WO2023190451A1 - 接合体の製造方法 - Google Patents

接合体の製造方法 Download PDF

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Publication number
WO2023190451A1
WO2023190451A1 PCT/JP2023/012389 JP2023012389W WO2023190451A1 WO 2023190451 A1 WO2023190451 A1 WO 2023190451A1 JP 2023012389 W JP2023012389 W JP 2023012389W WO 2023190451 A1 WO2023190451 A1 WO 2023190451A1
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Prior art keywords
pressure
temperature
mpa
coating film
laminate
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Ceased
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PCT/JP2023/012389
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English (en)
French (fr)
Japanese (ja)
Inventor
真一 山内
隆志 服部
圭 穴井
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Mitsui Kinzoku Co Ltd
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Mitsui Mining and Smelting Co Ltd
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Priority to JP2024512524A priority Critical patent/JPWO2023190451A1/ja
Publication of WO2023190451A1 publication Critical patent/WO2023190451A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00—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
    • 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
    • B22F7/08—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 with one or more parts not made from powder
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10W—GENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10
    • H10W72/00—Interconnections or connectors in packages
    • H10W72/071—Connecting or disconnecting

Definitions

  • the present invention relates to a method for manufacturing a joined body.
  • Patent Document 1 discloses that a laminate in which a substrate, a bonding layer, and a semiconductor element are sequentially stacked is prepared using a bonding layer containing sinterable metal particles having a particle size of 100 nm or less, A first pressure is applied between the semiconductor element and the substrate of the laminate at a first temperature lower than the sintering temperature of the sinterable metal particles of the bonding layer, and then the sintering of the sinterable metal particles of the bonding layer is applied.
  • a second pressure exceeding the first pressure is applied between the semiconductor element and the substrate of the laminate, which is at a second temperature higher than the sintering temperature, to sinter the bonding layer, and connect the semiconductor element to the substrate via the bonding layer.
  • a technique for joining is disclosed.
  • an object of the present invention is to provide a method for producing a bonded body that has excellent bonding strength between the bonded body and the bonding layer, particularly in the fillet portion.
  • the present inventors have conducted a drying process on the coating film placed on the first object before placing the second object on it. After that, by placing the second object to be joined and applying heat and pressure to the coating film at a predetermined timing, the adhesion between the first object to be joined and the coating film is improved, and as a result, the fillet It has been found that the bonding strength between the first object to be bonded and the bonding layer formed from the coating film can be improved.
  • the present invention provides a method for manufacturing a bonded body in which a first bonded body and a second bonded body are bonded together via a bonding layer, and the method includes a method for manufacturing a bonded body formed by bonding a first bonded body and a second bonded body through a bonding layer, and in which forming a coating film by applying a paste containing copper particles having a volume cumulative particle size D50 of more than 100 nm in % to the first object to be bonded; drying the coating film at a first temperature; and drying.
  • a subsequent step of placing the second object to be bonded on the coating film to form a laminate heating the laminate to a second temperature equal to or higher than the first temperature; applying a first pressure between the first object and the second object; heating the laminate to a third temperature higher than the second temperature; the step of applying a second pressure equal to or higher than the first pressure between the first object to be joined and the second object to be joined, and sintering the coating film to form the bonding layer.
  • the present invention provides a method.
  • FIG. 1 is a schematic diagram showing the first step of the method for manufacturing a joined body of the present invention.
  • FIG. 2 is a schematic diagram showing a step subsequent to the step shown in FIG. 1.
  • 1 and 2 are process diagrams illustrating a method for joining a joined body according to the present invention.
  • a paste containing copper particles is applied onto the first object 11 to form a coating film 12X.
  • the method for applying the paste is not particularly limited, and examples thereof include screen printing, gravure printing, dispense printing, reverse coating, and doctor blade methods.
  • the paste used in the present invention appropriately contains copper particles, an organic solvent, and a regulator described below.
  • the shape of the copper particles contained in the paste is not particularly limited, and both spherical and non-spherical particles can be used.
  • the fact that the copper particles are spherical means that the circularity coefficient measured by the following method is 0.85 or more.
  • the circularity coefficient is calculated by the following method. That is, when a scanning electron microscope image of a primary copper particle is taken, and the area of the two-dimensional projected image of the copper particle is S and the perimeter is L, the circularity coefficient of the copper particle is 4 ⁇ S/L 2 Calculated from the formula.
  • the fact that the copper particles are non-spherical means that the above-mentioned circularity coefficient is less than 0.85.
  • Specific examples of non-spherical shapes include flat shapes, polyhedral shapes such as hexahedrons and octahedrons, spindle shapes, and irregular shapes.
  • one of the two or more types of copper powder is a flat copper particle, and it is more preferable that the copper powder contains flat copper particles and spherical copper particles as described below.
  • the flat shape refers to a shape having a pair of plate surfaces forming the main surface of the particle and side surfaces perpendicular to these plate surfaces, and the plate surfaces and the side surfaces are each independently, It can be a flat, curved or uneven surface.
  • the particle size shall be determined by the following method. That is, the Heywood diameter of each of 50 or more primary copper particles with clear outlines is selected using an image observed with a scanning electron microscope at a magnification of 10,000 times or more and 150,000 times or less. Next, from the obtained Heywood diameter, the volume is calculated assuming that the particles are true spheres, and the volume cumulative particle size at 50% by volume of the cumulative volume is determined by D SEM50 .
  • the D SEM50 of the copper particles is preferably greater than 0.1 ⁇ m, more preferably 0.11 ⁇ m or more, and even more preferably 0.12 ⁇ m or more.
  • the D SEM50 is preferably 0.55 ⁇ m or less, more preferably 0.5 ⁇ m or less.
  • the particle size is determined by the volume cumulative particle size D 50 at a cumulative volume of 50% by volume by laser diffraction scattering particle size distribution measuring method.
  • this can be done by the following method. That is, 0.1 g of a measurement sample and an aqueous dispersant solution are mixed and dispersed for 1 minute using an ultrasonic homogenizer (manufactured by Nippon Seiki Seisakusho, US-300T). Thereafter, D 50 is calculated by measuring the particle size distribution using, for example, MT3300 EXII manufactured by Microtrack Bell as a laser diffraction scattering type particle size distribution measuring device.
  • the D50 of the copper particles is preferably 0.3 ⁇ m or more and 50 ⁇ m or less, more preferably 0.5 ⁇ m or more and 40 ⁇ m or less, and even more preferably 1 ⁇ m or more and 20 ⁇ m or less.
  • the content of copper particles in the paste is preferably 50% by mass or more, from the viewpoint of increasing the filling property of copper particles and maintaining sufficient bonding strength as a bonding layer, and is preferably 60% by mass or more and 95% by mass. % or less is more preferable.
  • a surface treatment agent may be attached to the surface of the copper particles. By attaching a surface treatment agent to the surface of the copper particles, excessive aggregation of the copper particles can be suppressed.
  • the surface treatment agent is not particularly limited, and fatty acids, aliphatic amines, silane coupling agents, titanate coupling agents, aluminate coupling agents, etc. can be used. By using these, it is possible to interact with the particle surface and improve the compatibility with the organic solvent contained in the paste, thereby improving the fluidity of the paste and preventing oxidation of the particle surface.
  • the viscosity value at a shear rate of 10 s -1 is preferably 10 Pa-s or more and 200 Pa-s or less, and more preferably 15 Pa-s or more and 200 Pa-s or less. preferable.
  • the viscosity is measured using a rheometer (viscoelasticity measuring device). The measured values were obtained using a parallel type sensor and a shear rate of 10 s -1 .
  • the viscosity of the paste can be measured using a rheometer MARS III manufactured by Thermo Scientific.
  • the conditions for measuring the viscosity of the paste are as follows. Measurement mode: Shear rate dependent measurement Sensor: Parallel type ( ⁇ 20mm) Measurement temperature: 25°C Gap: 0.300mm Shear rate: 0.05 ⁇ 120.01s -1 Measurement time: 2 minutes
  • the thickness of the coating film 12X is preferably 1 ⁇ m or more and 300 ⁇ m or less, and more preferably 5 ⁇ m or more and 250 ⁇ m or less so that the bonding layer described below can ensure sufficient bonding strength.
  • organic solvents examples include monoalcohols, polyhydric alcohols, polyhydric alcohol alkyl ethers, polyhydric alcohol aryl ethers, esters, nitrogen-containing heterocyclic compounds, amides, amines, and saturated hydrocarbons. These organic solvents can be used alone or in combination of two or more.
  • the paste may contain an appropriate adjusting agent for adjusting various properties as described above.
  • the modifier include reducing agents, viscosity modifiers, and surface tension modifiers.
  • the reducing agent is preferably one that promotes sintering of the copper particles, such as monoalcohol, polyhydric alcohol, amino alcohol, citric acid, oxalic acid, formic acid, ascorbic acid, aldehyde, hydrazine and its derivatives, hydroxylamine and its derivatives.
  • examples include derivatives, dithiothreitol, phosphite, hydrophosphite, phosphorous acid and its derivatives.
  • the viscosity modifier is preferably one that can adjust the viscosity of the paste, preferably within the above viscosity range, such as ketones, esters, alcohols, glycols, hydrocarbons, polymers, etc. .
  • the surface tension adjusting agent is preferably one that can adjust the surface tension of the coating film 12X, such as polymers such as acrylic surfactants, silicone surfactants, alkyl polyoxyethylene ethers, fatty acid glycerol esters, alcohols, carbonized Examples include hydrogen-based monomers, ester-based monomers, and glycol monomers.
  • polymers such as acrylic surfactants, silicone surfactants, alkyl polyoxyethylene ethers, fatty acid glycerol esters, alcohols, carbonized Examples include hydrogen-based monomers, ester-based monomers, and glycol monomers.
  • the first temperature is preferably a temperature that evaporates the organic solvent, regulator, etc. in the coating film 12X and does not sinter the copper particles. Therefore, the temperature is preferably 60°C or more and 150°C or less, more preferably 80°C or more and 130°C or less. Note that it is not necessary that the entire amount of the organic solvent be removed, and it is sufficient that the organic solvent be removed to the extent that the coating film 12X loses its fluidity. Therefore, the organic solvent may remain in the coating film 12X, and its content may be, for example, 15% by mass or less, particularly 10% by mass or less.
  • the coating film 12X can be dried in an inert atmosphere or in the air. Alternatively, the reaction may be carried out under reduced pressure.
  • the drying time is set to sufficiently evaporate the organic solvent, conditioning agent, etc. in the coating film 12X, and to sinter the copper particles having the above-mentioned D50 to obtain a bonding layer with sufficient thickness and sufficient bonding strength.
  • the drying time is preferably 1 minute or more, more preferably 5 minutes or more and 120 minutes or less, and even more preferably 10 minutes or more and 60 minutes or less.
  • the second object to be bonded 13 is placed on the dried coating film 12X to form a laminate 15.
  • both the first object 11 and the second object 13 contain metal on their surfaces to be welded.
  • a member having a surface made of metal can be used as at least one of the first object 11 and the second object 13.
  • metal refers to a metal itself that does not form a compound with other elements, or an alloy of two or more metals. Examples of such metals include copper, silver, gold, aluminum, palladium, nickel, and alloys consisting of a combination of two or more thereof.
  • the surface made of metal may be made of one kind of metal, or the surface made of metal may be made of one kind of metal. It may be composed of more than one metal. When composed of two or more metals, the surface may be an alloy. Generally, it is preferable that the metal surface be a flat surface, but it may be a curved surface in some cases.
  • the first object to be bonded 11 and the second object to be bonded 13 include, for example, a spacer or a heat sink made of the above-mentioned metal, a semiconductor element, and a substrate having at least one of the above-mentioned metals on its surface. etc.
  • the substrate for example, an insulating substrate having a metal layer such as copper on the surface of a ceramic or aluminum nitride plate can be used.
  • the semiconductor element contains one or more of elements such as Si, Ga, Ge, C, N, and As.
  • the first object to be bonded 11 is preferably a substrate.
  • the second object to be bonded 13 is preferably a spacer, a heat sink, or a semiconductor element.
  • a dried paste containing fine metal particles and an organic solvent can be used as at least one of the first object 11 and the second object 13.
  • a member having a surface made of metal can be used, and as the second object to be joined 13, a dried paste containing fine metal particles and an organic solvent can be used.
  • a dried form of paste it is preferable to apply the paste to a supporting base material made of metal such as copper and dry it to obtain a dried form.
  • the laminate 15 is held between predetermined jigs 16, 16, and the laminate 15 is heated to a second temperature higher than the first temperature.
  • a first pressure is applied between the first object 11 and the second object 13 of the body 15 .
  • This step is a pre-baking step for the coating film 12X, and in this step, the viscosity of the coating film 12X acts on the first and second objects 11 and 13 to be bonded. The relative position between the bonded bodies 13 is maintained, and the bonding strength due to the coating film 12X, which will later become the bonding layer 12, is increased.
  • the second temperature is preferably a temperature higher than or equal to the first temperature, specifically 100°C or higher and 300°C or lower, and more preferably 130°C or higher and 280°C or lower.
  • the first pressure is set from the viewpoint of ensuring good adhesion between the coating film 12X and the first object 11 and ensuring sufficient bonding strength between the bonding layer 12 at the fillet portion and the first object 11, It is preferably 0.001 MPa or more and 10 MPa or less, more preferably 1 MPa or more and 10 MPa or less, and still more preferably 2 MPa or more and 8 MPa or less.
  • the operation of placing the second object 13 on the dried coating film 12X is included between the heating to the first temperature and the heating to the second temperature.
  • This operation is performed by heating to a first temperature, taking out the first object 11 on which the coating film 12X is formed from the heating furnace, and then placing the second object 13 on the coating film 12X. It's okay.
  • heating to the first temperature and heating to the second temperature are performed independently.
  • the second object 13 to be bonded is placed on the coating film 12X, and the heating is performed from the first temperature to the second temperature. It may be done continuously.
  • the timing of the rise from the first temperature to the second temperature and the timing of application of the first pressure may or may not match.
  • the laminate 15 is heated to a third temperature higher than the second temperature, and the first object 11 and the second object 13 of the laminate 15 are heated using the jigs 16, 16. During this period, a second pressure higher than the first pressure is applied.
  • This step is a main firing step of the coating film 12X, and the coating film 12X is fired in this step to become the bonding layer 12 for the first object 11 and the second object 13 to be bonded.
  • the third temperature is preferably a temperature higher than or equal to the second temperature, specifically 180°C or higher and 350°C or lower, more preferably 200°C or higher and 300°C or lower.
  • the third temperature is preferably a temperature higher than or equal to the second temperature, specifically 180°C or higher and 350°C or lower, more preferably 200°C or higher and 300°C or lower.
  • the second pressure is preferably 1 MPa or more and 40 MPa or less, and more preferably 10 MPa or more and 30 MPa or less, from the viewpoint of ensuring sufficient bonding strength with the first object 11 and the second object 13.
  • the second pressure holding time is preferably 1 second or more and 60 minutes or less, more preferably 1 minute or more and 30 minutes or less.
  • Heating to the third temperature may be performed subsequent to heating to the second temperature, or may be performed independently. Further, the second temperature and the third temperature may be the same as long as the effects of the present invention are not impaired. Furthermore, the timing of the rise from the second temperature to the third temperature and the timing of application of the second pressure may or may not match. Further, the heating in this step may be performed in an inert atmosphere or in the air.
  • the organic solvent, conditioning agent, etc. inherent in the coating film 12X are properly removed. can be evaporated into Thereafter, the second object to be bonded 13 is placed on the coating film 12X and heated and applied at a second temperature and a first pressure, thereby improving the adhesion between the first object to be bonded 11 and the coating film 12X. Also at the fillet portion, a good bonding relationship can be obtained without the coating film 12X peeling off from the first object 11 to be bonded.
  • the rate of pressure increase to the first pressure is preferably 0.2 MPa/sec or more and 20 MPa/sec or less, more preferably 0.5 MPa/sec or more and 7 MPa/sec or less. This increases the bonding strength between the coating film 12X and the first object to be bonded 11, the bonding strength between the bonding layer 12 and the first object to be bonded 11, and further the bonding strength between the bonding layer 12 and the second object to be bonded 13. can be improved.
  • the pressure increase rate to the second pressure is preferably 0.2 MPa/s or more, and may be 1 MPa/s or more. Further, the rate of pressure increase to the second pressure is preferably 20 MPa/sec or less, more preferably 10 MPa/sec or less. This increases the bonding strength between the coating film 12X and the first object to be bonded 11, the bonding strength between the bonding layer 12 and the first object to be bonded 11, and further the bonding strength between the bonding layer 12 and the second object to be bonded 13. can be improved.
  • the ratio of the second temperature to the third temperature is preferably 0.28 or more and 1.00 or less, more preferably 0.36 or more and 0.95 or less on a Celsius basis. , more preferably 0.50 or more and 0.90 or less.
  • the ratio of the first pressure to the second pressure is preferably 0.025 or more and 1.00 or less, more preferably 0.05 or more and 0.80 or less, based on Pa. , more preferably 0.10 or more and 0.50 or less.
  • the bonding structure obtained according to the present invention takes advantage of the high bonding properties between the objects to be bonded and the bonding layer in the fillet portion, and is suitable for use in, for example, in-vehicle electronic circuits and electronic circuits in which power devices are mounted. .
  • the temperature is maintained at a predetermined temperature within a range that does not impede the effects of the present invention. It is also possible to heat the material or apply a predetermined pressure.
  • the present invention further discloses the following method for manufacturing a joined body.
  • an Ag-plated alumina chip was prepared (0.5 cm x 0.5 cm, thickness 0.5 mm) assuming a model member of a semiconductor power device. Next, the Ag-plated surface of this alumina chip was placed on the dried coating film, a load of 0.8 MPa was applied for 2 seconds, and the first object to be bonded, the coating film, and the second object to be bonded were laminated in this order. A laminate was formed.
  • Example 2 The steps from “(1) Preparation of paste” to “(3) Placing the second object to be bonded on the dried coating film (formation of laminate)” were carried out in the same manner as in Example 1.
  • Example 3 The steps from “(1) Preparation of paste” to “(3) Placing the second object to be bonded on the dried coating film (formation of laminate)" were carried out in the same manner as in Example 1.
  • Example 4 The steps from “(1) Preparation of paste” to “(3) Placing the second object to be bonded on the dried coating film (formation of laminate)" were carried out in the same manner as in Example 1.
  • Example 5 "(1) Preparation of paste” was carried out in the same manner as in Example 1. The steps from “(2) Applying the paste to the first object to be bonded” to “(3) Placing the second object to be bonded on the dried coating film (formation of a laminate)" are the same as in Example 1. Four sets were performed using the following procedure.
  • the delay and width of the S gate were adjusted so that the peak position of the S gate was on the surface of the copper plate.
  • the delay of the F gate was adjusted and the width was set to a peak width of 1.5 wavelengths.
  • the Z-axis coordinate of the probe was adjusted so that the amplitude of the observed peak was maximized, and observation was performed. Note that the brightness of the image was automatically set using the operation software (FineSAT) of the device, and image data for analysis was obtained. Next, peeling (%) of the fillet portion was calculated using this image data for analysis and image processing software imageJ.
  • a fillet portion with a threshold value of 201 or more in imageJ was defined as a peeled portion.
  • the coating film part is X
  • the joint part where the alumina chips are pressure bonded is Y (25 mm 2 )
  • the peeled part of the fillet part (X-Y) is Z
  • the peeled part of the fillet part (%) Z / (X-Y ) ⁇ 100 was calculated.
  • the peeling (%) of the fillet portion was calculated for four laminates, and the four average values were calculated. Table 1 shows the calculation results of the peeling (%) of the fillet portion. When the peeling of the fillet portion is 30% or less, it can be determined that the bonding strength between the object to be bonded and the bonding layer at the fillet portion is high.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Pressure Welding/Diffusion-Bonding (AREA)
  • Powder Metallurgy (AREA)
PCT/JP2023/012389 2022-03-30 2023-03-28 接合体の製造方法 Ceased WO2023190451A1 (ja)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020032161A1 (ja) * 2018-08-08 2020-02-13 三井金属鉱業株式会社 接合用組成物、並びに導電体の接合構造及びその製造方法
JP2020136580A (ja) * 2019-02-22 2020-08-31 株式会社大阪ソーダ 導電性接着剤を用いる接合方法
WO2020208713A1 (ja) * 2019-04-09 2020-10-15 三菱電機株式会社 パワー半導体モジュール及び電力変換装置
WO2021235447A1 (ja) * 2020-05-18 2021-11-25 田中貴金属工業株式会社 導電性組成物、導電性焼結部、および導電性焼結部を備えている部材

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020032161A1 (ja) * 2018-08-08 2020-02-13 三井金属鉱業株式会社 接合用組成物、並びに導電体の接合構造及びその製造方法
JP2020136580A (ja) * 2019-02-22 2020-08-31 株式会社大阪ソーダ 導電性接着剤を用いる接合方法
WO2020208713A1 (ja) * 2019-04-09 2020-10-15 三菱電機株式会社 パワー半導体モジュール及び電力変換装置
WO2021235447A1 (ja) * 2020-05-18 2021-11-25 田中貴金属工業株式会社 導電性組成物、導電性焼結部、および導電性焼結部を備えている部材

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