and unavoidable impurities.
- a brazing material is proposed in which 5 to 30% by mass of Ag powder particles having an average particle diameter of 1 to 15 ⁇ m is further added to the powder. This is achieved by adding an appropriate amount of Ag powder particles of an appropriate particle size and particle size distribution to an alloy powder having an Ag-Cu-In-Ti brazing material as a base material, thereby joining the copper plate. It has been found and proposed that the wrinkle-like unevenness formed on the surface of the brazing material layer is alleviated, and the bonding strength can be improved.
- the active metal hydride when the active metal hydride is contained in the alloy powder as in the brazing material proposed by the present inventors in Patent Document 2, it is caused by the decomposition of the active metal hydride due to oxygen etc. contained in the alloy powder. The generated active metal is altered. The modified active metal can no longer contribute to the formation of a compound layer having the function of securing the bondability between the ceramic substrate and the metal plate, and particularly when the content of the active metal hydride is low, the desired bonding strength There was a case that could not be secured. Also, in addition to the content of the active metal hydride in the alloy powder, for example, depending on the combination of each component of the brazing material such as the difference in particle size between the alloy powder and the Ag powder or the addition amount of Ag powder. There was a case where the bonding strength was insufficient.
- the present invention has been made in view of the above problems, and a brazing material using the brazing material and the brazing material in which the amount of In is reduced while maintaining the bonding strength between the ceramic substrate and the metal plate to the level of the prior art.
- the purpose is to provide a paste.
- Another object of the present invention is to provide a ceramic circuit board and a ceramic master circuit board having a metal plate and a ceramic substrate joined with a desired bonding strength by the above-mentioned brazing material.
- another object of the present invention is to provide a power semiconductor module in which the above-mentioned ceramic circuit board having a desired bonding strength is incorporated.
- the present inventors diligently studied to solve the above problems, and basically, (1) 3) Ag—Cu alloy powder, Ag powder, active metal hydride powder in which the amount of addition of In is reduced more than before.
- the brazing material is composed of mixed powder obtained by mixing seed powders, (2) The relationship between the particle sizes of the above three types of powders is set as alloy powder Ag Ag powder> active metal hydride powder, so as to obtain an appropriate particle size distribution When the additive amount of In in the alloy powder is reduced more than before by adjusting the mixed powder, and (3) adjusting the particle size and the addition amount of the active metal hydride powder in the mixed powder within a predetermined range
- One embodiment of the present invention based on this finding is mixing Ag, an active metal hydride powder, an alloy powder consisting of at least Ag: 55 to 80% by mass, In: 1 to 5% by mass, the balance Cu and unavoidable impurities.
- a brazing material for joining a ceramic substrate and a metal plate wherein the composition ratio of Ag to the total amount of Ag and Cu contained in the mixed powder is 0.57 to 0..
- the equivalent circle of the particles of the alloy powder, the Ag powder, and the active metal hydride powder containing 0.5 to 5.0% by mass of an active metal hydride powder having an equivalent circular mean diameter of 10 to 25 ⁇ m.
- the average diameter is in the relation of alloy powder ⁇ active metal hydride powder> Ag powder, and the above mixed powder is based on volume when the particle size distribution is measured according to JIS Z 8825-1.
- the 10% cumulative particle size (d10) is 3 to 10 ⁇ m
- the 50% cumulative particle size (d50) is 10 to 35 ⁇ m
- the 90% cumulative particle size (d90) has a particle size distribution of 30 to 50 ⁇ m.
- the brazing material is characterized in that a peak is present between the 50% cumulative particle size (d50) and the 90% cumulative particle size (d90) in the distribution.
- an active metal compound layer (hereinafter sometimes referred to as a compound layer) produced by the reaction between an element contained in the ceramic substrate and the active metal in the temperature rising process is a brazing material layer. It is uniformly formed on the bonding interface between the ceramic and the ceramic substrate.
- the compound layer is a layer that secures the bonding property between the brazing material layer and the ceramic substrate, that is, the bonding property between the metal plate and the ceramic substrate.
- the brazing material according to the present invention even when In of the alloy powder is reduced by the action of the combination of the configurations of the above (1) to (3), the bonding strength between the ceramic substrate and the metal plate is the same as before. Thus, even when repeated thermal stress due to the thermal cycle is applied to the residual stress to act on the ceramic circuit board, peeling of the metal plate from the ceramic substrate is prevented.
- the composition of the alloy powder is Ag: 55 to 80% by mass, In: 1 to 5% by mass, the balance Cu and unavoidable impurities.
- Ag is less than 55% by mass and more than 80% by mass, the melting point of the alloy powder is high.
- In is less than 1% by mass, the melting point of the alloy powder is high, and when it is more than 5% by mass, the cost of the brazing material is high and wrinkle-like irregularities causing voids are formed on the surface of the brazing material layer. It is easy to be done.
- the brazing material according to the present invention which is a mixed powder formed by mixing three powders of the above alloy powder, Ag powder and active metal hydride powder, has a composition ratio of Ag to the total amount of Ag and Cu contained in the mixed powder.
- Ag / (Ag + Cu) is 0.57 to 0.85.
- this composition ratio is less than 0.57 and exceeds 0.85, the alloy powder, the Ag powder and the active metal hydride powder are heated and melted, and the melting point of the brazing material in the state in which these melts are mixed becomes higher.
- the equivalent circle average diameter of the particles of the above alloy powder, Ag powder and active metal hydride powder is in the relation of alloy powder ⁇ active metal hydride powder> Ag powder, and the mixed powder is JIS Z 8825-1.
- 10% cumulative particle size (d10) is 3 to 10 ⁇ m
- 50% cumulative particle size (d50) is 10 to 35 ⁇ m
- 90% cumulative particle size d90) has a particle size distribution of 30 to 50 ⁇ m
- the presence of a peak between the 50% cumulative particle size (d50) and the 90% cumulative particle size (d90) in the frequency distribution ensures the desired bonding strength It is necessary to
- the brazing material when the brazing material is composed of only the alloy powder and the active metal hydride powder, the voids between the particles of the alloy powder and the active metal hydride powder increase, and the filling properties of the particles of each powder constituting the brazing material Decreases.
- a small diameter Ag powder having a relationship of equivalent circle average diameter of alloy powder ⁇ active metal hydride powder> Ag powder to the brazing material, and setting the particle size distribution of the mixed powder in the above range, FIG. As shown in the figure, the filling properties of the brazing material can be enhanced.
- FIG. 1 shows an alloy powder composed of 65.5 mass% of Ag with d10 of 8.7 ⁇ m, d50 of 24.2 ⁇ m, d90 of 45.5 ⁇ m, In 2 mass%, oxygen content of 0.05% and the balance of Cu. 15 parts by mass of Ag powder with d10 of 2.7 ⁇ m, d50 of 5.6 ⁇ m, d90 of 9.9 ⁇ m, d10 of 10.1 ⁇ m, d50 of 18.7 ⁇ m, d90 of 33.0 ⁇ m with active metal hydride powder It is an electron micrograph of 100 times which shows the form of the brazing material after adding 2 mass parts of certain titanium hydride powders. As shown in FIG.
- the Ag powder fills the voids between the particles of the alloy powder and the active metal hydride powder, and the filling property of the brazing material is improved. As a result, the bonding strength between the ceramic substrate and the metal plate is It can be improved.
- the equivalent circle average diameter of the particles of the alloy powder, Ag powder and active metal hydride powder should be in the relation of alloy powder> active metal hydride powder> Ag powder. Is preferred.
- grains of alloy powder is filled by addition of Ag powder and titanium hydride powder, and it is in the state which the filling property of each particle
- This high filling property works effectively for the relief of wrinkle-like unevenness on the surface of the brazing material layer to be described later and the improvement of the linearity of the outer edge of the printed pattern when the pasted wax is printed.
- the peak be present between the 60% cumulative particle diameter (d60) and the 80% cumulative particle diameter (d80).
- the bulk density of the brazing material configured as described above is 3.6 to 5.5 g / cm 3 .
- the bulk density of the brazing material is less than 3.6 g / cm 3 , the gaps between the alloy powder particles are not sufficiently filled with the Ag powder, and the bonding strength between the ceramic substrate and the metal plate becomes relatively low.
- the distribution of each particle of the brazing material becomes coarse, so it is necessary to bond the metal plate and the ceramic substrate The amount of material may be insufficient.
- (d50 ⁇ d10) / (d90 ⁇ d10) be 0.25 to 0.65.
- (d50 ⁇ d10) / (d90 ⁇ d10) is less than 0.25, the filling property of the brazing material is relatively poor because the number of small particles is small, and the bonding strength is reduced.
- it exceeds 0.65 there are many particles with small particle diameter, and the brazing material heated and melted at the time of joining easily spreads to the surface of the metal plate.
- (d50 ⁇ d10) / 40 (%) is preferably 0.15 to 0.65 ( ⁇ m /%) in order to further improve the filling property of the brazing material.
- the brazing material has a 50% cumulative particle diameter of Ag: 55 to 80% by mass, In: 1 to 5% by mass, an oxygen content of 0.1% by mass or less, the balance Cu and unavoidable impurities (D50) 15 to 40 ⁇ m alloy powder and 5 to 30 parts by mass of 50% cumulative particle diameter (d50) 1 to 15 ⁇ m Ag powder particles relative to 100 parts by mass of the alloy powder, and d10) 0.5 to 5 parts by weight of an active metal hydride powder having a particle size distribution of 5 to 15 ⁇ m, a 50% cumulative particle size (d50) of 10 to 25 ⁇ m, and a 90% cumulative particle size (d90) of 25 to 50 ⁇ m It is preferable to have Hereinafter, the brazing material of such a preferable embodiment will be described for each component thereof.
- the alloy powder contained in the brazing material of the preferred embodiment is basically composed of 55 to 85% by mass of Ag, 1 to 5% by mass of In, the balance Cu and unavoidable impurities, preferably the oxygen content It is 0.1 mass% or less.
- the oxygen content exceeds 0.1% by mass, the active metal produced from the active metal hydride powder which first decomposes in the temperature rising process easily reacts with oxygen to form an oxide, so that it can be used as an active metal. I will not play a role. That is, since the formation of the compound layer necessary for joining the ceramic substrate and the brazing material layer is suppressed, voids are formed at the joining interface, which results in a decrease in the joining strength.
- the oxygen content of each of the Ag powder and the active metal hydride powder is preferably 0.1% by mass or less.
- the ratio Ag / (Ag + Cu) of Ag to the total amount of Ag and Cu contained in the alloy powder is 0.6 to 0.7.
- Ag / (Ag + Cu) is less than 0.6, the melting point of the alloy powder is increased by deviating from the eutectic composition, so that undissolved matter may be generated in the alloy powder and the bonding strength may be reduced.
- it exceeds 0.7 the content of Ag in the brazing filler metal in the heated, melted and mixed state increases, the melting point of the brazing filler metal becomes high, unmelted residue occurs, and the bonding strength decreases. May.
- the alloy powder preferably contains 0.0001 to 0.5 mass% of Si.
- the content of Si is less than 0.0001% by mass, the melting point of the alloy powder is high, so that undissolved matter may be generated in the alloy powder, and the bonding strength may be reduced.
- alloy powders containing less than 0.0001% by mass of Si are very expensive.
- it exceeds 0.5% by mass a brittle Ti—Si phase is likely to be formed in the brazing material layer, which may lower the bonding strength.
- the d50 of the alloy powder produced by gas atomization and obtained by sieving etc. is desirably 15 to 40 ⁇ m.
- the brazing material heated and melted at the time of joining easily spreads to the surface of the metal plate.
- d50 exceeds 40 ⁇ m it is difficult to secure the dimensional accuracy of the printing pattern when the brazing material is made into a paste and screen printing or the like is performed.
- d50 of alloy particles is more preferably 20 to 30 ⁇ m.
- d10 of the alloy powder is 6 to 12 ⁇ m and d90 is 60 ⁇ m or less. If the d10 of the alloy powder is less than 6 ⁇ m, the melting rate will be fast, and the heated and melted brazing material may be excessively wet and spread.
- the preferred alloy powder d10 is 7 to 12 ⁇ m.
- d90 exceeds 60 ⁇ m, the melting speed of the alloy powder is low, and a part of the alloy powder is unmelted, so the bonding strength may be reduced.
- the preferred alloy powder d90 is 55 ⁇ m or less.
- the Ag powder preferably has a d50 of 1 to 15 ⁇ m and is added to the brazing material in the range of 5 to 30 parts by mass with respect to 100 parts by mass of the alloy powder.
- the d50 of the Ag powder When the d50 of the Ag powder is less than 1 ⁇ m, the difference in particle size between the alloy powder and the Ag powder becomes large, the dispersion state of the Ag powder in the brazing material becomes uneven, and the bonding strength between the metal plate and the ceramic plate decreases. There is a case. Moreover, printing unevenness may arise in the printing pattern formed by printing the brazing material made into a paste by screen printing. On the other hand, when the d50 of the Ag powder exceeds 15 ⁇ m, the Ag powder, which is considered to be melted or solid phase diffused due to contact with the alloy powder previously melted in the temperature rising process, causes undissolved matter, and the metal plate and ceramics Bonding strength with the plate may be reduced. It is desirable to add Ag powder having a d50 of 3 to 8 ⁇ m.
- the amount of addition of the Ag powder is less than 5 parts by mass, the effect of relieving wrinkle-like unevenness on the surface of the brazing material layer is low. On the other hand, if it exceeds 30 parts by mass, although there is an effect to suppress wrinkle-like unevenness on the surface of the brazing material layer, the amount of Ag component diffused to the surface of the metal plate increases, so the brazing material gets wet to the surface of the metal plate It may spread.
- the addition amount of Ag powder is preferably in the range of 10 to 25 parts by mass.
- d10 of Ag powder is 0.5 to 3.0 ⁇ m and d90 is 8.0 to 20.0 ⁇ m or less. If the d10 of the Ag powder is less than 0.5 ⁇ m, the melting rate is increased, and the heated and melted brazing material may be excessively wet and spread. On the other hand, when d90 exceeds 20.0 ⁇ m, the melting speed of the Ag powder is low, and a part of the Ag powder is unmelted, which may lower the bonding strength.
- each particle of the Ag powder contained in the brazing material uniformly contacts the solution of the alloy powder which melts earlier than the Ag powder in the temperature raising process. This makes it possible to uniformly dissolve Ag generated by melting or solid phase diffusion of Ag powder in contact with the solution of the alloy powder without segregation in the solution of the alloy powder.
- the active metal hydride powder has a particle size distribution of d50 of 10 to 25 ⁇ m, preferably d10 of 5 to 15 ⁇ m, and d90 of 25 to 50 ⁇ m, in an amount of 0.5 to 5 parts by weight based on 100 parts by weight of the alloy powder In the range, it is preferable to add to the brazing material separately from the alloy powder.
- the dispersed state of the active metal hydride powder becomes uneven, and in the brazing material, a portion where the particles of the powder are unevenly distributed and Will occur. Therefore, in the deficient portion, the active metal hydride is decomposed in the temperature rising process, and the active metal generated is deficient. Then, the element contained in the ceramic substrate reacts with the active metal, and a compound layer formed at the bonding interface between the brazing material layer and the ceramic substrate is not formed in the deficient portion, and a void (void) is generated in the deficient portion.
- junction strength may be reduced due to the formation of
- d10 exceeds 15 ⁇ m
- the particle size distribution may be too sharp
- the filling property of the brazing material may be relatively low
- the bonding strength between the ceramic substrate and the metal plate may be low.
- the particles of the active metal hydride powder When d50 of the active metal hydride powder exceeds 25 ⁇ m or d90 exceeds 50 ⁇ m, the particles of the active metal hydride powder have a distribution of particles in the brazing material because many particles having large particle sizes are contained in the powder. It tends to be coarse, resulting in particles lacking. Therefore, in the same manner as described above, the active metal is insufficient in the deficient portion, and the compound layer is not formed in the deficient portion, and the bonding strength between the ceramic substrate and the metal plate may be reduced. On the other hand, when d90 is less than 25 ⁇ m, the particle size distribution of the Ag powder may be too sharp, the filling property of the brazing material may be relatively low, and the bonding strength between the ceramic substrate and the metal plate may be low.
- the addition amount of the active metal hydride powder is less than 0.5 parts by mass, the compound layer of the active metal may not be sufficiently formed at the bonding interface, and the bonding strength of the ceramic substrate to the metal plate may be reduced.
- the addition amount exceeds 5.0 parts by mass, a brittle Ti-Si phase is formed in the brazing filler metal layer, and the strength of the brazing filler metal layer itself is reduced, which may reduce the bonding strength. is there.
- a more preferable range of the addition amount of the active metal hydride powder is 1.0 to 3.0 parts by mass.
- the active metal hydride hydrides of elements belonging to Group IVa of the periodic table can be used, and generally hydrides of titanium, zirconium and hafnium are used.
- the ceramic substrate is formed of nitride-based ceramics such as aluminum nitride and silicon nitride, or oxide-based ceramics such as alumina and zirconia
- hydride powder of titanium (Ti) as an active metal that is, titanium hydride It is preferable to use a powder.
- Titanium produced by decomposition of titanium hydride at a predetermined temperature has high reactivity with N which is an element contained in nitride ceramics or O which is an element contained in oxide ceramics, and has a brazing material layer
- the bonding strength can be further enhanced by forming a TiN layer or TiO 2 layer which is a compound layer at the bonding interface of the ceramic substrate and the ceramic substrate.
- titanium hydride powder as the active metal hydride powder.
- the titanium hydride is decomposed at a predetermined temperature by heat treatment in the bonding step to release hydrogen to form active titanium metal, which reacts with the element contained in the ceramic substrate to form a ceramic substrate and the like.
- a compound layer is formed at the bonding interface of the brazing material layer.
- the melting point of the alloy powder of the above composition is 750 to 880 ° C.
- the decomposition temperature of the titanium hydride powder is around 600 ° C., and the temperature difference between them is close to about 150 to 280 ° C. .
- titanium hydride powder By decomposing titanium hydride powder in such a manner that titanium hydride powder is decomposed at a temperature lower by 150 to 280 ° C. than the melting temperature of the alloy powder to form titanium metal, deterioration such as oxidation or carbonization of metal titanium before melting start of alloy powder occurs. It is prevented. As a result, the compound layer can be properly formed at the bonding interface between the ceramic substrate and the brazing material layer, and the bonding strength can be further improved.
- the behavior of the brazing material at the time of joining is not necessarily clear when the ceramic substrate and the metal plate are joined using the brazing material according to the present invention described above, it is presumed as follows. That is, in the alloy powder, the Ag powder and the active metal hydride powder contained in the brazing material, first, the active metal hydride powder is decomposed in the temperature raising process of the bonding step to form an active metal, and then the alloy powder is melted. The Ag powder is brought into contact with the solution of the alloy powder, and the Ag melts or diffuses into the solution.
- the brazing material according to the present invention an appropriate amount of In is added to the alloy powder which can suppress the formation of wrinkle-like unevenness on the surface of the brazing material layer, and Ag which further raises the melting point is separately added as Ag powder. ing.
- the melting point of the alloy powder itself is relatively low, close to the temperature at which the active metal hydride powder decomposes.
- the active metal produced by the decomposition of the active metal hydride powder is heated to the subsequent melting point of the alloy powder.
- the opportunity to react with oxygen, carbon, nitrogen, etc. present in the brazing material or in the atmosphere can be reduced, and an appropriate amount of active metal will be present in the brazing material.
- the brazing material (mixed powder) according to the present invention is a mixed powder in which the respective particle sizes of the alloy powder ⁇ active metal hydride powder> Ag powder are mixed, Since the powder has a predetermined particle size distribution, the Ag powder is uniformly disposed in the gaps between the respective particles of the alloy powder. As a result, each particle of the Ag powder uniformly contacts the molten alloy powder solution, and it becomes possible to uniformly dissolve Ag in the alloy powder solution without segregation.
- the active metal diffuses into the solution, the active metal and the element contained in the ceramic substrate react, and a compound layer is formed at the interface between the brazing material in the solution state and the ceramic substrate. Then, the brazing material layer formed through the cooling process adheres to the ceramic substrate with high strength via the above-mentioned compound layer, whereby high bonding strength between the ceramic substrate and the metal plate can be realized.
- the brazing material paste according to another aspect of the present invention is obtained by adding 1 to 10% by mass of a binder and 2 to 20% by mass of a solvent to the above-mentioned brazing material and kneading.
- a dispersant may be added.
- the brazing material paste can be made suitable for screen printing, calendar printing, and the like.
- the binder is less than 1% by mass, the shape retention property of the brazing material paste may be reduced, and the shape accuracy of the print pattern may be reduced.
- the binder exceeds 10% by mass, carbon remains in the brazing material layer formed after the brazing treatment, and a void (void) is formed between the metal plate and the ceramic substrate, and the bonding strength of both May reduce
- a binder is mix
- the solvent contained in the brazing material paste is less than 2% by mass, the flowability of the brazing material paste is lowered, and when printing is performed by screen printing or the like, defects such as blur may occur in the printed pattern.
- the amount of the solvent is more than 20% by mass, the shape retention property of the brazing material paste may be reduced, and the shape accuracy of the print pattern may be reduced.
- the brazing material paste is applied to a thickness of 45 ⁇ m on the surface of the ceramic substrate, heated at 835 ° C. for 1 hour in a vacuum of 5 ⁇ 10 ⁇ 3 Pa or less, and then cooled to form the brazing material.
- the surface roughness Rmax of the layer is 25 ⁇ m or less. That is, when the brazing material according to the present invention is used, the amount of addition of In in the alloy powder is reduced, so that wrinkle-like unevenness formed on the surface of the brazing material is reduced, and as a result, when treated under the above conditions Rmax is 25 ⁇ m or less.
- the formation of the concave portion on the surface is suppressed, so the void ratio of the bonding interface between the metal plate and the ceramic substrate is 5% or less.
- the viscosity of the brazing material paste is preferably 20 to 200 Pa ⁇ s. If the viscosity is less than 20 Pa ⁇ s, the flowability of the paste is excessive, the shape retention of the brazing material paste may be reduced, and the shape accuracy of the print pattern may be reduced. On the other hand, when the viscosity exceeds 200 Pa ⁇ s, the fluidity of the paste is significantly reduced, and when printing is performed by screen printing or the like, defects such as blur may occur in the printed pattern.
- the thickness of the printing pattern formed by printing the brazing material paste is preferably 20 to 80 ⁇ m. If the thickness of the printed pattern is less than 20 ⁇ m, voids may occur because the amount of brazing material necessary for bonding is insufficient. On the other hand, when the thickness exceeds 80 ⁇ m, the amount of the brazing material becomes excessive, and the heated and melted brazing material has a large wet spread, and when the metal plate is a circuit metal plate, the insulation between the circuits is defective. May be
- the brazing material paste is applied to at least one surface of the ceramic substrate and a metal plate is placed on the brazing material paste, and then 5 ⁇ 10 ⁇ 3 Pa It is characterized in that the void ratio of the brazing material layer of the ceramic circuit substrate in which the ceramic substrate and the metal plate are joined is 5% or less by heating at 835 ° C. for 1 hour in the following vacuum and then cooling. There is.
- the ceramic circuit board by using the brazing filler metal according to the present invention in which the amount of addition of In in the alloy powder is reduced, wrinkle-like unevenness formed on the surface of the brazing filler metal is reduced, and voids of the brazing filler metal layer
- the rate is 5% or less, and a ceramic circuit board having a desired bonding strength such as a peel strength of 15 (kN / m) or more, which is a value indicating the bonding strength between the ceramic substrate and the metal substrate, can be configured.
- the bonding temperature between the ceramic substrate and the metal plate of the ceramic circuit substrate is preferably selected from 770 to 880 ° C. If the bonding temperature is less than 770 ° C., the brazing material may be insufficiently melted, and a void may be formed between the metal plate and the ceramic substrate. On the other hand, if the bonding temperature exceeds 880 ° C., the heated and melted brazing material may have a large wet spread, and if the metal plate is a circuit metal plate, insulation between circuits may be poor. A more preferable bonding temperature is 790 to 850.degree.
- the atmosphere for bonding the two is a non-oxidizing atmosphere, such as in vacuum or argon. Bonding is performed in an inert gas. In the case of a vacuum atmosphere, bonding is performed by heat treatment in a vacuum of 1 Pa or less for 0.3 to 3 hours.
- the pressure is higher than 1 Pa and the amount of oxygen in the atmosphere is large, the active metal formed from the active metal hydride powder that decomposes first in the temperature raising process easily reacts with oxygen to form an oxide. It does not play a role as metal.
- a void remains in the joining interface to cause a decrease in the joining strength. More preferably, it is 0.1 Pa or less.
- the heat treatment time at the time of bonding of the ceramic substrate and the metal plate is 0.3 to 3 hours. If the heat treatment time is shorter than 0.3 hours, the brazing material may be insufficiently melted and a void may be formed between the metal plate and the ceramic substrate. On the other hand, when the heat treatment time exceeds 3 hours, the heated and melted brazing material is excessively wet and spread, and when the metal plate is a circuit metal plate, the insulation between the circuits may be poor. A more preferable heat treatment time is 0.5 to 1.5 hours.
- the metal plate and the ceramic substrate reliably contact the brazing material, and the bonding strength between the metal plate and the ceramic substrate can be improved.
- the load applied to the ceramic substrate and the metal plate is preferably a load of 10 to 100 g / cm 2 per area of the brazing material (brazing material paste) interposed therebetween.
- the brazing material paste is applied to at least one surface of the ceramic substrate, and a metal plate is placed on the brazing material paste, and then 5 ⁇ 10 ⁇ 3
- a ceramic master circuit board capable of collecting a plurality of ceramic circuit boards in which the ceramic board and the metal plate are joined by heating at 835 ° C. for 1 hour in a vacuum of at most Pa and then cooling.
- the void fraction of the brazing material layer of the ceramic circuit board collected from the ceramic master circuit board is 5% or less, and the void fraction of the brazing material layer formed within 10 mm from the end face of the ceramic master circuit board is 5% to It is a ceramic master circuit board which is 50%.
- the ceramic master circuit board is a basic size in the manufacturing process of the ceramic circuit board. That is, the ceramic master circuit board is a large-sized board 10 capable of collecting a plurality of (the nine in the case of FIG. 4) ceramic circuit board 1 shown in FIG. 3 as shown in FIG.
- the rectangular ceramic master circuit board 10 is within 10 mm from the end face of the ceramic master circuit board around the product part 6 which is a central region where a plurality of ceramic circuit boards 1 which are products are formed, and the product part 6. It has an end 5 formed.
- the method of manufacturing the ceramic master circuit board is basically the same as the method of manufacturing the ceramic circuit board.
- a large ceramic substrate 20 and a metal plate capable of forming a plurality of ceramic circuit substrates are prepared.
- the above-described brazing material paste is printed in the region corresponding to the product portion 6 of the ceramic substrate 20 to form a plurality of sets of product patterns corresponding to the circuit pattern shapes 4a to 4c of the circuit metal plate 4e.
- a brazing material is also printed on the end 5 of the ceramic substrate 20 to form a plurality of sets of end patterns corresponding to the shape of the end metal plate 5a.
- a large metal plate is placed on the ceramic substrate 20 while being positioned in the horizontal direction so as to be in contact with the product pattern and the end pattern printed on the ceramic substrate 20, and the metal is applied to the ceramic substrate under the above heat treatment conditions. Join the plates.
- the metal plate bonded to the ceramic substrate 20 is patterned by etching, and as shown in FIG. 4, a plurality of sets of circuit metal plates 4 e in the product portion 6 and a plurality of end metal plates 5 a in the end portion 5.
- the formed ceramic master circuit board 10 is formed.
- break grooves B corresponding to the size of the outer edge of the ceramic circuit board 1 to be collected are formed in the vertical and horizontal directions. Each of the ceramic circuit boards 1 can be collected.
- the end metal plate 5 a formed at the end 5 of the ceramic master circuit board 10 is bonded to the brazing material layer 7 a which is bonded to the ceramic substrate 2.
- Voids voids
- the void ratio is 5 to 50%.
- the voids contained in the brazing material layers 3a to 3c joining the circuit metal plates 4e (4a to 4c) of the ceramic circuit board 1 formed in the product portion 6 to the ceramic substrate 2 are suppressed, and the ceramic master
- the void ratio of each of the brazing material layers 3a to 3c of the ceramic circuit board 1 collected from the circuit board 10 is 5% or less.
- a power semiconductor comprising a semiconductor chip mounted on a circuit metal plate joined to one surface of the ceramic circuit substrate and a heat dissipation metal plate joined to the other surface of the ceramic substrate. It is a module ceramic. According to such a power semiconductor module, the bonding stability of the circuit metal plate and the ceramic substrate, and the heat radiation metal plate and the ceramic substrate can be maintained, so that a power semiconductor module excellent in mounting reliability with respect to cooling and heating cycles can be provided.
- the bonding strength between the ceramic substrate and the metal plate can be improved.
- the brazing material of the present invention is a mixture of at least Ag: 55 to 80% by mass, In: 1 to 5% by mass, alloy powder consisting of balance Cu and unavoidable impurities, Ag powder and active metal hydride powder.
- an active metal hydride powder having an equivalent circular mean diameter of particles of 10 to 25 .mu.m, and an equivalent of particles of the alloy powder, Ag powder and active metal hydride powder
- the circle average diameter is in the relation of alloy powder ⁇ active metal hydride powder> Ag powder, and the above mixed powder is based on volume when the particle size distribution is measured according to JIS Z 8825-1.
- the 10% cumulative particle size (d10) is 3 to 10 ⁇ m
- the 50% cumulative particle size (d50) is 10 to 35 ⁇ m
- the 90% cumulative particle size (d90) has a particle size distribution of 30 to 50 ⁇ m.
- the brazing material is characterized in that a peak is present between the 50% cumulative particle size (d50) and the 90% cumulative particle size (d90) in the distribution.
- the brazing material has a 50% cumulative particle diameter (d50) composed of Ag: 55 to 80% by mass, In: 1 to 5% by mass, an oxygen content of 0.1% by mass or less, the balance Cu and unavoidable impurities ) 5 to 30 parts by mass of 50% cumulative particle diameter (d50) and 1 to 15 ⁇ m of Ag powder particles with respect to 100 parts by mass of the alloy powder of 15 to 40 ⁇ m, and 10% accumulated particle diameter (d10) Mixed with 0.5 to 5 parts by mass of active metal hydride powder having a particle size distribution of 5 to 15 ⁇ m, 50% cumulative particle size (d50) of 10 to 25 ⁇ m, and 90% cumulative particle size (d90) of 25 to 50 ⁇ m Can be obtained preferably.
- d50 50% cumulative particle diameter
- the powder is sprayed such that d50 becomes the target particle diameter by gas atomization, and the powder having the target particle diameter or more is cut by sieving, and a powder having the target particle diameter is used.
- Ag powder and activated metal hydride powder can be obtained.
- the brazing material is a mixed powder of an alloy powder, an Ag powder and an active metal hydride powder.
- Each powder can be mixed using a stirrer such as a ball mill or an attritor to obtain a powdery mixed powder composed only of metal particles.
- a stirrer such as a ball mill or an attritor to obtain a powdery mixed powder composed only of metal particles.
- an organic solvent and a binder may be added to each powder, and mixing may be performed using a ball mill, a planetary mixer, a three-roll mill, or the like to obtain a pasted brazing material (brazing material paste).
- methyl cellosolve, ethyl cellosolve, isophorone, toluene, ethyl acetate, terpineol, diethylene glycol monobutyl ether, texanol etc. is used as an organic solvent, and acrylic resin such as polyisobutyl methacrylate etc. as a binder It is preferable to use high molecular compounds such as ethyl cellulose and methyl cellulose.
- Ceramics constituting a ceramic substrate which is a sintered body include aluminum oxide (alumina: Al 2 O 3 ), zirconium oxide (zirconia: ZrO 2 ) and other oxide ceramics, aluminum nitride (AlN), silicon nitride Various ceramics such as Si 3 N 4 ), titanium nitride (TiN) and other nitride ceramics, silicon carbide (SiC), titanium carbide (TiC) and other carbide ceramics, other boride ceramics etc. It can be suitably used according to the conditions of use.
- the ceramic substrate constituting the ceramic circuit substrate used for a power semiconductor module (IGBT module) or the like to which a high voltage and a large current is loaded is aluminum nitride or silicon nitride having high thermal conductivity, particularly high in strength and broken. It is desirable to be made of silicon nitride excellent in toughness and thermal conductivity.
- a ceramic substrate with silicon nitride form the ceramic substrate with silicon nitride having a thickness of 0.1 to 1.0 mm and a thermal conductivity of 50 W / m ⁇ K, preferably 70 W / m ⁇ K or more. Is preferred.
- the metal plate to be joined to the ceramic substrate is not particularly limited as long as it can be joined by the brazing material and the melting point of the metal plate is higher than the melting point of the brazing material.
- copper, copper alloy, aluminum, aluminum alloy, silver, silver alloy, nickel, nickel alloy, nickel plated nickel, nickel plated tungsten, nickel plated iron alloy, etc. should be used.
- Aluminum is inferior to copper in electrical resistance and high thermal conductivity (low thermal resistance), it is preferable in that it has mounting reliability with respect to cooling and heating cycles by using the plastic deformability possessed by aluminum. .
- Silver can be used if emphasis is placed on electrical resistance.
- the thermal stress at the time of bonding can be reduced because their coefficient of thermal expansion is close to that of aluminum nitride or silicon nitride. It is preferable because it can be done.
- a metal plate mainly made of copper, such as copper or copper alloy from the viewpoint of electrical resistance and stretchability, high thermal conductivity (low thermal resistance), and little migration.
- FIG. 2 is a cross-sectional view taken along the line AA of FIG. 3 (a).
- FIG. 3A which is a plan view of the ceramic circuit board
- FIG. 3B which is a bottom view, hatching is applied to the circuit metal plates 4e (4a to 4c) and the heat radiation metal plate 4d for understanding. (The same applies to Figs. 4 and 5).
- the ceramic circuit board 1 has a circuit metal plate 4e consisting of three metal plates 4a to 4c constituting a circuit pattern disposed on the upper surface (one surface) of the ceramic substrate 2, and a lower surface It has the metal plate 4d for thermal radiation arrange
- the metal plates 4a to 4c of the circuit metal plate 4e are joined to the upper surface of the ceramic substrate 2 via the brazing material layers 3a to 3c, respectively, and the heat dissipation metal plate 4d is the ceramic substrate via the brazing material layer 3d. It is joined to the lower surface of 2.
- each of the brazing material layers 3a to 3d is formed by solidification after the brazing material passes through the heat treatment in the bonding step.
- the method for manufacturing the ceramic circuit board 1 will be described with reference to FIG.
- the following manufacturing method is an example in the case of manufacturing the ceramic circuit board 1 using the ceramic master circuit board described with reference to FIG. 4, even in the case of manufacturing the ceramic circuit board 1 individually, Basically, it can be manufactured as well.
- the circuit pattern of the metal plate 4e for circuits is formed using the pattern printing etching method in the following manufacturing method, it can also be formed using a direct mounting method or a multistage etching method.
- the steps related to the circuit metal plate 4e and the heat radiation metal plate 4d are the same except for the etching step for forming the circuit pattern, so only the steps related to the circuit metal plate 4e will be described. The description of the steps related to 4d will be omitted as appropriate.
- the process of applying the brazing material paste will be described with reference to FIG. 5 (a).
- coating methods such as screen printing method, metal mask printing method, roll coating method, spraying, transfer and the like There is.
- the paste-form brazing material may be applied to the ceramic substrate 20 by screen printing or the like. It is customary.
- the brazing material paste When printing (applying) the brazing material paste by screen printing, the brazing material paste is printed on the upper surface of the ceramic substrate 20 with a screen having an appropriate mesh (opening), and the circuit pattern of the circuit metal plate A plurality of product patterns 8a to 8c corresponding to the shape (9 sets in the case of the drawing) product portion 6 and a plurality of end patterns 9a corresponding to the shape of the end metal plate (12 in the case of the drawing) ) Form at the end 5.
- the end pattern 9 a is similarly formed on the lower surface of the ceramic substrate 20.
- the average thickness of the product patterns 8a to 8c and the end pattern 9a can be made 20 to 80 ⁇ m.
- the dimensions of the product patterns 8a to 8c and the end patterns 9a may be smaller than the dimensions of the circuit patterns in consideration of the wetting and spreading of the brazing material at the time of joining.
- degreasing process performed after the brazing material paste application process will be described.
- degreasing is performed to remove the binder components contained in the product patterns 8a to 8c and the end pattern 9a.
- the conditions such as the heating temperature and heating time in the degreasing step vary depending on the binder component, but the degreasing atmosphere is oxidized in the non-oxidizing atmosphere of the inert gas or vacuum atmosphere to oxidize the active metal hydride powder. It is preferable without Even in an oxidizing atmosphere, it is preferable that the active metal hydride powder is not oxidized more than necessary by limiting the amount of oxygen. That is, degreasing may be performed in a low oxygen concentration atmosphere or a wet atmosphere.
- the wet atmosphere is an atmosphere formed by supplying a non-oxidizing atmosphere gas in water or hot water and then supplying the gas to the treatment chamber.
- the amount of oxygen contained in the brazing material after the degreasing treatment is preferably 0.3% by mass or less.
- the degreasing process can be performed at a predetermined temperature prior to the bonding process.
- the degreasing treatment can be performed simultaneously in the bonding process without separately providing This is preferable because the bonding strength between the ceramic substrate and the metal plate is further improved without the ashed carbon remaining substantially in the brazing material layer.
- the degreasing treatment was simultaneously performed in the bonding step.
- a large plate-like metal plate to be a circuit metal plate is formed on the product patterns 8a to 8c and the end pattern 9a formed by applying the brazing material paste in the application step.
- the metal plate 40 is placed on the upper surface of the ceramic substrate 20 so that the contact 10 is in contact.
- the metal plate 40 is positioned at a predetermined position with respect to the ceramic substrate 20 in the horizontal direction, and the metal plate 10 covers all of the product patterns 8a to 8c and the end pattern 9a formed on the upper surface of the ceramic substrate 20.
- the metal plate 40 is aligned.
- a metal plate serving as a heat radiation copper plate is similarly positioned and mounted on the lower surface of the ceramic substrate 20, and in a state where they are stacked, the metal plate is fixed and held by an appropriate jig or the like.
- the two metal plates and the ceramic substrate 20 placed on the upper and lower surfaces of the ceramic substrate 20 are heat-treated in a predetermined atmosphere, at a predetermined temperature, and for a predetermined time, and then cooled.
- the metal plate 10 is joined to the upper surface of the ceramic substrate 20 via the brazing material layers 3a to 3c formed by solidification of the product patterns 8a to 8c and the brazing material layer 5a formed by solidification of the end pattern 9a.
- the brazing material heated and melted in the bonding step sufficiently spreads on the ceramic substrate 20 and the metal plate 10 existing in the region to be the ceramic circuit substrate 10 to ensure sufficient bonding strength and the thermal expansion coefficients of both.
- the heating temperature is desirably set to 770 to 880 ° C. in order to suppress the decrease in the thermal cycle resistance due to the residual stress caused by the difference in
- the bonding atmosphere is preferably processed in a non-oxidizing atmosphere, particularly in a vacuum atmosphere, more preferably in a vacuum of 1 Pa or less Desirably, bonding is preferably performed in a vacuum of 0.1 Pa or less.
- the ceramic substrate 20 and the metal plate are adhered to each other by applying an appropriate load to the ceramic substrate 20 in a laminated state and the metal plate disposed on the upper and lower surfaces thereof, so that a good bonding state Can be obtained.
- the load to be applied is preferably 10 to 100 g / cm 2 per area of the brazing material (brazing material paste) interposed between the ceramic substrate 20 and the metal plates disposed above and below it.
- the resist film formed on the upper surface of the metal plate 10 in a pattern corresponding to the shapes of the circuit metal plate 4e and the end metal plate 5a in the etching step may use either a thermosetting or UV curing resist. . Also, either an ink type or a film type may be used.
- the former can form a resist film of a desired pattern using a screen printing method, and the latter can be attached to the surface of the metal plate 10, and then a resist film of a desired pattern can be formed by exposure and development. After a resist film is formed on the upper surface of the metal plate 10, unnecessary portions of the metal plate are etched away by an etching solution.
- the circuit metal plate is a metal plate mainly composed of copper
- the ceramic master circuit board 10 on which the plurality of ceramic circuit boards 1 having the circuit metal plate 4e and the plurality of end metal plates 5a are formed. Is formed. Thereafter, the ceramic master circuit board 10 is folded in advance along the size of the outer edge of the ceramic circuit board 1 along the size of the outer edge of the ceramic circuit board 1 and the ceramic circuit board 1 formed in the product portion 6 is separated. The individual ceramic circuit boards 1 can be obtained by singulating them.
- a brazing material removal step may be provided in which a brazing material removal solution containing hydrogen and ammonium acid fluoride is used.
- a foreign matter removing step may be provided in which foreign matter such as carbon adhering to the surface of the circuit metal plate 4e or the ceramic substrate 20 is removed by a cleaning agent containing an oxidizing agent.
- Example of experiment The present invention will be specifically described based on Experimental Examples 1 to 3.
- the dimensions shown in FIG. 4 having the end portion 5 formed within 10 mm from the outer peripheral end are capable of forming nine pieces of the ceramic circuit board 1 having the dimensions shown in FIG.
- the ceramic master circuit board 10 of FIG. Silicon nitride, aluminum nitride and alumina were used as the ceramic substrate 2 (20), and the thickness was 0.32 mm.
- the bending strength of the ceramic substrate made of silicon nitride is 700MPa, the fracture toughness value is 6.5MPa 1/2 , the bending strength of the ceramic substrate made of aluminum nitride is 350MPa, the fracture toughness value is 3.5MPa 1/2 , and alumina
- the bending strength of the resulting ceramic substrate was 350 MPa, and the fracture toughness value was 4.0 MPa 1/2 .
- the metal plate for forming the circuit metal plate 4e and the heat radiation metal plate 4d was a copper substrate (oxygen-free copper JIS H3100 C1020H), and had thicknesses of 0.5 mm and 0.4 mm, respectively.
- the amounts added of the binder, the solvent and the like contained in the brazing material paste and the kneading conditions were the same as in Experimental Examples 2 and 3. Also, the particle size distribution etc. of the brazing material of each experiment number which is a mixed powder of alloy powder, Ag powder and active metal hydride powder are confirmed in Table 3 in the state of mixed powder, alloy powder, Ag powder and active metal hydride The equivalent circle mean diameter of powder particles and the addition amount of active metal hydride powder are shown in Table 4 for each experiment number.
- component analysis is performed on Cu, Ag, Ti, Hf, and Zr in the 0.5 ⁇ 0.5 mm field of view selected based on the positioning marks formed on the surface of the sample table, and the distribution of each element is mapped
- the particles containing Ag and Cu are specified as alloy particles, the particles containing Ag as Ag powder, and the particles containing Ti, Hf or Zr as an active metal hydride powder did.
- SEM scanning electron microscope
- Addition amount of active metal hydride The addition amount (% by mass) of the active metal hydride contained in the brazing material is analyzed in the brazing material by analyzing with a high frequency plasma emission analyzer (IRIS ADVANTAGE manufactured by Thermo Jarrel Ash). The content of Ti was measured, and the value of Ti obtained based on the chemical formula weight was calculated by multiplying it by 1.0426.
- IRIS ADVANTAGE manufactured by Thermo Jarrel Ash
- the brazing material paste is formed on a large ceramic substrate made of silicon nitride, alumina or aluminum nitride having dimensions of 130 mm long ⁇ 90 mm wide ⁇ 0.32 mm thick and has a mesh size of 150 Printed by screen printing using a screen mask, the product patterns 8a to 8c and the end pattern 9a shown in FIG. 5A are formed on the upper surface (one surface), and the lower surface (the other surface) is formed.
- a pattern for joining a heat radiation metal plate (not shown) was formed.
- the thickness of each pattern is 45 ⁇ m, and the dimension in the planar direction is 0.2 mm smaller than the dimensions of the circuit metal plate 4 e and the heat dissipation metal plate 4 d shown in FIG. 4.
- the ceramic substrate 20 coated with the brazing material paste was heated at a temperature of 120 ° C. in the air for 30 minutes to remove the solvent contained in the brazing material paste.
- the large metal plate 40 serving as a circuit metal plate is not provided on the upper surface side of the ceramic substrate 20 and the heat dissipation metal plate is provided on the lower surface side.
- a large metal plate is stacked on the ceramic 20, and heat treatment is performed while controlling the inside of the bonding furnace so as to obtain a temperature pattern TA indicated by a solid line and a pressure pattern PA indicated by a broken line in FIG. It joined.
- the temperature holding area T1 appearing first is a temperature area in which the degreasing treatment for removing the binder contained in the brazing material is performed, and is held at a temperature of 380 ° C. for 12 hours.
- the temperature holding zone T1 where degreasing treatment is performed the temperature is raised at a temperature rising rate of 10 ° C./min (temperature rising portion T2), and thereafter, at a temperature of 580 ° C. which is equal to or less It held (temperature holding area T3).
- zone I of temperature holding area T3 controlled the joining furnace so that the pressure in a furnace might be 1 Pa or less.
- the temperature holding area T3 is a temperature area provided such that the pressure in the furnace in the temperature holding area T5 described below is 5 ⁇ 10 -3 Pa by lowering the pressure in the furnace at the end of the temperature holding area T3. .
- the temperature holding area T3 is not necessarily required.
- the temperature distribution in the furnace becomes uniform, and the variation due to the position of the decomposition state of the active metal hydride powder in the temperature raising portion T4 thereafter can be prevented.
- the temperature holding area T3 After the temperature holding area T3, the temperature is raised at a temperature rising rate of 10 ° C./min (temperature rising portion T4), and thereafter held at a temperature of 835 ° C. for 1 hour (temperature holding area T5). It cooled by the minute (cooling area T6), and obtained the joined object by which the metal plate was joined to the upper and lower surfaces of ceramic substrate 20. As shown in the pressure pattern PA, the bonding furnace was controlled such that the pressure in the furnace became 5 ⁇ 10 ⁇ 3 Pa or less for the time zone J of the temperature holding area T 5.
- the circuit metal plate 4e (metal plates 4a to 4c shown in FIG. 5C) is formed on the surface of a large metal plate serving as a circuit metal plate disposed on the upper surface side in the obtained bonded body. And a resist film of a pattern corresponding to the end metal plate 5a, and a resist film of a pattern corresponding to the heat radiation metal plate was formed on the surface of a large metal plate serving as a heat radiation metal plate disposed on the lower surface side. Thereafter, an etchant, ferric chloride (FeCl 3), is sprayed onto the metal plate to remove unnecessary portions of the metal plate, and nine sets of circuit metal plates 4e and a plurality of end portions are formed on the upper surface side of the ceramic substrate 20. A ceramic master circuit board was obtained in which the metal plate 5a was arranged on the lower surface side with nine sets of heat radiation method metal plates (not shown).
- Table 5 shows various characteristics of the brazing material of each experimental number obtained in the above-mentioned Experimental Example 1, the ceramic circuit board, and the test piece.
- the various characteristics of the ceramic circuit board of Experimental example 1 shown in Table 5 and a test piece were confirmed as follows. The same confirmation was also made in Experimental Examples 2 and 3 described below.
- the surface roughness of the brazing material layer was determined as follows. A ceramic substrate having the same composition as the ceramic substrate constituting the ceramic circuit substrate of each experiment number, and having dimensions of 50 ⁇ 30 mm in length and width was prepared. On the surface of the ceramic substrate, the same brazing paste as the one used in each experimental example was applied so as to have vertical and horizontal dimensions of 40 ⁇ 20 mm and a thickness of 45 ⁇ m. Then, the ceramic substrate to which the brazing material paste was applied was subjected to heat treatment under the same conditions as the temperature pattern and pressure pattern described with reference to FIG. 8, and the brazing material layer was formed in a state exposed on the surface of the ceramic substrate. Test pieces were prepared. Then, the surface roughness (Rmax) of the formed brazing filler metal layer was confirmed with a surface roughness measuring device (Surfcom 130A, manufactured by Tokyo Seimitsu Co., Ltd.) in accordance with JIS B0601.
- the bonding strength between the ceramic substrate and the metal plate was confirmed by the following peel strength test.
- a ceramic substrate and a metal plate 41 having the same composition as the ceramic substrate and the metal plate constituting the ceramic circuit substrate of each experimental example were prepared. Then, as shown in FIG. 7, the same brazing material paste as used in each experimental example is applied to the upper surface of the ceramic substrate 21 with a size of 20 ⁇ 2 mm, and the metal plate 41 is applied to the side surface of the ceramic substrate 21. The metal plate 41 was superimposed on the ceramic substrate 21 via the brazing material paste so that one end portion was protruded by 5 mm.
- the void ratio contained in the brazing filler metal layers 3a to 3c formed in the product portion 6 of the ceramic master circuit board 10 shown in FIG. 4 and the brazing filler metal layer 7a formed in the end portion 5 was determined as follows. First, the ceramic master circuit board 10 is immersed in a solvent, and all the brazing material layers 3a to 3d, the edges of the upper and lower surfaces of the product portion 6 are treated with an ultrasonic flaw detector (Mi-scope made by Hitachi Construction Machinery, frequency: 50 MHz). The area of the void of all the brazing filler metal layers 7a on the upper and lower surfaces of the portion 5 was measured.
- the void ratio of the product portion 6 (that is, the ceramic circuit board) is obtained by dividing the value obtained by adding the areas of the voids confirmed in all the brazing material layers 3a to 3d by the area of all the brazing material layers 3a to 3d. Calculated. Further, the void fraction of the end portion 5 was calculated by dividing the value obtained by adding the areas of the voids confirmed in all the brazing material layers 7a by the area of all the brazing material layers 7a.
- the insulation test failure rate, the circuit pattern size failure rate and the thermal cycle test failure rate of the ceramic circuit board were confirmed as follows.
- 22 ceramic master circuit boards capable of collecting 9 ceramic circuit boards were prepared for each experiment number, and the obtained 198 ceramic circuit boards were subjected to the inter-circuit insulation test, the circuit pattern size inspection described below and A thermal cycle test was conducted, and the rate of failure was regarded as a failure rate.
- (1) Inter-Circuit Insulation Test In the inter-circuit insulation test, as shown in FIG.
- the metal plates 4a to 4 constituting the circuit pattern of the circuit metal plate 4e formed on the upper surface of the ceramic circuit board 1
- the electrode terminals are brought into contact with predetermined measurement points C to H for three sets of metal plates 4a, 4b, 4a, 4c and 4b, 4c facing each other through gaps 4f, 4g among 4c, and the DC 1000 V is applied.
- This is a test to confirm that the resistance value when applied for 30 seconds is 1 G ⁇ or more.
- the electrode terminals were brought into contact with the measurement points C and D, and the insulation resistance between C and D was confirmed.
- thermal cycle test one cycle of heating / cooling cycle with cooling at -55 ° C for 30 minutes and heating at 160 ° C for 30 minutes is repeated 1000 times to make a ceramic circuit It was determined to be defective when it was added to the substrate and part of the circuit metal plate or the heat dissipation metal plate was peeled off from the ceramic substrate.
- the peel strength (bonding strength) between the ceramic substrate and the metal plate in the formed test piece is 15 kN / m or more, and the ceramic master circuit board
- the failure rate of the thermal cycle test of the ceramic circuit board taken from the sample also became 5% or less.
- the wetting and spreading of the brazing material heated and melted at the time of joining is appropriate, the defective rate of insulation test between circuits of the ceramic circuit board and the defective rate of circuit pattern size also become 5% or less.
- Experiment No. 27 shows that the composition ratio of Ag to the total amount of Ag and Cu contained in the mixed powder is Ag / (Ag + Cu) It is 0.91 and the melting temperature of brazing material is high and melting residue occurs, so the peel strength is low, and the wetting and spreading of the brazing material is also excessive, and the thermal cycle test failure rate, inter-circuit insulation test failure rate and circuit pattern size failure rate Both were high.
- Experiment No. 31 which is the configuration of the brazing material of Patent Document 1
- the content of In of the alloy powder is large, and metallic titanium powder is added to the alloy powder, so the surface roughness (Rmax) of the brazing material layer is It was rough and the void fraction in the product part was high, the peel strength was low, and the thermal cycle test failure rate was high.
- Experiment No. 32 which is the configuration of the brazing filler metal of Patent Document 2
- the content of Ti is low although the content of In in the alloy powder is large, and the particle diameter of Ag powder is smaller than the particle diameter of the alloy powder. Although the size is improved, the surface roughness (Rmax) of the brazing material layer is rough due to the small size, the peel strength is low, and the rate of failure of the thermal cycle test is high.
- the addition amount of the active metal hydride powder in the mixed powder is 0.25 to 5.50% by mass. It is confirmed that the effects of the present invention can be exhibited.
- the mixed powder containing the active metal hydride powder having the addition amount in the above range is preferably formed by adding 0.3 to 6 parts by mass of the active metal hydride powder to 100 parts by mass of the alloy powder. it can.
- the desirable range of the addition amount of the active metal hydride powder in the mixed powder is 0.40 to 4.50% by mass, more preferably 0.90 to 2.70% by mass.
- the particle size distribution of the mixed powder is hardly affected even when the level of the addition amount is changed in the above range because the proportion of the active metal hydride powder in the brazing material is low. It was done.
- the addition amount of Ag powder is 3.0 to 33.0 parts by mass with respect to 100 parts by mass of alloy powder, the effect of the present invention can be exhibited, and the preferable addition amount is It was confirmed that the content is 5.0 to 30.0 parts by mass, more preferably 10.0 to 25.0 parts by mass.
- the experiment numbers 23-26 titanium hydride as the active metal (TiH 2) powder using hafnium hydride (HfH 2) and zirconium hydride (ZrH 2) Other than alumina as the ceramic substrate other than silicon nitride
- TiH 2 titanium hydride as the active metal
- HfH 2 hafnium hydride
- ZrH 2 zirconium hydride
- a ceramic circuit substrate having a ceramic substrate formed of alumina and aluminum nitride has a low flexural strength and fracture toughness of the ceramic substrate, so the ceramic substrate itself is cracked in the thermal cycle test and the thermal cycle test failure rate is high.
- the test piece for confirming the surface roughness of the above-mentioned brazing material layer and the peel strength are confirmed on the surface of the ceramic substrate made of silicon nitride.
- the test pieces were manufactured according to the method of manufacturing the test pieces. The result of having observed the surface of the brazing material layer formed in the test piece which confirms the surface roughness of a brazing material layer is shown in FIG.
- FIG. 6 (a) is a 20 ⁇ stereomicrograph showing the condition of the surface of the brazing material layer formed using the brazing material according to the present invention.
- the particle size distribution of each of the alloy powder comprising Ag 65.5 mass%, In 2 mass%, oxygen content 0.05%, balance Cu and unavoidable impurities, Ag powder and titanium hydride (active metal hydride) powder is as follows: 15 parts by mass of Ag powder and 2 parts by mass of titanium hydride powder were added to 100 parts by mass of the alloy powder.
- FIG. 6 (b) is a 20 ⁇ stereomicrograph showing the condition of the surface of the brazing material layer formed using the brazing material based on the conventional example described in Patent Document 1.
- the specifications of each of the alloy powder and titanium powder of the used brazing material are as follows, and the compounding ratio of the alloy powder and the titanium powder was 98: 2. Alloy powder (Composition) Ag 37% by mass, In 30% by mass, oxygen content 0.05%, balance Cu (particle size distribution) d10: 8.7 ⁇ m, d50: 24.2 ⁇ m, d90: 45.5 ⁇ m Titanium powder d50: 8.0 ⁇ m
- the brazing filler metal layer formed of the brazing filler metal of the conventional example not containing Ag particles and active metal hydrides of Patent Document 1 has wrinkle-like irregularities formed on almost the entire surface thereof.
- the surface roughness (Rmax) of the brazing material layer was 25 ⁇ m or more.
- the peel strength of the test piece manufactured using the brazing material of patent document 1 was 10 (kN / m) or less.
- the brazing material layer formed of the brazing material according to the present invention has almost no ridge-like unevenness formed on its surface, and the surface roughness of the brazing material layer is 25 ⁇ m. It was below. And the peel strength of the test piece manufactured using the brazing material of patent document 1 was 15 (kN / m) or more. That is, it was confirmed that when the surface roughness Rmax of the brazing material layer is 25 ⁇ m or less, desired bonding strength can be secured.
- a ceramic master circuit board was produced in the same manner as in the above-mentioned Experiment Example 1 using the brazing material pastes of Experiment Nos. 36 to 52.
- a ceramic substrate a ceramic substrate similar to the above-mentioned Experimental example 1 made of silicon nitride was used.
- Various characteristics of the brazing material of each experimental number obtained in Experimental Example 2, the ceramic circuit board, and the test piece are as shown in Table 6.
- Example 3 In Experimental Example 3, the level of particle size distribution and bulk density of the brazing material as the mixed powder was changed to confirm the influence on bonding strength and the like.
- the mixed powder particle size distribution, bulk density, etc. were adjusted by changing the particle size distribution of each of the alloy powder, the Ag powder and the titanium hydride powder and the level of the addition amount.
- a ceramic master circuit board was manufactured in the same manner as in the above-mentioned Experimental Example 1 using the brazing material pastes of Experimental Nos. 53 to 93.
- a ceramic substrate a ceramic substrate similar to the above-mentioned Experimental example 1 made of silicon nitride was used.
- the peel strength (bonding strength) between the ceramic substrate and the metal plate in the formed test piece is 15 kN / m or more, and the ceramic master circuit board
- the failure rate of the thermal cycle test of the ceramic circuit board taken from the sample also became 5% or less.
- the wetting and spreading of the brazing material heated and melted at the time of joining is appropriate, the defective rate of insulation test between circuits of the ceramic circuit board and the defective rate of circuit pattern size also become 5% or less.
- the failure rate of the thermal cycle test is insufficient due to the lack of peel strength (bonding strength) as described below. Due to high or excessive wetting and spreading of the brazing material, the inter-circuit insulation test failure rate or the circuit pattern size failure rate was high.
- the equivalent circular diameter of each particle of titanium hydride powder confirmed in the state of mixed powder is in the range of 10 to 25 ⁇ m. In this case, it was confirmed that the desired peel strength was obtained, the rate of failure in the thermal cycle test was low, and furthermore, the spreading of the brazing material was appropriate and the rate of failure in inter-circuit insulation test and the rate of circuit pattern size failure were also low.
- a mixed powder containing titanium hydride having an equivalent circular diameter in this range is preferably an alloy of titanium hydride powder having a particle size distribution in the range of d10 of 5 to 15 ⁇ m, d50 of 10 to 25 ⁇ m, and d90 of 25 to 50 ⁇ m. It turned out that it can form by adding to powder.
- the preferable range of the equivalent circular diameter of each particle of the titanium hydride powder is 12 to 22 ⁇ m, more preferably 15 to 20 ⁇ m, as viewed from each defect rate.
- Hydrogenation preferably having a particle size distribution in the range of d10 of 7 to 12 ⁇ m, d50 of 13 to 22 ⁇ m, d90 of 25 to 39 ⁇ m, and d10 of 8 to 11 ⁇ m, d50 of 15 to 20 ⁇ m, and d90 of 26 to 35 ⁇ m It can be formed by adding titanium powder to the alloy powder. Furthermore, in Experiment No. 60 in which the additive amount of titanium hydride powder in the mixed powder was 2.65% by mass, the peel strength was improved, but in Experiment No.
- the brazing material in the state of the mixed powder is (1) Equivalent circle average diameter of particles of alloy powder, Ag powder and active metal hydride powder is in a relation of alloy powder ⁇ active metal hydride powder> Ag powder, and (2) in accordance with JIS Z 8825-1.
- the preferable range of the particle size distribution of the mixed powder is that d10 is 4 to 8 ⁇ m, d50 is 15 to 18 ⁇ m, and d90 is 35 to 49 ⁇ m.
- the inter-circuit insulation test failure rate, the circuit pattern size failure rate, and the thermal cycle test failure rate all become 3.0% or less.
- the range of the particle size distribution of the mixed powder is further confirmed to be d10 of 4.7 to 7 ⁇ m, d50 of 16 to 26 ⁇ m, and d90 of 36 to 47 ⁇ m.
- the mixed powder having the above particle size distribution is preferably an alloy powder having a d10 of 6 to 12 ⁇ m, a d50 of 15 to 40 ⁇ m, and a d90 of 60 ⁇ m or less, a d10 of 0.5 to 3 ⁇ m, a d50 of 1 to 15 ⁇ m, and a d90 of 8 It was confirmed that the film can be formed by adding an Ag powder of ⁇ 20 ⁇ m.
- the more preferable range of the particle size distribution of the alloy powder is that d10 is 7 to 12 ⁇ m, d50 is 20 to 35 ⁇ m, d90 is 55 ⁇ m or less, d10 is 8 to 11 ⁇ m, d50 is 20 to 30 ⁇ m, and d90 is 40 to 50 ⁇ m. If it is in the range, it is suitable. In addition, as a preferable range of the particle size distribution of the Ag powder, it was confirmed that d10 is 1 to 3.5 ⁇ m, d50 is 3 to 8 ⁇ m, and d90 is 8 to 14 ⁇ m.
- the experiment No. 81 in which the value of (d50 ⁇ d10) / (d90 ⁇ d10) is 0.68 corresponds to the inter-circuit insulation as to the experiment No. 63 in which the particle size distribution is almost the same except for d90.
- the test failure rate decreased.
- the experiment No. 82 in which the value of (d50 ⁇ d10) / (d90 ⁇ d10) is 0.19 the cold heat cycle failure rate is lower than that of the experiment No. 80 which has substantially the same particle size distribution except d90. Therefore, it was confirmed that (d50-d10) / (d90-d10) is preferably in the range of 0.2 to 0.65. A further preferred range is 0.3 to 0.5.
- the experiment number 83 in which the value of (d50 ⁇ d10) / 40% is 0.66 ⁇ m /% is the same as the experiment number 63 in which the particle size distribution is almost the same except for d50. Decreased.
- the experiment No. 84 in which the value of (d50 ⁇ d10) / 40% is ⁇ m /% the cold-heat cycle failure rate is lower than that of the experiment No. 80, which has substantially the same particle size distribution except d10. It is considered that this is because the filling property of each particle in the mixed powder (brazing material) is low. Therefore, it was confirmed that the range of 0.15 to 0.65 is preferable for (d50-d10) / 40%. A further preferred range is 0.25 to 0.55.
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Abstract
Description
好ましい態様のろう材に含まれる合金粉末は、上記のとおり、基本的に、Agを55~85質量%、Inを1~5質量%、残部Cu及び不可避不純物で構成され、好ましくは酸素含有量0.1質量%以下としたものである。酸素含有量が0.1質量%を超えると、昇温過程において最初に分解する活性金属水素化物粉末から生成する活性金属が、容易に酸素と反応して酸化物となるため、活性金属としての役割を果たさなくなる。すなわち、セラミックス基板とろう材層を接合するために必要な化合物層の生成が抑制されるため、接合界面にボイドが形成され接合強度の低下を招く。同様な理由で、Ag粉末および活性金属水素化物粉末の酸素含有量は、いずれも0.1質量%以下であることが好ましい。
Ag粉末は、d50が1~15μmのものを、合金粉末100重量部に対し5~30質量部の範囲で、ろう材に添加することが好ましい。後述する活性金属水素化物粉末とこのAg粉末を、合金粉末とは別の粉末として添加することにより、上記した粒度分布を有する合金粉末の粒子間の間隙に均一に埋めることができ、ろう材の充填性をより高めることができる。
活性金属水素化物粉末は、d50が10~25μm、好ましくはd10が5~15μmで、d90が25~50μmの粒度分布を有するものを、合金粉末100重量部に対し0.5~5質量部の範囲で、合金粉末とは別にろう材に添加することが好ましい。
本発明の別の態様であるろう材ペーストは、上記ろう材に対し、バインダーを1~10質量%、溶剤を2~20質量%添加し、混練することにより得たものである。なお、溶剤中におけるろう材およびバインダーの分散性を向上するため、分散剤を添加してもよい。ろう材ペーストを上記組成とすることにより、スクリーン印刷やカレンダー印刷などに適するろう材ペーストとすることができる。ここで、バインダーが1質量%よりも少ない場合には、ろう材ペーストの保形性が低下し、印刷パターンの形状精度が低下する場合がある。一方で、バインダーが10質量%を超えると、ろう付け処理後に形成されたろう材層中にカーボンが残存し、金属板とセラミック基板との間にボイド(空孔)が形成され、両者の接合強度を低下させる場合がある。なお、上記範囲でバインダーを配合すれば、印刷されたろう材から加熱等してバインダーを除去する脱脂工程において、バインダーが速やかに除去されるので好適である。
本発明の更に別の態様であるセラミックス回路基板は、セラミック基板の少なくとも一方の面に上記ろう材ペーストを塗布し、当該ろう材ペースト上に金属板を載置した後、5×10-3Pa以下の真空中において835℃で1時間加熱し、その後冷却することにより、前記セラミックス基板と金属板とが接合されたセラミックス回路基板のろう材層のボイド率が5%以下であることを特徴としている。かかるセラミックス回路基板によれば、合金粉末におけるInの添加量が低減された本発明に係るろう材を使用することにより、ろう材の表面に形成された鱗状凹凸が低減され、ろう材層のボイド率は5%以下であり、セラミックス基板と金属基板との接合強度を示す値であるピール強度が15(kN/m)以上と、所望の接合強度を有するセラミックス回路基板を構成することができる。
本発明の更に別の態様であるセラミックスマスター回路基板は、セラミックス基板の少なくとも一方の面に上記ろう材ペーストを塗布し、当該ろう材ペースト上に金属板を載置した後、5×10-3Pa以下の真空中において835℃で1時間加熱し、その後冷却することにより、前記セラミックス基板と金属板とが接合された、複数のセラミックス回路基板を採取することが出来るセラミックスマスター回路基板において、前記セラミックスマスター回路基板から採取されたセラミックス回路基板のろう材層のボイド率が5%以下で、前記セラミックスマスター回路基板の端面から10mm以内の端部に形成されたろう材層のボイド率が5%~50%であるセラミックスマスター回路基板である。
本発明の更に別の態様は、上記セラミックス回路基板の一方の面に接合した回路用金属板に半導体チップを搭載し、前記セラミックス基板の他方の面に放熱用金属板を接合してなるパワー半導体モジュールセラミックスである。かかるパワー半導体モジュールによれば、回路用金属板とセラミックス基板および放熱用金属板とセラミックス基板の接合安定性が維持できることで、冷熱サイクルに対する実装信頼性に優れたパワー半導体モジュールが提供できる。
実験例1~3に基づき本発明を具体的に説明する。以下の実験例1~3では、図3に示す寸法を有するセラミックス回路基板1を製品部6に9枚形成可能な、外周端から10mm以内に形成された端部5を有する図4に示す寸法のセラミックスマスター回路基板10を作成した。セラミックス基板2(20)としては窒化珪素、窒化アルミおよびアルミナを使用し、その厚みは0.32mmとした。なお、窒化珪素からなるセラミックス基板の曲げ強度は700MPa、破壊靱性値は6.5MPa1/2、窒化アルミからなるセラミックス基板の曲げ強度は350MPa、破壊靱性値は3.5MPa1/2、アルミナからなるセラミックス基板の曲げ強度は350MPa、破壊靱性値は4.0MPa1/2であった。また、回路用金属板4eおよび放熱用金属板4dを形成する金属板はいずれも銅基板(無酸素銅 JISH3100 C1020H)を使用し、厚みは各々0.5mmおよび0.4mmとした。
実験例1では、上記説明した本発明に係るろう材の有効性を確認するとともに、(1)Ag粉末および水素化チタン粉末(活性金属水素化物粉末)の組成比と混合粉末の粒度分布の関係および混合粉末の粒度分布、(2)合金粉末中のAgおよびInの添加量、(3)合金粉末におけるAg/(Ag+Cu)、(4)活性金属水素化物の材質、(5)セラミックス基板の材質について、水準および材質を変化させて接合強度等に及ぼす影響を確認した。
(1)粒度分布
合金粉末、Ag粉末および活性金属水素物粉末ならびにこれらを混合した混合粉末なあびに合金粉末およびAg粉末の粒度分布は、JISZ8825-1に準拠し、レーザ回折式の粒度測定装置(日機装製 型式:MT3300)で確認した。また、活性金属水素物粉末の粒度分布は、JISZ8825-1に準拠し、レーザ回折式の粒度測定装置(堀場製作所製 型式:LA-920)で確認した。
(2)かさ密度
混合粉末のかさ密度は、JISZ2504に準拠し、かさ密度測定装置(筒井理化学器械製)で確認した。
(3)等価円平均直径
合金粉末・Ag粉末・活性金属水素化物粉末の粒子の等価円平均直径は、次のようにして行った。まず、混合粉末から任意に採取した試料を、試料台の表面に配置されたカーボンテープ上に載置し、試料中の各粒子の位置を固定し、その後電子線マイクロアナライザ(EPMA)で観察した。そして、試料台の表面に形成された位置決めマークを基準に選択した0.5×0.5mmの視野において、Cu、Ag、Ti、HfおよびZrについて成分分析を行い、各元素の分布をマップ化してなる成分分析データに基づきAgおよびCuが含まれている粒子は合金粒子、Agを主とする粒子はAg粉末、Ti、HfまたはZrを主とする粒子は活性金属水素化物粉末であると特定した。次に、走査型電子顕微鏡(SEM)で、試料台の位置決めマークに基づき上記と同一の視野にて画像データを取得した。そして、上記マップ化された成分分析データと照らし合せ、合金粉末・Ag粉末・活性金属水素化物粉末の各々の粒子を同視野から任意に各々50個抽出した。なお、成分分析データおよび画像データを確認し、互いに接触しているまたは重なっていると考えられる粒子は、抽出から除外した。上記抽出した合金粉末・Ag粉末・活性金属水素化物粉末の各々の粒子の画像データに基づき、各粒子の面積を算出し、当該面積から各粒子の等価円直径を求めた。次いで、上記と同様にして6視野の測定を行い、合金粉末・Ag粉末・活性金属水素化物粉末の各粒子について、各々300個の等価円直径のデータを得、その平均値を各実験番号の等価円平均直径とした。
(4)活性金属水素化物の添加量
ろう材中に含まれる活性金属水素化物の添加量(質量%)は、高周波プラズマ発光分析装置(サーモジャーレルアッシュ製 IRIS ADVANTAGE)で分析してろう材中におけるTiの含有量を測定し、化学式量に基づき得られたTiの値に1.0426を乗じて算出した。
(1)回路間絶縁試験
回路間絶縁試験は、図3(a)に示すように、セラミックス回路基板1の上面に形成された回路用金属板4eの回路パターンを構成している金属板4a~4cのうち、ギャップ4f・4gを介し相対している3組の金属板4a・4b、4a・4cおよび4b・4cについて、各々、所定の測定点C~Hに電極端子を接触させ、DC1000Vで30秒印加した際の抵抗値が1GΩ以上あることを確認する試験である。例えば、ギャップ4fを介し相対している金属板4a・4bについては、測定点C・Dに各々電極端子を接触させ、C・D間の絶縁抵抗を確認した。ギャップ4gを介して相対している金属板4b・4c、およびギャップ4fを介して相対している金属板4a・4cについても、同様に、各々測定点E・FおよびG・Hの間の絶縁抵抗を確認した。そして、いずれかの測定点の間で抵抗値が1GΩ以下となったセラミックス回路基板は不良と判断した。なお、接合工程においてろう材の水平方向の濡れ拡がりが大きい場合には、図2に示すろう材層3a~3cの間のギャップ4f・4gの幅が狭くなり、絶縁抵抗が低くなる。
(2)回路パターン寸法検査
回路パターン寸法検査は、図3に示すセラミックス回路基板1のセラミックス基板2の外縁と回路用金属板4eおよび放熱用金属板4dの外縁間の寸法(図の場合には0.5mm)を工具顕微鏡で測定し、その寸法が一部でも0.25~0.75mmの間でない場合には不良と判断した。なお、図5(b)を参照して説明した接合工程において、溶融したろう材がセラミックス基板の上下面に配置した金属板の表面にまで濡れ拡がり付着した場合には、図5(c)を参照して説明したその後のエッチング工程において、当該付着したろう材により金属板のエッチングが妨げられるため、特にセラミックス基板2の外縁と回路用金属板4eおよび放熱用金属板4dの外縁間の寸法不良が生じやすくなる。
(3)冷熱サイクル試験
冷熱サイクル試験については、-55℃での冷却を30分、160℃での加熱を30分とする昇温/降温サイクルを1サイクルとし、これを1000回繰り返してセラミックス回路基板に付加し、セラミックス基板から回路用金属板または放熱用金属板が一部でも剥離した場合には不良と判断した。
セラミックス基板自体にクラックが生じ、冷熱サイクル試験不良率は高かった。
合金粉末 d10:8.7μm、d50:24.2μm、d90:45.5μm
Ag粉末 d10:2.7μm、d50:5.6μm、d90:9.9μm
水素化チタン粉末 d10:10.1μm、d50:18.7μm、d90:33.0μm
合金粉末 (組成)Ag37質量%、In30質量%、酸素含有量0.05%、残部Cu(粒度分布)d10:8.7μm、d50:24.2μm、d90:45.5μm
チタン粉末 d50:8.0μm
実験例2では、(1)合金粉末に含まれる酸素の含有量、(2)合金粉末に含まれるSiの含有量について、水準を変化させつつ接合強度等に及ぼす影響を確認した。
実験例3では、混合粉末であるろう材の粒度分布およびかさ密度等の水準を変化させ、接合強度等に及ぼす影響を確認した。ここで、混合粉末粒度分布およびかさ密度等は、合金粉末、Ag粉末および水素化チタン粉末の各々の粒度分布および添加量の水準を変化させることで調整した。
2 セラミックス基板
3a(3b~3d、7a) ろう材層
4a(4b~4c) 金属板
4e 回路用金属板
4d 放熱用金属板
5a 端部金属板
8a(8b~8c) 製品パターン
9a 端部パターン
10 セラミックスマスター回路基板
20 大型のセラミックス基板
40 大型の金属板
Claims (16)
- 少なくとも、Ag:55~80質量%、In:1~5質量%、残部Cu及び不可避不純物からなる合金粉末、Ag粉末ならびに活性金属水素化物粉末を混合して成る混合粉末である、セラミックス基板と金属板とを接合するろう材であって、
前記混合粉末に含まれるAgおよびCuの総量に対するAgの組成比Ag/(Ag+Cu)が0.57~0.85であり、
粒子の等価円平均直径が10~25μmである活性金属水素化物粉末を0.5~5.0質量%含み、
前記合金粉末、Ag粉末および活性金属水素化物粉末の粒子の等価円平均直径が、合金粉末≧活性金属水素化物粉末>Ag粉末の関係にあり、
前記混合粉末は、JIS Z 8825-1に準拠して粒度分布を測定したときの体積基準の累積分布において、10%累積粒子径(d10)が3~10μm、50%累積粒子径(d50)が10~35μm、90%累積粒子径(d90)が30~50μmの粒度分布を有するとともに、頻度分布において、50%累積粒子径(d50)と90%累積粒子径(d90)の間にピークが存在することを特徴とするろう材。 - 前記ピークが60%累積粒子径(d60)と80%累積粒子径(d80)の間に存在する請求項1に記載のろう材。
- かさ密度が3.6~5.5g/cm3である請求項1または2のいずれかに記載のろう材。
- (d50-d10)/(d90-d10)が0.25~0.65である請求項1乃至3のいずれかに記載のろう材。
- (d50-d10)/40(%)が、0.15~0.65(μm/%)である請求項1乃至4のいずれかに記載のろう材。
- Ag:55~80質量%、In:1~5質量%、酸素含有量0.1質量%以下、残部Cu及び不可避不純物からなる50%累積粒子径(d50)15~40μmの合金粉末と、前記合金粉末100質量部に対し、50%累積粒子径(d50)1~15μmのAg粉末粒子を5~30質量部、および、10%累積粒子径(d10)が5~15μm、50%累積粒子径(d50)が10~25μm、90%累積粒子径(d90)が25~50μmの粒度分布を有する活性金属水素化物粉末を0.5~5質量部を有する請求項1乃至5のいずれかに記載のろう材。
- 前記活性金属水素化物粉末は水素化チタン粉末である請求項1乃至6のいずれかに記載のろう材。
- 前記合金粉末に含まれるAgおよびCuの総量に対するAgの比Ag/(Ag+Cu)が、0.6~0.7である請求項1乃至7のいずれかに記載のろう材。
- 前記合金粉末は、Siを0.0001~0.5質量%含む請求項1乃至8のいずれかに記載のろう材。
- 前記合金粉末の10%累積粒子径(d10)が6~12μm、90%累積粒子径(d90)が60μm以下である請求項1乃至9のいずれかに記載のろう材。
- 前記Ag粉末の10%累積粒子径(d10)が0.5~3.5μm、90%累積粒子径(d90)が8~20μmである請求項1乃至10の何れかに記載のろう材。
- 請求項1乃至11のいずれかに記載のろう材に対し、バインダーを1~10質量%、溶剤を2~20質量%添加し、混練したろう材ペースト。
- 前記ろう材ペーストを、セラミックス基板の面上に厚さ45μm塗布した後、5×10-3Pa以下の真空中において835℃で1時間加熱し、その後冷却して形成されるろう材層の表面の表面粗さRmaxが25μm以下である請求項12に記載のろう材ペースト。
- セラミックス基板の少なくとも一方の面に請求項13又は14のいずれかに記載のろう材ペーストを塗布し、前記ろう材ペースト上に金属板を載置した後、5×10-3Pa以下の真空中において835℃で1時間加熱し、その後冷却することにより、前記セラミックス基板と金属板とが接合されたセラミックス回路基板のろう材層のボイド率が5%以下であるセラミックス回路基板。
- セラミックス基板の少なくとも一方の面に請求項13又は14のいずれかに記載のろう材ペーストを塗布し、前記ろう材ペースト上に金属板を載置した後、5×10-3Pa以下の真空中において835℃で1時間加熱し、その後冷却することにより、前記セラミックス基板と金属板とが接合された、複数のセラミックス回路基板を採取することが出来るセラミックスマスター回路基板において、前記セラミックスマスター回路基板から採取されたセラミックス回路基板のろう材層のボイド率が5%以下で、前記セラミックスマスター回路基板の端面から10mm以内の端部に形成されたろう材層のボイド率が5%~50%であるセラミックスマスター回路基板。
- 請求項14に記載のセラミックス回路基板の一方の面に接合した回路用金属板に半導体チップを搭載し、前記セラミックス基板の他方の面に放熱用金属板を接合してなるパワー半導体モジュール。
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US14/127,476 US9780011B2 (en) | 2011-06-30 | 2012-07-02 | Brazing material, brazing material paste, ceramic circuit substrate, ceramic master circuit substrate, and power semiconductor module |
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US20140126155A1 (en) | 2014-05-08 |
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EP2727898A9 (en) | 2014-08-20 |
CN103619779B (zh) | 2015-07-01 |
CN103619779A (zh) | 2014-03-05 |
JP5725178B2 (ja) | 2015-05-27 |
JPWO2013002407A1 (ja) | 2015-02-23 |
EP2727898A4 (en) | 2016-03-23 |
US9780011B2 (en) | 2017-10-03 |
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