WO2017047627A1 - Module de conversion thermoélectrique et dispositif de conversion thermoélectrique - Google Patents

Module de conversion thermoélectrique et dispositif de conversion thermoélectrique Download PDF

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Publication number
WO2017047627A1
WO2017047627A1 PCT/JP2016/077080 JP2016077080W WO2017047627A1 WO 2017047627 A1 WO2017047627 A1 WO 2017047627A1 JP 2016077080 W JP2016077080 W JP 2016077080W WO 2017047627 A1 WO2017047627 A1 WO 2017047627A1
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Prior art keywords
thermoelectric conversion
silver
layer
conversion module
conversion element
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PCT/JP2016/077080
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English (en)
Japanese (ja)
Inventor
宗太郎 大井
修司 西元
雅人 駒崎
航 岩崎
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三菱マテリアル株式会社
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Priority claimed from JP2016168783A external-priority patent/JP6750404B2/ja
Application filed by 三菱マテリアル株式会社 filed Critical 三菱マテリアル株式会社
Priority to KR1020187010529A priority Critical patent/KR20180056681A/ko
Priority to CN201680052731.8A priority patent/CN108028306B/zh
Priority to US15/760,658 priority patent/US20190058101A1/en
Priority to EP16846498.0A priority patent/EP3352233B1/fr
Publication of WO2017047627A1 publication Critical patent/WO2017047627A1/fr

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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
    • H10N10/80—Constructional details
    • H10N10/82—Connection of interconnections
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
    • H10N10/01—Manufacture or treatment
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
    • H10N10/10—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects operating with only the Peltier or Seebeck effects
    • H10N10/13—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects operating with only the Peltier or Seebeck effects characterised by the heat-exchanging means at the junction
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
    • H10N10/10—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects operating with only the Peltier or Seebeck effects
    • H10N10/17—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects operating with only the Peltier or Seebeck effects characterised by the structure or configuration of the cell or thermocouple forming the device
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
    • H10N10/80—Constructional details
    • H10N10/81—Structural details of the junction
    • H10N10/817—Structural details of the junction the junction being non-separable, e.g. being cemented, sintered or soldered
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
    • H10N10/80—Constructional details
    • H10N10/85—Thermoelectric active materials
    • H10N10/851—Thermoelectric active materials comprising inorganic compositions
    • H10N10/855—Thermoelectric active materials comprising inorganic compositions comprising compounds containing boron, carbon, oxygen or nitrogen

Definitions

  • the present invention relates to a thermoelectric conversion module in which a plurality of P-type thermoelectric conversion elements and N-type thermoelectric conversion elements are arranged in combination, and a thermoelectric conversion apparatus using the thermoelectric conversion module.
  • thermoelectric conversion module a pair of P-type thermoelectric conversion elements and N-type thermoelectric conversion elements are combined in a connected state with electrodes between a pair of wiring boards, in the order of P, N, P, and N. It is set as the structure electrically connected in series so that it may be arrange
  • both ends are connected to a DC power source, and heat is transferred in each thermoelectric conversion element by the Peltier effect (P type moves heat in the same direction as current and N type moves in the opposite direction to current). be able to.
  • thermoelectric conversion element an electromotive force can be generated in each thermoelectric conversion element by the Seebeck effect when a temperature difference is provided between the wiring boards by arranging one of the wiring boards on the high temperature side and the other on the low temperature side. For this reason, it is possible to use a thermoelectric conversion module for cooling, heating, or power generation.
  • Patent Document 1 discloses a thermoelectric conversion module in which an electrode is bonded to one surface of an insulating substrate as a wiring substrate.
  • the insulating substrate include a ceramic substrate such as aluminum nitride in addition to the resin substrate, and examples of the electrode include those made of copper, silver, silver-palladium, and the like. Solder is used for joining the electrodes of the wiring board and the thermoelectric conversion elements.
  • Patent Document 2 discloses that since the insulating substrate is made of a material having a small linear expansion coefficient, a linear notch is provided on the outer surface of the insulating substrate in order to prevent damage due to thermal strain. .
  • Patent Document 3 an intermediate layer made of titanium, a titanium alloy, or the like is provided between the electrode and the thermoelectric conversion element in order to prevent the phenomenon that the electrode material diffuses into the thermoelectric conversion element at a high temperature. It is disclosed.
  • thermoelectric conversion module in which an electrode and a thermoelectric conversion element are soldered, if the operating temperature is high (for example, 300 ° C. to 500 ° C.), the solder layer is softened and the joint reliability is lowered. There is a problem to do.
  • the ceramic substrate may be cracked.
  • the cut portion is formed in the insulating substrate as described in Patent Document 2, the cut portion may be a starting point of cracking.
  • the present invention has been made in view of such circumstances, and firmly bonds the thermoelectric conversion element and the electrode, prevents the ceramic substrate from cracking, and diffuses the electrode material to the thermoelectric conversion element.
  • the purpose is to prevent and improve reliability.
  • thermoelectric conversion module of the present invention is a thermoelectric conversion module comprising a pair of opposing wiring boards and a plurality of thermoelectric conversion elements connected between the wiring boards via the wiring boards,
  • the wiring substrate includes a ceramic substrate and an electrode layer made of aluminum or an aluminum alloy formed on one surface of the ceramic substrate and connected to the thermoelectric conversion element. A silver underlayer formed on the surface and bonded to the thermoelectric conversion element is provided.
  • the silver underlayer does not soften even at high temperatures, it has excellent bonding reliability. Therefore, excellent heat resistance is exhibited by using the wiring substrate having this silver underlayer on the high temperature side.
  • the electrode layer As described in Patent Document 1, since the deformation resistance of copper is large, the ceramic substrate is likely to crack due to thermal stress, but aluminum having a smaller deformation resistance than copper or By using the electrode layer made of an aluminum alloy, it is possible to reduce the thermal stress on the ceramic substrate and suppress the occurrence of cracks.
  • the silver underlayer is formed on the electrode layer, the aluminum component of the electrode layer is prevented from diffusing into the thermoelectric conversion element, and high reliability can be maintained for a long time.
  • the silver underlayer is composed of a glass layer formed on the electrode layer and a silver layer made of a silver fired body laminated on the glass layer. Can be.
  • the glass layer on the electrode layer surface reacts with the oxide film on the electrode layer surface and the oxide film can be removed from the electrode layer surface, the electrode layer and the thermoelectric conversion element can be more reliably joined.
  • thermoelectric conversion module of the present invention a metallized layer made of any one of gold, silver, and nickel may be formed on the end surface joined to the electrode layer in the thermoelectric conversion element.
  • the metallized layer can further strengthen the bonding between the end face of the thermoelectric conversion element and the electrode layer.
  • thermoelectric conversion module of the present invention the silver underlayer and the metallized layer of the thermoelectric conversion element are bonded directly or via a silver bonding layer made of a sintered body of silver.
  • thermoelectric conversion element When the silver underlayer and the metallized layer of the thermoelectric conversion element are directly joined, there is no soldering material, so even when used in a high temperature environment, the bonding material between the electrode layer and the thermoelectric conversion element There is no occurrence of melting or the like, and the electrode layer and the thermoelectric conversion element are reliably bonded. Therefore, it can be used stably even in a high temperature environment. On the other hand, when a silver bonding layer is interposed, the same kind of metal as that of the silver base layer can be bonded more firmly.
  • thermoelectric conversion module of the present invention when the metallized layer is made of either gold or silver, a barrier layer made of either nickel or titanium is formed between the end face of the thermoelectric conversion element and the metallized layer. It is good to be. These barrier layers reliably prevent the diffusion of gold or silver into the thermoelectric conversion element, which may occur slightly when the metallized layer is made of gold or silver, and maintain the characteristics of the thermoelectric conversion element well. Can do.
  • the electrode layer may be made of aluminum having a purity of 99.99% by mass or more.
  • Aluminum having a purity of 99.99% by mass or more (so-called 4N aluminum) has a smaller deformation resistance, so it can absorb thermal strain at high temperatures and reliably prevent cracking of the ceramic substrate.
  • thermoelectric conversion module of the present invention a heat transfer metal layer may be bonded to the other surface of the ceramic substrate.
  • the heat transfer metal layer By providing the heat transfer metal layer, heat transfer can be improved, and the electrode layer is disposed on one surface of the ceramic substrate and the heat transfer metal layer is disposed on the other surface.
  • the front and back can have a symmetrical structure, the warpage of the wiring board can be prevented, the assemblability to the thermoelectric conversion module is good, and the long-term reliability can be improved.
  • thermoelectric conversion module comprising: the thermoelectric conversion module; a heat sink for heat absorption bonded to the heat transfer metal layer in one wiring substrate; and a heat sink for heat dissipation bonded to the heat transfer metal layer in the other wiring substrate.
  • a thermoelectric conversion module may be used. And it can also be set as the thermoelectric conversion apparatus provided with the thermoelectric conversion module with the heat sink, and the liquid cooling type cooler fixed to the said heat sink for thermal radiation.
  • the bonding reliability is excellent, and diffusion of the electrode layer material to the thermoelectric conversion element can be prevented.
  • the deformation resistance of the electrode layer is small, the ceramic substrate can be prevented from cracking, and a thermoelectric conversion module with high long-term reliability can be obtained.
  • FIG. 2 is a cross-sectional plan view taken along the line AA in FIG.
  • FIG. 3 is a cross-sectional plan view in the direction of the arrow along line BB in FIG.
  • FIG. 2 is an enlarged cross-sectional view of the vicinity of a joint portion between an electrode layer of a wiring board and a thermoelectric conversion element in FIG. 1.
  • It is an expanded sectional view which shows the joining state of the silver base layer to an electrode layer.
  • It is the graph which modeled the change of the curvature of the thermoelectric conversion module accompanying the temperature change at the time of use.
  • It is a longitudinal cross-sectional view which shows the thermoelectric conversion module of 2nd Embodiment of this invention.
  • FIG. 8 is an enlarged cross-sectional view of the vicinity of the joint between the electrode layer of the wiring board and the thermoelectric conversion element in FIG. 7. It is a longitudinal cross-sectional view which shows the example of the thermoelectric conversion apparatus which attached the heat sink to the thermoelectric conversion module.
  • thermoelectric conversion module 1 of this embodiment has a P-type thermoelectric conversion element 3 and an N-type thermoelectric conversion element 4 connected between a pair of opposed wiring boards 2A and 2B. It is the structure arranged in a shape (one-dimensional shape) or a planar shape (two-dimensional shape).
  • FIGS. 1 to 3 show an example in which two pairs of P-type thermoelectric conversion elements 3 and N-type thermoelectric conversion elements 4 are arranged. It is provided in a line.
  • thermoelectric conversion module 1 is entirely housed in a case 5 and is attached so as to be interposed between a high temperature side channel 6 through which high temperature gas flows and a low temperature side channel 7 through which cooling water flows.
  • a conversion device 81 is configured.
  • a heat sink 8 having rod-like fins 8a is provided in the high temperature side flow path 6, and an elastic member 9 such as a spring for pressing the heat sink 8 toward the wiring board 2A is provided.
  • electrode layers 12 and 13 are formed on one surface of the ceramic substrate 11, and a heat transfer metal layer 14 is formed on the other surface.
  • the ceramic substrate 11 include aluminum nitride (AlN), alumina (Al 2 O 3 ), silicon nitride (Si 3 N 4 ), silicon carbide (SiC), a carbon plate, and a diamond thin film substrate formed on a graphite plate.
  • An insulating ceramic substrate having high thermal conductivity is used. The thickness of the ceramic substrate 11 is 0.2 mm to 1.5 mm.
  • the electrode layers 12, 13 are arranged on the first wiring board 2 ⁇ / b> A on the upper side in FIG. 1, which is one wiring board, as shown in FIG. 2.
  • An electrode layer 12 composed of two electrode portions 12A and 12B having a rectangular shape in plan view and connected to each pair is formed.
  • the second wiring board 2B on the lower side of FIG. 1, which is the other wiring board has a pair of thermoelectric conversion elements 3, 3 connected to each other by the electrode layer 12 of the first wiring board 2A. 4
  • an electrode portion 13 ⁇ / b> A that connects one pair of N-type thermoelectric conversion elements 4 and the other pair of P-type thermoelectric conversion elements 3 is formed at the center of the row of thermoelectric conversion elements 3 and 4.
  • Electrode portions 13B and 13C connected to one pair of P-type thermoelectric conversion elements 3 and the other pair of N-type thermoelectric conversion elements 4 are respectively formed at both ends. These three electrode portions 13A to 13C constitute an electrode layer 13. Further, the external wiring portion 15 is formed integrally with the electrode portions 13B and 13C at both ends or by welding different members, for example.
  • Electrode layers 12 and 13 are made of aluminum or an aluminum alloy, and are formed by being bonded to the surface of the ceramic substrate 11.
  • aluminum as a material of the electrode layers 12 and 13, aluminum (so-called 4N aluminum) having a purity of 99.99% by mass or more is preferable.
  • the size (area) of each electrode portion 12A, 12B, 13A to 13C is slightly larger than the area of the end face of the thermoelectric conversion elements 3 and 4, depending on the size of the thermoelectric conversion elements 3 and 4 connected to these electrode portions. It is set large.
  • the electrode layers 12 and 13 have a thickness of 0.05 mm to 2.0 mm.
  • the heat transfer metal layer 14 is made of aluminum or an aluminum alloy like the electrode layers 12 and 13 and is formed by being bonded to the surface of the ceramic substrate 11.
  • aluminum as the material, aluminum (so-called 4N aluminum) having a purity of 99.99% by mass or more is preferable.
  • the thickness is not particularly limited, but is preferably about the same thickness as the electrode layers 12 and 13.
  • the electrode layers 12 and 13 and the heat transfer metal layer 14 are joined to the ceramic substrate 11 by brazing or the like.
  • a silver underlayer 21 is formed on the surfaces of the electrode layers 12 and 13, and the end faces of the thermoelectric conversion elements 3 and 4 are joined to the silver underlayer 21.
  • the silver underlayer 21 is a layer formed by applying a glass-containing silver paste on the surface of the electrode layers 12 and 13 and baking it, and as shown in FIGS. 4 and 5, the electrode layers 12 and 13 side.
  • the glass layer 23 is formed in two layers, and the silver layer 24 is formed on the glass layer 23.
  • fine conductive particles 31 having a particle size of about several nanometers are dispersed inside the glass layer 23.
  • the conductive particles 31 are crystalline particles containing at least one of silver and aluminum.
  • the conductive particles 31 in the glass layer 23 can be observed by using, for example, a transmission electron microscope (TEM).
  • TEM transmission electron microscope
  • fine glass particles 32 having an average particle diameter of about several nanometers are dispersed inside the silver layer 24.
  • the electrode layers 12 and 13 are made of aluminum having a purity of 99.99% by mass or more, an aluminum oxide film 35 naturally generated in the atmosphere is formed on the surfaces of the electrode layers 12 and 13. However, in the portion where the silver underlayer 21 is formed, the aluminum oxide film 35 is removed by the formation of the glass layer 23, and the silver underlayer 21 is formed directly on the electrode layers 12 and 13. That is, as shown in FIG. 5, the aluminum constituting the electrode layers 12 and 13 and the glass layer 23 of the silver underlayer 21 are directly bonded.
  • the thickness t0 of the aluminum oxide film 35 that naturally occurs on the electrode layers 12 and 13 is in the range of 1 nm ⁇ t0 ⁇ 6 nm.
  • the thickness tg of the glass layer 23 is in the range of 0.01 ⁇ m ⁇ tg ⁇ 5 ⁇ m
  • the thickness ta of the silver layer 24 is in the range of 1 ⁇ m ⁇ ta ⁇ 100 ⁇ m.
  • the total thickness of the silver underlayer 21 is 1.01 ⁇ m to 105 ⁇ m.
  • the volume density of silver is 55% to 90%
  • the volume density of glass is 1% to 5%
  • the remainder is pores.
  • the electrical resistance value P in the thickness direction of the silver underlayer 21 is 0.5 ⁇ or less.
  • the electrical resistance value P in the thickness direction of the silver underlayer 21 is the electrical resistance between the surface of the silver underlayer 21 (surface of the silver layer 24) and the surfaces of the electrode layers 12 and 13. Resistance value. This is because the electric resistance of aluminum (4N aluminum) constituting the electrode layers 12 and 13 is very small compared to the electric resistance in the thickness direction of the silver underlayer 21.
  • the surface center point of the silver underlayer 21 and the distance below the silver by the same distance as the distance along the surface direction from the surface center point of the silver underlayer 21 to the periphery of the silver underlayer 21.
  • the electrical resistance between the points on the electrode layers 12 and 13 away from the periphery of the formation 21 is measured.
  • thermoelectric conversion element 3 As a material of the P-type thermoelectric conversion element 3 and the N-type thermoelectric conversion element 4, a silicide-based material, an oxide-based material, a skutterudite (intermetallic compound of transition metal and pnictogen), a half-Whistler, or the like is used. It can. Of these, silicide-based materials that have little impact on the environment and have abundant resource reserves are attracting attention.
  • Manganese silicide (MnSi 1.73 ) is a P-type thermoelectric conversion element 3 and magnesium silicide (Mg 2 Si) is an N-type.
  • the thermoelectric conversion element 4 is obtained.
  • thermoelectric conversion elements 3 and 4 are formed in a prismatic shape having a square cross section (for example, 1 mm to 8 mm on one side), for example, and the length (the length along the facing direction of the wiring boards 2A and 2B) is 2 mm to 8 mm. It is said.
  • a metallized layer 25 including one of nickel, silver, and gold is formed on both end faces of each thermoelectric conversion element 3, 4. Further, when the metallized layer 25 is made of silver or gold, a barrier made of a single layer made of either nickel or titanium or a laminated structure thereof is further provided between the metallized layer 25 and each of the thermoelectric conversion elements 3 and 4. Layer 26 is formed.
  • the metallized layer 25 is formed of silver, the same kind of metal is bonded to the silver base layer 21 and a better bonded state can be obtained.
  • thermoelectric conversion module 1 configured as described above.
  • the wiring boards 2A and 2B are obtained by bonding the electrode layers 12 and 13 to one surface of the ceramic substrate 11 and the heat transfer metal layer 14 to the other surface with an Al—Si brazing material or the like. Specifically, an aluminum plate to be the electrode layers 12 and 13 and an aluminum plate to be the heat transfer metal layer 14 are laminated on the ceramic substrate 11 through brazing materials, and these are pressed in the laminating direction at 610 ° C. The electrode layers 12 and 13 and the heat transfer metal layer 14 are joined to the ceramic substrate 11 by heating to ⁇ 650 ° C.
  • the ceramic substrate 11 and the electrode layers 12 and 13 and the heat transfer metal layer 14 have different thermal expansion coefficients, thermal distortion is likely to occur at the joint portion, but the electrode layers 12 and 13 and the heat transfer metal layer 14 are Since it is formed of aluminum or an aluminum alloy, thermal strain can be absorbed. In addition, since the electrode layers 12 and 13 and the heat transfer metal layer 14 are provided symmetrically via the ceramic substrate 11, the occurrence of warpage can be prevented.
  • the glass-containing silver paste contains a silver powder, a glass (lead-free glass) powder, a resin, a solvent, and a dispersant. It is set to 60 mass% or more and 90 mass% or less of the whole silver paste, and the remainder is made into resin, a solvent, and a dispersing agent.
  • the silver powder has a particle size of 0.05 ⁇ m or more and 1.0 ⁇ m or less, and for example, an average particle size of 0.8 ⁇ m is suitable.
  • the glass powder has any one of bismuth oxide (Bi 2 O 3 ), zinc oxide (ZnO), boron oxide (B 2 O 3 ), lead oxide (PbO 2 ), and phosphorus oxide (P 2 O 5 ) as a main component.
  • the glass transition temperature is 300 ° C. or higher and 450 ° C. or lower, the softening temperature is 600 ° C. or lower, and the crystallization temperature is 450 ° C. or higher.
  • glass powder containing lead oxide, zinc oxide and boron oxide and having an average particle size of 0.5 ⁇ m is suitable.
  • solvent those having a boiling point of 200 ° C. or more are suitable, and for example, diethylene glycol dibutyl ether is used.
  • Resin is used to adjust the viscosity of the glass-containing silver paste, and those that decompose at 350 ° C. or higher are suitable.
  • ethyl cellulose is used.
  • a dicarboxylic acid-based dispersant is appropriately added.
  • You may comprise a glass-containing silver paste, without adding a dispersing agent.
  • This glass-containing silver paste is prepared by premixing a mixed powder obtained by mixing silver powder and glass powder and an organic mixture obtained by mixing a solvent and a resin together with a dispersant using a mixer, and the resulting premixed mixture is obtained using a roll mill. After mixing while kneading, the resulting kneaded product is produced by filtering with a paste filter.
  • the viscosity of the glass-containing silver paste is adjusted to 10 Pa ⁇ s or more and 500 Pa ⁇ s or less, more preferably 50 Pa ⁇ s or more and 300 Pa ⁇ s or less.
  • the glass-containing silver paste is applied to the electrode layers 12 and 13 by a screen printing method or the like, and dried and then fired at a temperature of 350 ° C. to 645 ° C. for 1 minute to 60 minutes.
  • a temperature of 350 ° C. to 645 ° C. for 1 minute to 60 minutes At this time, when the glass layer 23 is formed, the aluminum oxide film 35 naturally generated on the surfaces of the electrode layers 12 and 13 is melted and removed, and the glass layer 23 is directly attached to the electrode layers 12 and 13. Then, the silver layer 24 is formed on the glass layer 23.
  • the silver layer 24 is securely held and fixed on the electrode layers 12 and 13.
  • conductive particles (crystalline particles) 31 containing at least one of silver and aluminum are dispersed in the glass layer 23, and it is assumed that the particles are precipitated in the glass layer 23 during firing. Yes. Also, fine glass particles 32 are dispersed inside the silver layer 24. The glass particles 32 are presumed to be agglomeration of the remaining glass components in the process of firing the silver particles.
  • the heat treatment conditions for forming the silver underlayer 21 are set such that the heating temperature is in the range of 350 ° C. or more and 645 ° C. or less, and the holding time at the heating temperature is in the range of 1 minute or more and 60 minutes or less.
  • the average crystal grain size of the silver layer in the silver underlayer formed after the heat treatment is adjusted within the range of 0.5 ⁇ m to 3.0 ⁇ m.
  • the firing becomes insufficient and the silver underlayer 21 may not be sufficiently formed.
  • the heating temperature exceeds 645 ° C. and when the holding time at the heating temperature exceeds 60 minutes, the firing proceeds too much and the average crystal grains of the silver layer 24 in the silver underlayer 21 formed after the heat treatment There is a possibility that the diameter does not fall within the range of 0.5 ⁇ m to 3.0 ⁇ m.
  • the lower limit of the heating temperature during the heat treatment is preferably 400 ° C. or higher, and more preferably 450 ° C. or higher.
  • the holding time at the heating temperature is preferably 5 minutes or more, and more preferably 10 minutes or more.
  • the heating temperature during the heat treatment is preferably 600 ° C. or lower, more preferably 575 ° C. or lower. Further, the holding time at the heating temperature is preferably 45 minutes or less, and more preferably 30 minutes or less.
  • thermoelectric conversion elements 3 and 4 for example, manganese silicide (MnSi 1.73 ) and magnesium silicide (Mg 2 Si), which are silicide materials, are respectively prepared as mother alloys and, for example, a particle diameter of 75 ⁇ m or less is obtained by a ball mill. After the pulverization, for example, a disk-shaped or square plate-shaped bulk material is produced by plasma discharge sintering, hot pressing, hot isostatic pressing, and this is cut into, for example, a prismatic shape, whereby thermoelectric conversion elements 3 and 4 are produced. Formed as.
  • thermoelectric conversion elements 3 and 4 a metallized layer 25 including any one of nickel, silver, and gold, and if necessary, a single layer made of either nickel or titanium, or these layers A barrier layer 26 having a laminated structure is formed.
  • the metallized layer 25 and the barrier layer 26 are formed by plating, sputtering or the like.
  • thermoelectric conversion elements between the wiring boards 2A and 2B so that the metal base layer 25 on the end faces of the thermoelectric conversion elements 3 and 4 are superimposed on the silver base layer 21 of the electrode layers 12 and 13 of the wiring boards 2A and 2B. 3 and the N-type thermoelectric conversion element 4 are arranged side by side.
  • the pressing force in the stacking direction 5 MPa or more and 40 MPa or less
  • the heating temperature 200 ° C. or more and 400 ° C. or less
  • the holding time at the heating temperature heating for 1 minute to 60 minutes To do.
  • the silver layer 24 of the silver underlayer 21 of the electrode layers 12 and 13 and the metallized layer 25 of the thermoelectric conversion elements 3 and 4 are directly bonded by solid phase diffusion bonding.
  • the applied pressure when the applied pressure is less than 5 MPa, the bonding strength between the thermoelectric conversion elements 3 and 4 and the electrode layers 12 and 13 may be insufficient. When the applied pressure exceeds 40 MPa, the ceramic substrate 11 may be cracked.
  • the applied pressure is more preferably 10 MPa or more and 35 MPa or less.
  • thermoelectric conversion elements 3, 4 and the electrode layers 12, 13 When the heating temperature is less than 200 ° C. and the holding time at the heating temperature is less than 1 minute, the bonding strength between the thermoelectric conversion elements 3, 4 and the electrode layers 12, 13 may be insufficient, When the temperature exceeds 400 ° C. and when the holding time at the heating temperature exceeds 60 minutes, the characteristics of the thermoelectric conversion elements 3 and 4 may be deteriorated by heat.
  • thermoelectric conversion element 3 and the N-type thermoelectric conversion element 4 are integrated in a state of being connected in series between the wiring boards 2A and 2B. Then, the thermoelectric conversion elements 3 and 4 joined and integrated between the wiring boards 2A and 2B are hermetically accommodated in a case 5 formed of stainless steel or the like, and the inside is kept in a vacuum or reduced pressure state. Then, the thermoelectric conversion module 1 is produced and packaged.
  • the external wiring portion 15 is drawn outside in an insulated state with respect to the case 5. Note that the case 5 is not necessarily required, and the case 5 may not be provided.
  • thermoelectric conversion module 1 configured in this manner is used as an external heat source on one wiring board (first wiring board) 2A side of both wiring boards 2A and 2B.
  • a high-temperature side flow path 6 through which a high-temperature fluid of °C to 500 °C circulates as shown by an arrow is in contact, and cooling water of 80 °C to 100 °C circulates as a heat medium on the other wiring board (second wiring board) 2B side
  • the low temperature side flow path 7 to be contacted is contacted.
  • thermoelectric conversion module 1 of this embodiment since the electrode layers 12 and 13 and the heat transfer metal layer 14 of the wiring boards 2A and 2B are formed of aluminum or aluminum alloy having a low deformation resistance, the thermal stress on the ceramic substrate 11 is reduced. And generation
  • the electrode layers 12 and 13 and the heat transfer metal layer 14 are symmetrically arranged via the ceramic substrate 11, warpage at the time of bonding is reduced, and the subsequent incorporation of the thermoelectric conversion elements 3 and 4 is performed. Work becomes easy.
  • thermoelectric conversion elements 3 and 4 are bonded to the electrode layers 12 and 13 by the silver underlayer 21, the silver underlayer 21 is not softened like solder even when used at a high temperature. Excellent in properties.
  • the silver underlayer 21 is interposed between the electrode layers 12 and 13 and the thermoelectric conversion elements 3 and 4, the aluminum component of the electrode layers 12 and 13 may diffuse into the thermoelectric conversion elements 3 and 4. And high reliability can be maintained in the long term.
  • thermoelectric conversion module 1 has high reliability because the occurrence of warpage is reduced with respect to temperature changes during use.
  • FIG. 6 schematically shows a change in warpage of the thermoelectric conversion module 1 due to a temperature change during use. Since the wiring boards 2A and 2B are assembled with the warpage reduced as described above, the warpage of the thermoelectric conversion module 1 is almost “0” at room temperature, and the fluid at 300 ° C. to 500 ° C. is placed in the high temperature side channel 6. , And a fluid of 80 ° C. to 100 ° C. flows through the low temperature side flow path 7, the thermoelectric conversion module 1 has a temperature distribution particularly on the front and back of the high temperature side wiring board (first wiring board) 2A. As a result, there is a risk of warping as the temperature rises.
  • thermoelectric conversion module 1 can maintain stable performance over the long term.
  • thermoelectric conversion module 51 a silver bonding layer 22 is further formed on the silver base layer 21, and the thermoelectric conversion elements 3 and 4 are bonded by the silver bonding layer 22.
  • the silver bonding layer 22 is a fired body of silver formed by firing silver particles, and is formed by applying and heating a silver paste made of silver powder and resin or the like.
  • the silver bonding layer 22 has a silver volume density of 55% to 95%, and the remainder is pores.
  • the thickness is 5 ⁇ m to 50 ⁇ m.
  • the glass particle 32 observed by the silver layer 24 of the silver base layer 21 does not exist, or even when it exists, there are very few.
  • thermoelectric conversion elements In order to join the thermoelectric conversion elements to the electrode layers 12 and 13 by the silver joining layer 22, first, a silver paste is applied on the silver base layer 21 of the electrode layers 12 and 13 of the wiring boards 2A and 2B.
  • This silver paste contains silver powder having a particle size of 0.05 ⁇ m to 100 ⁇ m, a resin, and a solvent.
  • ethyl cellulose or the like can be used as the resin used for the silver paste.
  • a solvent used for the silver paste ⁇ -terpineol or the like can be used.
  • the composition of the silver paste is such that the silver powder content is 60% by mass or more and 92% by mass or less of the entire silver paste, the resin content is 1% by mass or more and 10% by mass or less of the entire silver paste, and the balance is the solvent. Good.
  • the silver paste contains an organic metal compound powder such as carboxylic acid metal salt such as silver formate, silver acetate, silver propionate, silver benzoate, silver oxalate, etc. It can also be made. Moreover, 0 mass% or more and 10 mass% or less of reducing agents, such as alcohol and an organic acid, can also be contained with respect to the whole silver paste as needed.
  • the silver paste has a viscosity adjusted to 10 Pa ⁇ s to 100 Pa ⁇ s, more preferably 30 Pa ⁇ s to 80 Pa ⁇ s.
  • thermoelectric conversion elements 3 and 4 After applying this silver paste on the silver underlayer 21 of the electrode layers 12 and 13 of the wiring boards 2A and 2B by screen printing or the like and drying, the end faces of the thermoelectric conversion elements 3 and 4 are placed on the silver paste layer.
  • the P-type thermoelectric conversion element 3 and the N-type thermoelectric conversion element 4 are arranged side by side between the wiring boards 2A and 2B so that the metallized layers 25 are overlapped.
  • heating and sintering are performed in a heating furnace under conditions in which the pressing force in the stacking direction is 0 MPa to 10 MPa, the heating temperature is 150 ° C. to 600 ° C., and the holding time is 1 minute to 60 minutes.
  • the electrode layers 12 and 13 on which the silver underlayer 21 is formed and the thermoelectric conversion elements 3 and 4 are bonded via the silver bonding layer 22.
  • thermoelectric conversion elements 3 and 4 are directly bonded to the silver base layer 21 of the electrode layers 12 and 13, the height variation of the components affects the bonding property, and the plane of the components Even in such a case, the silver underlayer 21 on the surface of the electrode layers 12 and 13 is connected to the silver underlayer 21 via the silver bonding layer 22, as in the thermoelectric conversion module 51 of this embodiment.
  • both the high temperature side and low temperature side wiring boards are formed with a silver underlayer formed on the electrode layer and bonded to the thermoelectric conversion element. What is necessary is just to form and join with a thermoelectric conversion element. Also in the second embodiment, both the high temperature side and low temperature side wiring boards are formed with a silver underlayer on the electrode layer and bonded to the thermoelectric conversion element by the silver bonding layer. The structure should just be applied to the junction part of an electrode layer and a thermoelectric conversion element.
  • the silver underlayer is a layer in which a silver foil is joined on the electrode layer by brazing or solid phase diffusion, in addition to the glass layer and the silver layer formed by firing as in the embodiment.
  • a layer by silver plating and a layer by silver sputtering are also included.
  • the electrode layer is formed on one surface of the ceramic substrate and the heat transfer metal layer is formed on the other surface, only the electrode layer may be formed.
  • both the wiring boards are brought into contact with the high temperature side flow path or the low temperature side flow path, they are not necessarily limited to those having a flow path configuration, and may be anything in contact with the heat source and the cooling medium.
  • thermoelectric conversion element only one P-type or N-type thermoelectric conversion element is arranged in series between a pair of wiring boards, and unitized for each P-type or N-type, and the unit of the P-type thermoelectric conversion element and N It is also possible to connect a unit of a thermoelectric conversion element to form a thermoelectric conversion module.
  • each electrode part and the cross-sectional shape of each thermoelectric conversion element are not limited to a square, but may be a rectangle, a circle, or the like.
  • a silver oxide paste when forming a silver bonding layer, can be used instead of the silver paste.
  • the silver oxide paste contains silver oxide powder, a reducing agent, a resin, and a solvent, and in addition to these, contains an organometallic compound powder.
  • the content of the silver oxide powder is 60% by mass or more and 92% by mass or less of the entire silver oxide paste, and the content of the reducing agent is 5% by mass or more and 15% by mass or less of the entire silver oxide paste.
  • the content is 0% by mass or more and 10% by mass or less of the entire silver oxide paste, and the remainder is a solvent.
  • the reduced silver particles deposited by reducing the silver oxide at the time of bonding (firing) are very fine, for example, with a particle size of 10 nm to 1 ⁇ m. Therefore, a dense silver bonding layer can be formed and bonded more firmly.
  • thermoelectric conversion module 51 As another form of the above embodiment, as shown in FIG. 9, a structure in which a heat sink is joined to the thermoelectric conversion module 51 shown in FIG. However, in FIG. 9, the case 5 is not used.
  • the heat sinks 60 and 61 are made of aluminum or aluminum alloy, copper or copper alloy, aluminum silicon carbide composite (AlSiC) formed by impregnating aluminum or aluminum alloy in a porous body made of silicon carbide, or the like.
  • the heat sink may be provided with pin-shaped fins 62 or may be a flat plate without the fins 62.
  • a heat sink 61 having a flat plate-like heat sink 60 on the high temperature side and pin-like fins 62 on the low temperature side is provided.
  • the thickness of the top plate portion 61a can be set to 0.5 mm to 8 mm, respectively.
  • the thermoelectric conversion module 51 is provided with a flat heat sink 60 on one side and a heat sink 61 having fins 62 on the other side.
  • the high-temperature side is fixed in a state where a flat heat sink 60 is in contact with a heat source 65 such as a furnace wall, and the low-temperature side is a heat sink having fins 62 in a liquid-cooled cooler 70 through which cooling water or the like can flow.
  • 61 is fixed to constitute the thermoelectric converter 82.
  • the liquid cooling cooler 70 has a flow path 71 formed therein, and is fixed in a state where the top plate portion 61 a of the heat sink 61 is in contact with the periphery of the opening 72 on the side wall, and the fins 62 are connected to the flow path 71 from the opening 72. It is arranged in the inserted state.
  • Reference numeral 76 denotes a resin seal member interposed between the liquid cooling type cooler 70 and the top plate portion 61 a of the heat sink 61.
  • the heat transfer metal layer 14 and the heat sinks 60 and 61 were made of vacuum brazing using an Al—Si brazing material or the like, brazing in a nitrogen atmosphere using a flux, or using an Al brazing material containing Mg. Bonded by fluxless brazing, solid phase diffusion bonding, or the like. By setting it as such a structure, the thermal resistance of the thermoelectric conversion elements 3 and 4 and the heat source 65 and the thermal resistance of the thermoelectric conversion elements 3 and 4 and the liquid cooling cooler 70 can be reduced.
  • a wiring substrate was fabricated by bonding a 4N-aluminum electrode layer and a heat transfer metal layer to a ceramic substrate made of silicon nitride having a thickness of 0.32 mm using an Al-Si brazing material.
  • the electrode layer and the heat transfer metal layer had the same thickness and were 0.18 mm.
  • a glass-containing silver paste was applied to the surface of the electrode layer by screen printing and baked at 500 ° C. to 550 ° C. in the atmosphere to form a silver underlayer having a thickness of 10 ⁇ m.
  • the copper terminal was joined to the electrode part for the external connection of an electrode layer by ultrasonic welding.
  • thermoelectric conversion element made of manganese silicide and an N-type thermoelectric conversion element made of magnesium silicide were each formed in a prismatic shape.
  • a metallized layer made of silver was formed on the end face of the thermoelectric conversion element.
  • thermoelectric conversion element is sandwiched between both wiring boards so that the end face of the thermoelectric conversion element is superimposed on the silver underlayer of the electrode layer, and in this state, heating temperature: 300 ° C., pressure: 10 MPa, heating Temperature retention time: 30 minutes and firing in air.
  • the test body (Example 1) of the thermoelectric conversion module which directly joined the thermoelectric conversion element which has a metallization layer, and the silver base layer of an electrode layer was produced.
  • the silver paste described in the above embodiment was applied on the silver underlayer of the electrode layer by using a dispenser, and the end surfaces of the thermoelectric conversion elements were overlapped on the silver paste.
  • thermoelectric conversion element was sandwiched between the wiring boards, and in this state, the substrate was baked in the atmosphere at a heating temperature of 300 ° C., a pressing force of 10 MPa, and a holding time at the heating temperature of 30 minutes. Thereby, the test body (Example 2) of the thermoelectric conversion module which joined the thermoelectric conversion element which has a metallization layer to the silver base layer of the electrode layer via the silver joining layer was also produced.
  • thermoelectric conversion module (Comparative Example 1) in which a thermoelectric conversion element is bonded by a silver bonding layer without forming a silver underlayer on the surface of the electrode layer, and the electrode layer are formed of a copper alloy
  • a test body (Comparative Example 2) in which a silver base layer was formed thereon and a thermoelectric conversion element was bonded was also produced.
  • thermoelectric conversion module was subjected to 300 cycles of cooling cycle between ⁇ 40 ° C. and 300 ° C., the bonding state between the electrode layer of the wiring board and the thermoelectric conversion element, the crack of the ceramic substrate.
  • the change in electrical resistance was defined as “good” when the rate of change after the cooling cycle was 5% or less with respect to the initial state, and “bad” when it exceeded 5%.
  • Comparative Example 1 cracks were not observed in the ceramic substrate, but peeling was observed at the joint between the electrode layer and the thermoelectric conversion element, so that the bonding was poor. In Comparative Example 2, cracks were generated in the ceramic substrate. Was. For this reason, in any case, an appropriate electrical resistance value could not be obtained.
  • Thermoelectric conversion module can be used for a cooling device, a heating device, or a power generation device.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)

Abstract

L'invention concerne un module de conversion thermoélectrique (1) qui est obtenu en reliant une pluralité d'éléments de conversion thermoélectrique (3, 4) par le biais d'une paire de substrats de câblage (2A, 2B) qui se font mutuellement face dans un état tel que les éléments de conversion thermoélectrique (3, 4) sont combinés les uns avec les autres entre les substrats de câblage (2A, 2B). Chacun des substrats de câblage (2A, 2B) est obtenu en formant une couche d'électrode (12, 13) sur une surface d'un substrat en céramique (11), ladite couche d'électrode (12, 13) étant reliée aux éléments de conversion thermoélectrique (3, 4) et étant constituée d'aluminium ou d'un alliage d'aluminium. Au moins la couche d'électrode (12) qui est disposée sur le côté à haute température est pourvue d'une couche à base d'argent (21) dans laquelle une couche de verre et une couche d'argent sont stratifiées dans la surface ; et la couche d'argent de la couche à base d'argent (21) est connectée aux éléments de conversion thermoélectrique (3, 4).
PCT/JP2016/077080 2015-09-18 2016-09-14 Module de conversion thermoélectrique et dispositif de conversion thermoélectrique WO2017047627A1 (fr)

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KR1020187010529A KR20180056681A (ko) 2015-09-18 2016-09-14 열전 변환 모듈 및 열전 변환 장치
CN201680052731.8A CN108028306B (zh) 2015-09-18 2016-09-14 热电转换模块及热电转换装置
US15/760,658 US20190058101A1 (en) 2015-09-18 2016-09-14 Thermoelectric conversion module and thermoelectric conversion device
EP16846498.0A EP3352233B1 (fr) 2015-09-18 2016-09-14 Module de conversion thermoélectrique et dispositif de conversion thermoélectrique

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