TW201840416A - 接合材及使用其之接合體 - Google Patents

接合材及使用其之接合體 Download PDF

Info

Publication number
TW201840416A
TW201840416A TW107110271A TW107110271A TW201840416A TW 201840416 A TW201840416 A TW 201840416A TW 107110271 A TW107110271 A TW 107110271A TW 107110271 A TW107110271 A TW 107110271A TW 201840416 A TW201840416 A TW 201840416A
Authority
TW
Taiwan
Prior art keywords
silver
bonding layer
bonding
bonding material
bonded
Prior art date
Application number
TW107110271A
Other languages
English (en)
Inventor
堀達朗
遠藤圭一
藤本英幸
栗田哲
Original Assignee
日商同和電子科技有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 日商同和電子科技有限公司 filed Critical 日商同和電子科技有限公司
Publication of TW201840416A publication Critical patent/TW201840416A/zh

Links

Classifications

    • 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
    • B22F7/062—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 involving the connection or repairing of preformed parts
    • B22F7/064—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 involving the connection or repairing of preformed parts using an intermediate powder layer
    • 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
    • B22F7/02—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 layers
    • B22F7/04—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 layers with one or more layers not made from powder, e.g. made from solid metal
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0545—Dispersions or suspensions of nanosized particles
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
    • 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
    • B22F1/17—Metallic particles coated with metal
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/48—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor
    • H01L23/488—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of soldered or bonded constructions
    • H01L23/495—Lead-frames or other flat leads
    • H01L23/49579—Lead-frames or other flat leads characterised by the materials of the lead frames or layers thereon
    • H01L23/49582—Metallic layers on lead frames
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
    • H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L24/27—Manufacturing methods
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
    • H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
    • H01L24/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
    • H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L24/31—Structure, shape, material or disposition of the layer connectors after the connecting process
    • H01L24/32—Structure, shape, material or disposition of the layer connectors after the connecting process of an individual layer connector
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
    • H01L24/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
    • H01L24/83—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a layer connector
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
    • H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
    • H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
    • H01L29/16—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only elements of Group IV of the Periodic Table
    • H01L29/1608—Silicon carbide
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/18—Printed circuits structurally associated with non-printed electric components
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/25—Noble metals, i.e. Ag Au, Ir, Os, Pd, Pt, Rh, Ru
    • B22F2301/255—Silver or gold
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/02—Bonding areas; Manufacturing methods related thereto
    • H01L2224/04—Structure, shape, material or disposition of the bonding areas prior to the connecting process
    • H01L2224/04026—Bonding areas specifically adapted for layer connectors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/02—Bonding areas; Manufacturing methods related thereto
    • H01L2224/04—Structure, shape, material or disposition of the bonding areas prior to the connecting process
    • H01L2224/05—Structure, shape, material or disposition of the bonding areas prior to the connecting process of an individual bonding area
    • H01L2224/0554—External layer
    • H01L2224/05599—Material
    • H01L2224/056—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof
    • H01L2224/05638—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof the principal constituent melting at a temperature of greater than or equal to 950°C and less than 1550°C
    • H01L2224/05639—Silver [Ag] as principal constituent
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/02—Bonding areas; Manufacturing methods related thereto
    • H01L2224/04—Structure, shape, material or disposition of the bonding areas prior to the connecting process
    • H01L2224/05—Structure, shape, material or disposition of the bonding areas prior to the connecting process of an individual bonding area
    • H01L2224/0554—External layer
    • H01L2224/05599—Material
    • H01L2224/056—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof
    • H01L2224/05638—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof the principal constituent melting at a temperature of greater than or equal to 950°C and less than 1550°C
    • H01L2224/05644—Gold [Au] as principal constituent
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/02—Bonding areas; Manufacturing methods related thereto
    • H01L2224/04—Structure, shape, material or disposition of the bonding areas prior to the connecting process
    • H01L2224/05—Structure, shape, material or disposition of the bonding areas prior to the connecting process of an individual bonding area
    • H01L2224/0554—External layer
    • H01L2224/05599—Material
    • H01L2224/056—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof
    • H01L2224/05663—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof the principal constituent melting at a temperature of greater than 1550°C
    • H01L2224/05664—Palladium [Pd] as principal constituent
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L2224/27—Manufacturing methods
    • H01L2224/27001—Involving a temporary auxiliary member not forming part of the manufacturing apparatus, e.g. removable or sacrificial coating, film or substrate
    • H01L2224/27005—Involving a temporary auxiliary member not forming part of the manufacturing apparatus, e.g. removable or sacrificial coating, film or substrate for aligning the layer connector, e.g. marks, spacers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L2224/27—Manufacturing methods
    • H01L2224/273—Manufacturing methods by local deposition of the material of the layer connector
    • H01L2224/2731—Manufacturing methods by local deposition of the material of the layer connector in liquid form
    • H01L2224/2732—Screen printing, i.e. using a stencil
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L2224/27—Manufacturing methods
    • H01L2224/278—Post-treatment of the layer connector
    • H01L2224/27848—Thermal treatments, e.g. annealing, controlled cooling
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L2224/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
    • H01L2224/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
    • H01L2224/29001—Core members of the layer connector
    • H01L2224/29099—Material
    • H01L2224/291—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof
    • H01L2224/29138—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof the principal constituent melting at a temperature of greater than or equal to 950°C and less than 1550°C
    • H01L2224/29139—Silver [Ag] as principal constituent
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L2224/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
    • H01L2224/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
    • H01L2224/29001—Core members of the layer connector
    • H01L2224/29099—Material
    • H01L2224/29198—Material with a principal constituent of the material being a combination of two or more materials in the form of a matrix with a filler, i.e. being a hybrid material, e.g. segmented structures, foams
    • H01L2224/29199—Material of the matrix
    • H01L2224/29294—Material of the matrix with a principal constituent of the material being a liquid not provided for in groups H01L2224/292 - H01L2224/29291
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L2224/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
    • H01L2224/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
    • H01L2224/29001—Core members of the layer connector
    • H01L2224/29099—Material
    • H01L2224/29198—Material with a principal constituent of the material being a combination of two or more materials in the form of a matrix with a filler, i.e. being a hybrid material, e.g. segmented structures, foams
    • H01L2224/29298—Fillers
    • H01L2224/29299—Base material
    • H01L2224/293—Base material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof
    • H01L2224/29338—Base material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof the principal constituent melting at a temperature of greater than or equal to 950°C and less than 1550°C
    • H01L2224/29339—Silver [Ag] as principal constituent
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L2224/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
    • H01L2224/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
    • H01L2224/29001—Core members of the layer connector
    • H01L2224/29099—Material
    • H01L2224/29198—Material with a principal constituent of the material being a combination of two or more materials in the form of a matrix with a filler, i.e. being a hybrid material, e.g. segmented structures, foams
    • H01L2224/29298—Fillers
    • H01L2224/29399—Coating material
    • H01L2224/2949—Coating material with a principal constituent of the material being a polymer, e.g. polyester, phenolic based polymer, epoxy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L2224/31—Structure, shape, material or disposition of the layer connectors after the connecting process
    • H01L2224/32—Structure, shape, material or disposition of the layer connectors after the connecting process of an individual layer connector
    • H01L2224/321—Disposition
    • H01L2224/32151—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
    • H01L2224/32221—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
    • H01L2224/32245—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
    • H01L2224/83—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a layer connector
    • H01L2224/8319—Arrangement of the layer connectors prior to mounting
    • H01L2224/83192—Arrangement of the layer connectors prior to mounting wherein the layer connectors are disposed only on another item or body to be connected to the semiconductor or solid-state body
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
    • H01L2224/83—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a layer connector
    • H01L2224/832—Applying energy for connecting
    • H01L2224/83201—Compression bonding
    • H01L2224/83203—Thermocompression bonding, e.g. diffusion bonding, pressure joining, thermocompression welding or solid-state welding
    • H01L2224/83204—Thermocompression bonding, e.g. diffusion bonding, pressure joining, thermocompression welding or solid-state welding with a graded temperature profile
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
    • H01L2224/83—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a layer connector
    • H01L2224/8338—Bonding interfaces outside the semiconductor or solid-state body
    • H01L2224/83399—Material
    • H01L2224/834—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof
    • H01L2224/83438—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof the principal constituent melting at a temperature of greater than or equal to 950°C and less than 1550°C
    • H01L2224/83447—Copper [Cu] as principal constituent
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
    • H01L2224/83—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a layer connector
    • H01L2224/838—Bonding techniques
    • H01L2224/8384—Sintering
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
    • H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L24/02—Bonding areas ; Manufacturing methods related thereto
    • H01L24/04—Structure, shape, material or disposition of the bonding areas prior to the connecting process
    • H01L24/05—Structure, shape, material or disposition of the bonding areas prior to the connecting process of an individual bonding area
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/10—Details of semiconductor or other solid state devices to be connected
    • H01L2924/102—Material of the semiconductor or solid state bodies
    • H01L2924/1025—Semiconducting materials
    • H01L2924/1026—Compound semiconductors
    • H01L2924/1027—IV
    • H01L2924/10272—Silicon Carbide [SiC]
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/30—Technical effects
    • H01L2924/35—Mechanical effects
    • H01L2924/351—Thermal stress
    • H01L2924/3512—Cracking

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Nanotechnology (AREA)
  • Power Engineering (AREA)
  • Computer Hardware Design (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Ceramic Products (AREA)
  • Parts Printed On Printed Circuit Boards (AREA)

Abstract

本發明之課題在於提供一種接合材及使用該接合材將電子零件接合至基板上的接合體，該接合材可藉由即使反覆進行冷熱循環也不易產生大型龜裂的銀接合層，將電子零件接合至基板上。 其解決手段為一種接合體，其係隔著含有銀之燒結體的銀接合層，於銅基板上接合有作為電子零件之(接合面業經銀鍍敷的)SiC晶片等半導體晶片；在前述接合體中，銀接合層之抗剪強度為60MPa以上，且該銀接合層之(111)面的微晶徑為78nm以下。

Description

接合材及使用其之接合體
本發明涉及一種接合材及使用其之接合體，且特別涉及一種由含有銀微粒子之銀糊所構成的接合材，以及藉由使用該接合材所形成之銀接合層於基板上接合有電子零件的接合體。
發明背景 以往，在銅基板等金屬基板上搭載有半導體晶片等電子零件的半導體裝置中，電子零件係利用焊料而被固定在基板上；近年顧及到對人體及環境等所帶來的負擔，逐漸從習知之含鉛焊料轉換至無鉛焊料。
並且，針對這類的半導體裝置之半導體晶片檢討採用比以往廣泛使用之Si晶片損耗更低且具優異特性的SiC晶片。但，在基板上搭載有SiC晶片之半導體裝置有時也會在溫度超過200℃的情況下動作，所以將SiC晶片固定於基板上的焊料就必須使用熔點高的高溫焊料，而這類的高溫焊料很難無鉛化。
另一方面，近年有提議使用含有銀微粒子之銀糊作為接合材，使被接合物間夾著接合材再對被接合物間施加壓力並同時加熱預定時間，使接合材中之銀燒結，藉以透過銀接合層將被接合物彼此接合(譬如參考專利文獻1)。由這種以銀糊構成之接合材形成的銀接合層，熔點比通常的焊料高，所以現有嘗試將之替代焊料來將半導體晶片等電子零件固定於基板上。
先前技術文獻 專利文獻 專利文獻1：日本特開2011-80147號公報(段落編號0014-0020)
發明概要 發明欲解決之課題 但，在基板上搭載有SiC晶片等半導體晶片之半導體裝置中，若使用由銀糊構成之接合材將半導體晶片固定於基板上，在半導體裝置動作時銀接合層會達到超過100℃之高溫，一旦因為反覆半導體裝置之啟動與關閉等而使得冷熱循環或功率循環反覆進行，便可能因半導體晶片或基板與銀接合層之熱膨脹率的不同，於銀接合層上產生巨大的龜裂，造成半導體晶片破損，連帶引發半導體裝置故障。
於是，本發明有鑑於上述習知之問題點，其目的在於提供一種接合材及使用該接合材將電子零件接合至基板的接合體，該接合材可藉由即使反覆進行冷熱循環也不易產生大型龜裂的銀接合層，將電子零件接合至基板上。
用以解決課題之手段 為了解決上述課題，本發明之接合體的特徵在於，隔著含有銀之燒結體的銀接合層於基板上接合有電子零件；在前述接合體中，銀接合層之抗剪強度為60MPa以上且該銀接合層之(111)面的微晶徑為78nm以下。在該接合體中，電子零件之與銀接合層的接合面宜經貴金屬鍍敷，且經銀鍍敷更佳。又，電子零件宜為SiC晶片。另，基板宜為銅基板。
又，本發明之接合材，係由含有銀微粒子之銀糊所構成；其特徵在於：將該接合材塗佈於銅基板上，在大氣環境中施加10MPa之荷重並同時以120秒鐘升溫至280℃後，在280℃下保持180秒鐘進行燒成，使接合材中之銀燒結而形成銀接合層，此時銀接合層之抗剪強度為60MPa以上且該銀接合層之(111)面的微晶徑為78nm以下。在該接合材中，銀微粒子之平均一次粒徑宜為1~100nm。又，該接合材亦可含有平均一次粒徑0.2~10μm的銀粒子。
另，在本說明書中，「平均一次粒徑」意指銀微粒子或銀粒子藉由掃描型電子顯微鏡(SEM)或穿透型電子顯微鏡照片(TEM像)求得之一次粒徑的平均值。
發明效果 根據本發明，可提供一種接合材及使用該接合材將電子零件接合至基板上的接合體，該接合材可藉由即使反覆進行冷熱循環也不易產生大型龜裂的銀接合層，將電子零件接合至基板上。
用以實施發明之形態 本發明之接合體的實施形態如圖1所示，係隔著含有銀之燒結體的銀接合層12，於基板10(理想為銅基板)上接合有電子零件14(理想為SiC晶片等半導體晶片)的接合體，其中，銀接合層之抗剪強度為60MPa以上(宜為70MPa以上，更宜為90~150MPa)，且該銀接合層之(111)面的微晶徑為78nm以下(宜為75nm以下，更宜為45~74nm)。另，電子零件14之接合面宜經金、銀、鈀等貴金屬鍍敷，以提高接合力。
又，本發明之接合材的實施形態係以由含有銀微粒子之銀糊所構成的接合材，將該接合材塗佈於銅基板上，在大氣環境中施加10MPa之荷重並同時以120秒鐘升溫至280℃後，在280℃保持180秒鐘進行燒成，使接合材中之銀燒結而形成銀接合層，此時銀接合層之抗剪強度為60MPa以上(宜為70MPa以上，更宜為90~150MPa)，且該銀接合層之(111)面的微晶徑為78nm以下(宜為75nm以下，更宜為45~74nm)。
如此一來，只要銀接合層之抗剪強度為60MPa以上且該銀接合層之(111)面的微晶徑為78nm以下，即可藉由即使反覆進行冷熱循環也不易產生大型龜裂的銀接合層，將電子零件接合至基板上。
為了提高藉由銀接合層將電子零件等接合至基板時的接合強度(抗剪強度)，宜提高接合時之燒成溫度或拉長燒成時間等以便使銀可充分進行燒結。如此，銀若充分進行燒結，便會在銀接合層與基板之間引發原子擴散，進而提高接合強度。但已知，銀若充分進行燒結，會強烈作用於結晶成長，使銀接合層之微晶徑變大，一旦反覆進行冷熱循環，便容易於銀接合層產生巨大的龜裂。
上述接合材宜連同銀微粒子還含有溶劑及分散劑。
溶劑只要具有可輕易將接合材塗佈於基板上之黏度且可使銀燒結形成銀接合層的溶劑即可，可單獨使用1種溶劑，亦可將2種以上溶劑組合使用。接合材中之溶劑含量宜為1~25質量%，且5~20質量%更佳。該溶劑可使用極性溶劑或非極性溶劑，若從與接合材中之其他成分的相溶性及環境負荷的觀點來看，宜使用極性溶劑。極性溶劑譬如可使用水、醇、多元醇、二元醇醚、1-甲基吡咯啶酮、吡啶、萜品醇、丁卡必醇、丁卡必醇乙酸酯、Texanol、苯氧基丙醇、二乙二醇單丁基醚、二乙二醇單丁基醚乙酸酯、γ-丁內酯、乙二醇單甲基醚乙酸酯、乙二醇單乙基醚乙酸酯、甲氧基丁基乙酸酯、甲氧基丙基乙酸酯、二乙二醇單乙基醚乙酸酯、乳酸乙酯、1-辛醇等。這類的極性溶劑，宜使用1-癸醇、1-十二醇、1-十四醇、3-甲基-1,3-丁二酯3-羥基-3-甲基丁基乙酸酯、2-乙基-1,3-己二醇(辛二醇)、己基二甘醇、2-乙基己基甘醇、二丁基二甘醇、甘油、二羥萜品醇、乙酸二氫䓝烯酯、2-甲基-丁-2,3,4-三醇(異戊二烯三醇A(IPTL-A)、Nippon Terpene Chemicals, Inc.製)、2-甲基-丁-1,3,4-三醇(異戊二烯三醇B(IPTL-B)、Nippon Terpene Chemicals, Inc.製)、TERSOLVE IPG-2Ac(Nippon Terpene Chemicals, Inc.製)、TERSOLVE MTPH(Nippon Terpene Chemicals, Inc.製)、TERSOLVE DTO-210(Nippon Terpene Chemicals, Inc.製)、TERSOLVE THA-90(Nippon Terpene Chemicals, Inc.製)、TERSOLVE THA-70(Nippon Terpene Chemicals, Inc.製)、TERSOLVE TOE-100(Nippon Terpene Chemicals, Inc.製)、二氫䓝烯基氧基乙醇(Nippon Terpene Chemicals, Inc.製)、䓝烯基甲基醚(Nippon Terpene Chemicals, Inc.製)、二氫䓝烯基甲基醚(Nippon Terpene Chemicals, Inc.製)等；更宜使用1-癸醇、1-十二醇、2-乙基1,3-己二醇(辛二醇)、二丁基二甘醇、2-甲基-丁-2,3,4-三醇(異戊二烯三醇A(IPTL-A))及2-甲基-丁-1,3,4-三醇(異戊二烯三醇B(IPTL-B))中之至少一種。
若添加分散劑，可提高接合材中之銀微粒子的分散性，縮小由接合材形成之銀接合層的微晶徑。可單獨使用1種分散劑，亦可將2種以上分散劑組合使用。接合材中之分散劑含量宜為0.01~2質量%，且0.03~0.7質量%更佳。該分散劑可使用丁氧乙氧乙酸等羧酸系分散劑或磷酸酯系分散劑。
要在200~350℃之低溫下將接合材中之銀微粒子加熱使銀燒結而形成高抗剪強度的銀接合層，銀微粒子之平均一次粒徑宜為1~100nm且40~100nm更佳。又，要形成高抗剪強度的銀接合層，接合材中之銀微粒子含量宜為60~97質量%且75~95質量%更佳。而且，為了保持接合材中之銀微粒子的分散狀態，銀微粒子宜被有機化合物被覆。尤其，為了可在燒結銀時從銀微粒子去除而形成高抗剪強度的銀接合層，被覆銀微粒子的有機化合物宜為碳數3~8之脂肪酸或胺。
又，接合材亦可含有平均一次粒徑0.2~10μm且宜為0.2~3μm的銀粒子。這種微米大小的銀粒子若在200~350℃之低溫下將接合材中之銀微粒子加熱，使銀燒結，便可藉由已熔接的銀微粒子彼此連結而以整體形成銀接合層。添加這種微米大小的銀粒子，可高度維持接合材中之銀含量，同時可降低接合材之黏度，製得具有容易塗佈於基板之黏度的接合材。接合材含有微米大小的銀粒子時，接合材中之平均一次粒徑0.2~10μm的銀粒子含量為60質量%以下，且銀微粒子含量與平均一次粒徑0.2~10μm之銀粒子含量合計為61~97質量%為佳。又，為了提高接合材中之充填性，微米大小的銀粒子宜被有機化合物(宜為碳數6~24之脂肪酸或胺)被覆。
另，為了藉由接合材製得抗剪強度高且微晶徑小的銀接合層，宜以濕式噴射磨機將銀微粒子與溶劑等混合而製得的混合物裂解。
為了使用上述接合材製得基板上接合有電子零件之接合體，可將上述接合材塗佈於基板上，形成塗膜，並視需求在70~160℃下加熱5~60分鐘，以使塗膜中之至少一部分溶劑揮發而形成預備乾燥膜後，於塗膜或預備乾燥膜上配置電子零件，在200~350℃下燒成90秒~30分鐘，藉以使塗膜中之銀燒結，形成銀接合層，電子零件便能藉由該銀接合層接合至基板。另，形成預備乾燥膜時的加熱溫度可依溶劑之種類或量來任意設定。又，燒成溫度可在200~350℃之範圍內做調整，不過一旦燒成溫度變高，銀之燒結便會進展而提高銀接合層之抗剪強度，微晶徑也有變大之傾向。此外，燒成時間可在90秒~30分鐘之間做調整，不過燒成時間一旦變長，銀之燒結便會進展而提高銀接合層之抗剪強度，微晶徑也有變大之傾向。此外，在燒成時，宜對電子零件與基板之間施加5~40MPa之荷重。該荷重若變高，有銀接合層之抗剪強度變高、微晶徑變小之傾向。 實施例
以下詳細說明本發明之接合材及使用其之接合體的實施例。
[實施例1] 於300mL燒杯中放入純水180.0g，添加硝酸銀(東洋化學股份有限公司製)33.6g並使其溶解，調製出作為原料液之硝酸銀水溶液。
另於5L燒杯中放入3322.0g之純水，在該純水內噴吹氮氣30分鐘，去除溶氧並同時升溫至40℃。於該純水中添加作為(銀微粒子被覆用)有機化合物之山梨酸(和光純藥工業股份有限公司製)44.8g後，添加28%之氨水(和光純藥工業股份有限公司製)7.1g作為穩定劑。
在攪拌該添加有氨水後之水溶液的同時，從氨水之添加時間點(反應開始時)起算經過5分鐘後，添加純度80%之含水肼(大塚化學股份有限公司製)14.91g作為還原劑，調製出含還原劑之水溶液作為還原液。自反應開始時起算經過9分鐘後，將液溫已調整至40℃之原料液(硝酸銀水溶液)全部加入還原液(含還原劑之水溶液)中使其進行反應，並進一步攪拌80分鐘後，在升溫速度1℃/分鐘下將液溫從40℃升溫至60℃，停止攪拌。
以上述方式形成被山梨酸被覆之銀微粒子的凝聚物後，以No.5C之濾紙過濾含有該銀微粒子之凝聚物的液體，並以純水洗淨經該濾過所得的回收物而獲得銀微粒子之凝聚物。使該銀微粒子之凝聚物在真空乾燥機中於80℃下乾燥12小時後，獲得銀微粒子之凝聚物的乾燥粉末。將以上述方式製得之銀微粒子之凝聚物的乾燥粉末裂解，調整2次凝聚物的大小。另，以掃描型電子顯微鏡(SEM)求算該銀微粒子之平均一次粒徑，得85nm。
接下來，將以上述方式調整2次凝聚物之大小(且被山梨酸被覆)的銀微粒子之凝聚物的乾燥粉末(銀粒子1)89.0g、作為第1溶劑之辛二醇(ODO)(協和發酵化學股份有限公司製2-乙基-1,3-己二醇)9.25g、作為第2溶劑之2-甲基-丁-2,3,4-三醇(異戊二烯三醇A(IPTL-A))(Nippon Terpene Chemicals, Inc.製)1.5g及作為分散劑之2-丁氧乙氧乙酸(BEA)(東京化成工業股份有限公司製)0.25g予以混合。利用捏合脫泡機((股)EME公司製V-mini300型號)，在公轉速度1400rpm、自轉速度700rpm下將該混合物捏合30秒鐘。將該捏合物以混合溶劑(JAPAN ALCOHOL TRADING Co., Ltd.製Solmix AP-7)稀釋攪拌，並利用濕式噴射磨機裝置(Rix Co.製RM-L1000EP)裂解，再以真空攪拌脫泡混合機進行真空脫泡後，使所有的混合溶劑(Solmix AP-7)蒸發而製得由銀糊所構成的接合材1，且該銀糊含有89.0質量%之銀粒子1、9.25質量%之第1溶劑(ODO)、1.5質量%之第2溶劑(IPTL-A)及0.25質量%之分散劑(BEA)。
利用流變儀(黏彈性測定裝置)(Thermo公司製HAAKE Rheostress 600、使用錐形體：C35/2°)，在25℃下測定該接合材1之黏度，以5rpm(15.7[1/S])測定得黏度為36(Pa・s)，並且，在25℃下以1rpm(3.1[1/S])測定之黏度相對於以5rpm測定之黏度之比(1rpm之黏度/5rpm之黏度)(Ti值)為3.1。另，以加熱減量法求算接合材1中之Ag濃度，Ag濃度得88.4質量%。
如以下利用刮板粒度計(BYK公司之50μm不鏽鋼)評估該接合材1(銀糊)中所含銀微粒子之粒度。首先，以酒精溶劑(Solmix)清潔刮板粒度計(grind gauge)並使其充分乾燥後，在刮板粒度計之溝槽較深側(50μm側)放置5~10g左右的銀糊，以兩手拇指及其他手指夾取刮板，並將刮板放置成刮板長邊與刮板粒度計之寬度方向平行且刮板粒度計之溝槽較深側的前端與刀尖接觸，保持刮板與刮板粒度計表面呈垂直，同時在與溝槽長邊呈直角之狀態，以等速度於1~2秒內將刮板粒度計拉至溝深為0處並在拉完後3秒以內，照射光線以利於看清銀糊的模樣，再從相對於溝槽長邊之直角方向且與刮板粒度計表面呈20~30°角度之方向，觀察銀糊上出現明顯線條的部分，沿著溝槽可獲得第1條出現之線條(第1刮痕(1st scratch)、最大粒徑Dmax)及第4條出現之線條(第4刮痕(4th scratch))的粒度，並且取均勻出現10條以上之線條作為平均粒徑D50 之粒度。並且忽視在出現明顯線條之前所顯現的斷斷續續的線條，又由於刮板粒度計左右各1支，所以係以其2支所得數值之平均值為測定結果。其結果，第1刮痕為1μm以下，第4刮痕為1μm以下，平均粒徑D50 為1μm以下。
接下來，於20mm×20mm×2mm之銅基板(C1020)上配置厚120μm之金屬遮罩，使用網板印刷機(Panasonic Factory Solutions Sales & Engineering Japan Co., Ltd.製SP18P-L)，藉由金屬刮刀將上述接合材1在銅基板上塗成10mm×10mm之大小且厚度(印刷膜厚)為105μm。然後，將塗上接合材1之銅基板放置於金屬甕上並設置於烘箱(Yamato Scientific Co., Ltd.製)內，在大氣環境中以118℃加熱14分鐘進行預備乾燥，藉此去除接合材1中之溶劑，形成預備乾燥膜。接著，將形成有預備乾燥膜之銅基板冷卻至25℃後，於預備乾燥膜上配置(於接合面施有銀鍍敷之5mm×5mm×0.3mm大小的)SiC晶片並設置於熱壓機(DOWA Electronics Materials Co., Ltd.製)內，在大氣環境中施加10MPa之荷重並同時在120秒鐘內升溫至280℃，在達280℃後保持180秒鐘進行正式燒成，使接合材1中之銀燒結，形成銀接合層，而製得藉由該銀接合層將(接合面施有銀鍍敷之)SiC晶片接合至銅基板上的接合體1。
針對該接合體1以超音波顯微鏡(C-SAM SONOSCAN公司製)觀察銀接合層有無空隙，結果察無空隙。又，若以接合體1之厚度減去SiC晶片與銅基板之厚度後的厚度作為銀接合層厚度，則銀接合層厚度為46μm。另，將接合體1放入冷熱衝擊裝置(ESPEC Co.製TSA-71H-W)內進行冷熱衝擊試驗，該冷熱衝擊試驗係在大氣環境中於9分鐘內從200℃冷卻至-40℃後再於6分鐘內升溫至200℃為一循環，進行100循環。針對該冷熱衝擊試驗後之接合體1，以超音波顯微鏡(C-SAM SONOSCAN公司製)觀察銀接合層有無空隙，結果於接合體1之銀接合層表面的四隅端部(4個角部)確認了空隙。從該接合體1之銀接合層表面的四隅朝中央部拉4條直線，令該等直線之線段長度為La、於該等直線上存有空隙之長度為Lc、且4個Lc中最大Lc相對於La之比率為龜裂進展率，則龜裂進展率(%)(=Lc×100/La)得17%，接合體1之銀接合層的龜裂進展率低於30%，表示接合體1之銀接合層的接合良好。
又，於10mm×10mm×1mm之銅基板(C1020)上配置厚120μm之金屬遮罩，使用網板印刷機(Panasonic Factory Solutions Sales & Engineering Japan Co., Ltd.製SP18P-L)，藉由金屬刮刀將上述接合材1在銅基板上塗成7mm×7mm之大小且厚度(印刷膜厚)為105μm。然後，將塗上接合材1之銅基板放置於金屬甕上並設置於烘箱(Yamato Scientific Co., Ltd.製)內，在大氣環境中以118℃加熱14分鐘進行預備乾燥，藉此去除接合材1中之溶劑，形成預備乾燥膜。接著，將形成有預備乾燥膜之銅基板冷卻至25℃後，於預備乾燥膜上配置(3mm×3mm×2mm大小的)銅塊並設置於熱壓機(DOWA Electronics Materials Co., Ltd.製)內，在大氣環境中施加10MPa之荷重並同時在120秒鐘內升溫至280℃，在達280℃後保持180秒鐘進行正式燒成，使接合材1中之銀燒結，形成銀接合層，而製得藉由該銀接合層將銅塊接合至銅基板上的接合體2。
根據JIS Z3918-5(2003年)之「無鉛焊料試驗方法-第5部：焊接接頭之拉伸及剪切試驗方法」來測定該接合體2之接合強度。具體上係將接合體2之銅基板予以固定，再將與該銅基板接合之銅塊朝水平方向推壓，並以接合強度試驗機(DAGE公司製萬能型黏結強度試驗機系列4000)測定銅塊與銀接合層之界面、銀接合層內部、及銀接合層與銅基板之界面中之任一者最先破損時之力(N)。在該試驗中，令剪切高度為400μm、剪切速度為5mm/分鐘，並在室溫下進行測定。又，在剪切試驗方法中係直接測定破損時之力(N)，且接合強度為依接合面積決定之值，所以可算出接合面積(3mm×3mm=9mm2 )除以破損時之力(N)之值作為接合強度(平均抗剪強度)。其結果，接合體2之抗剪強度為113MPa，接合強度很高。
又，於20mm×20mm×2mm之銅基板(C1020)上配置厚120μm之金屬遮罩，使用網板印刷機(Panasonic Factory Solutions Sales & Engineering Japan Co., Ltd.製SP18P-L)，藉由金屬刮刀將上述接合材1在銅基板上塗成10mm×10mm之大小且厚度(印刷膜厚)為105μm。然後，將塗上接合材1之銅基板放置於金屬甕上並設置於烘箱(Yamato Scientific Co., Ltd.製)內，在大氣環境中以118℃加熱14分鐘進行預備乾燥，藉此去除接合材1中之溶劑，形成預備乾燥膜。接著，將形成有預備乾燥膜之銅基板冷卻至25℃後，於預備乾燥膜上配置(5mm×5mm×0.3mm大小的)SiC晶片並設置於熱壓機(DOWA Electronics Materials Co., Ltd.製)內，在大氣環境中施加10MPa之荷重並同時在120秒鐘內升溫至280℃，在達280℃後保持180秒鐘進行正式燒成，使接合材1中之銀燒結，形成銀接合層。另，於該銀接合層未接合有(接合面未施加銀鍍敷的)SiC晶片。
針對以上述方式形成之銀接合層，利用X射線繞射裝置((股)Rigaku製RINT-2100型號)，以Co管球(40kV/30mA)作為X射線源，測定40~50°/2θ之範圍，進行X射線繞射(XRD)測定。再從由該X射線繞射測定取得之X射線繞射圖案，利用Scherrer算式(Dhkl=Kλ/βcosθ)求出微晶徑(Dx)。該算式中，Dhkl為微晶徑之大小(與hkl呈垂直方向上的微晶大小)(nm)，λ為測定X射線之波長(nm)(使用Co靶時為0.178892nm)，β為由微晶大小決定之繞射線的寬幅(rad)(以半值寬表示)，θ為繞射角的布拉格角(rad)(入射角與反射角相等時的角度，採用峰頂(peak top)之角度)，K為Scherrer常數(會依D或β之定義等而異，令K=0.94)。又，於計算係採用(111)面之尖峰資料。其結果，微晶徑(Dx)在(111)面為69nm。
[實施例2] 於300mL燒杯中放入純水180.0g，添加硝酸銀(東洋化學股份有限公司製)33.6g並使其溶解，調製出作為原料液之硝酸銀水溶液。
另於5L燒杯中放入3322.0g之純水，在該純水內噴吹氮氣30分鐘，去除溶氧並同時升溫至60℃。於該純水中添加作為(銀微粒子被覆用)有機化合物之山梨酸(和光純藥工業股份有限公司製)44.8g後，添加28%之氨水(和光純藥工業股份有限公司製)7.1g作為穩定劑。
在攪拌添加該氨水後之水溶液的同時，從氨水之添加時間點(反應開始時)起算經過5分鐘後，添加純度80%之含水肼(大塚化學股份有限公司製)14.91g作為還原劑，調製出含還原劑之水溶液作為還原液。自反應開始時起算經過9分鐘後，將液溫已調整至60℃之原料液(硝酸銀水溶液)全部加入還原液(含還原劑之水溶液)中使其反應，並在自反應開始時起算經過25分鐘之時間點結束攪拌。
以上述方式形成被山梨酸被覆之銀微粒子的凝聚物後，以No.5C之濾紙過濾含有該銀微粒子之凝聚物的液體，並以純水洗淨經該濾過所得的回收物而獲得銀微粒子之凝聚物。使該銀微粒子之凝聚物在真空乾燥機中於80℃下乾燥12小時後，獲得銀微粒子之凝聚物的乾燥粉末。將以上述方式製得之銀微粒子之凝聚物的乾燥粉末裂解，調整2次凝聚物的大小。另，以掃描型電子顯微鏡(SEM)求算該銀微粒子之平均一次粒徑，得60nm。
接下來，將以上述方式調整2次凝聚物之大小(且被山梨酸被覆)的銀微粒子之凝聚物的乾燥粉末(銀粒子2)45.0g、平均一次粒徑300nm之銀粒子(DOWA Electronics Materials Co., Ltd.製Ag-2-1C)(銀粒子3)45.0g、作為第1溶劑之辛二醇(ODO)(協和發酵化學股份有限公司製2-乙基-1,3-己二醇)9.25g、作為第2溶劑之2-甲基-丁-2,3,4-三醇(異戊二烯三醇A(IPTL-A))(Nippon Terpene Chemicals, Inc.製)0.5g及作為分散劑之2-丁氧乙氧乙酸(BEA)(東京化成工業股份有限公司製)0.25g予以混合。利用捏合脫泡機((股)EME公司製V-mini300型號)，在公轉速度1400rpm、自轉速度700rpm下將該混合物捏合30秒鐘。將該捏合物以混合溶劑(JAPAN ALCOHOL TRADING Co., Ltd.製Solmix AP-7)稀釋攪拌，並利用濕式噴射磨機裝置(Rix Co.製RM-L1000EP)裂解，再以真空攪拌脫泡混合機進行真空脫泡後，使所有的混合溶劑(Solmix AP-7)蒸發而製得由銀糊所構成的接合材2，且該銀糊含有45.0質量%之銀粒子2、45.0質量%之銀粒子3、9.25質量%之第1溶劑(ODO)、0.5質量%之第2溶劑(IPTL-A)及0.25質量%之分散劑(BEA)。
針對該接合材2，以與實施例1同樣的方法求算黏度、Ti值、Ag濃度及粒度，結果在25℃下以5rpm測定之黏度得6.5(Pa・s)，Ti值為2.5，Ag濃度得89.2質量%。又，第1刮痕為1μm以下，第4刮痕為1μm以下，平均粒徑D50 為1μm以下。
另，使用該接合材2，以與實施例1同樣的方法製作(銅基板上接合有接合面施有銀鍍敷之SiC晶片的)接合體1，並觀察銀接合層有無空隙，求出銀接合層厚度。其結果，於銀接合層未察有空隙，且銀接合層厚度為46μm。又，針對該接合體1，以與實施例1同樣的方法進行冷熱衝擊試驗後，觀察銀接合層有無空隙，並求算銀接合層之龜裂進展率。其結果，於接合體1之銀接合層表面的四隅確認有空隙，龜裂進展率為26%，低於30%，故接合體1之銀接合層的接合良好。
另，使用接合材2，以與實施例1同樣的方法製作(銅基板上接合有銅塊的)接合體2並求算抗剪強度，得78MPa，接合強度很高。又使用接合材2，以與實施例1同樣的方法，試著隔著銀接合層將(接合面未施加銀鍍敷的)SiC晶片與銅基板接合，結果未能於銀接合層接合(接合面未施加銀鍍敷的)SiC晶片。另，針對該銀接合層以與實施例1同樣的方法求算微晶徑(Dx)，結果，(111)面之微晶徑得71nm。
[實施例3] 除了將與實施例2同樣的(平均一次粒徑60nm的)銀微粒子(銀粒子2)、(平均一次粒徑300nm的)銀粒子(銀粒子3)及第1溶劑(ODO)之量分別設為46.5g、46.5g及6.25g以外，以與實施例2同樣的方法製得由銀糊所構成之接合材3，且該銀糊含有46.5質量%之銀粒子2、46.5質量%之銀粒子3、6.25質量%之第1溶劑(ODO)、0.5質量%之第2溶劑(IPTL-A)及0.25質量%之分散劑(BEA)。
針對該接合材3，以與實施例1同樣的方法求算黏度、Ti值、Ag濃度及粒度，結果在25℃下以5rpm測定之黏度得40(Pa・s)，Ti值為5.4，Ag濃度得92.1質量%。又，第1刮痕為1μm以下，第4刮痕為1μm以下，平均粒徑D50 為1μm以下。
另，使用該接合材3，以與實施例1同樣的方法製作(銅基板上接合有接合面施有銀鍍敷之SiC晶片的)接合體1，並觀察銀接合層有無空隙，求出銀接合層厚度。其結果，於銀接合層未察有空隙，且銀接合層厚度為60μm。又，針對該接合體1，以與實施例1同樣的方法進行冷熱衝擊試驗後，觀察銀接合層有無空隙，並求算銀接合層之龜裂進展率。其結果，於接合體1之銀接合層表面的四隅確認有空隙，龜裂進展率為17%，低於30%，故接合體1之銀接合層的接合良好。
另，使用接合材3，以與實施例1同樣的方法製作(銅基板上接合有銅塊的)接合體2並求算抗剪強度，得93MPa，接合強度很高。又使用接合材3，以與實施例1同樣的方法，試著隔著銀接合層將(接合面未施加銀鍍敷的)SiC晶片與銅基板接合，結果未能於銀接合層接合(接合面未施加銀鍍敷的)SiC晶片。另，針對該銀接合層以與實施例1同樣的方法求算微晶徑(Dx)，結果，(111)面之微晶徑得73nm。
[比較例1] 將與實施例1同樣的(平均一次粒徑85nm的)銀微粒子(銀粒子1)82.0g、作為第1溶劑之辛二醇(ODO)(協和發酵化學股份有限公司製2-乙基-1,3-己二醇)11.99g、作為第2溶劑之2-甲基-丁-2,3,4-三醇(異戊二烯三醇A(IPTL-A))(Nippon Terpene Chemicals, Inc.製)6.0g、作為燒結助劑之氧二乙酸(縮二羥乙酸(DGA))(Midori Kagaku Co., Ltd.製)0.01g予以混合。利用捏合脫泡機((股)EME公司製V-mini300型號)將該混合物在公轉速度1400rpm、自轉速度700rpm下捏合30秒鐘後，以三輥機(EXAKT公司製)使其分散後，添加辛二醇(ODO)0.82g作為稀釋溶劑而製得由銀糊所構成之接合材4，且該銀糊含有81.33質量%之銀粒子1、12.71質量%之第1溶劑(ODO)、5.95質量%之第2溶劑(IPTL-A)及0.01質量%之燒結助劑(DGA)。
針對該接合材4，以與實施例1同樣的方法求算黏度、Ti值、Ag濃度及粒度，結果在25℃下以5rpm測定之黏度得25(Pa・s)，Ti值為3.5，Ag濃度得80.2質量%。又，第1刮痕為16μm以下，第4刮痕為10μm以下，平均粒徑D50 為4μm以下。
另，使用該接合材4並將正式燒成時的荷重改為5MPa，除此以外以與實施例1同樣的方法製作(銅基板上接合有接合面施有銀鍍敷之SiC晶片的)接合體1，並觀察銀接合層有無空隙，求出銀接合層厚度。其結果，於銀接合層未察有空隙，且銀接合層厚度為41μm。又，針對該接合體1，以與實施例1同樣的方法進行冷熱衝擊試驗後，觀察銀接合層有無空隙，並求算銀接合層之龜裂進展率。其結果，於接合體1之銀接合層表面的四隅確認有空隙，龜裂進展率為100%，高於30%，故接合體1之銀接合層的接合不佳。
另，使用接合材4並將正式燒成時的荷重改為5MPa，除此以外以與實施例1同樣的方法製作(銅基板上接合有銅塊的)接合體2並求算抗剪強度，得38MPa，接合強度很低。又，使用接合材4並將正式燒成時的荷重改為5.0MPa，除此以外以與實施例1同樣的方法，試著隔著銀接合層將(接合面未施加銀鍍敷的)SiC晶片與銅基板接合，結果未能於銀接合層接合(接合面未施加銀鍍敷的)SiC晶片。另，針對該銀接合層以與實施例1同樣的方法求算微晶徑(Dx)，結果，(111)面之微晶徑得98nm。
[比較例2] 使用與比較例1同樣的接合材4，以與實施例1同樣的方法製作(銅基板上接合有接合面施有銀鍍敷之SiC晶片的)接合體1，並觀察銀接合層有無空隙，求出銀接合層厚度。其結果，於銀接合層未察有空隙，且銀接合層厚度為37μm。又，針對該接合體1，以與實施例1同樣的方法進行冷熱衝擊試驗後，觀察銀接合層有無空隙，並求算銀接合層之龜裂進展率。其結果，於接合體1之銀接合層表面的四隅確認有空隙，龜裂進展率為79%，高於30%，故接合體1之銀接合層的接合不佳。
另，使用接合材4，以與實施例1同樣的方法製作(銅基板上接合有銅塊的)接合體2並求算抗剪強度，得28MPa，接合強度很低。又使用接合材4，以與實施例1同樣的方法，試著隔著銀接合層將(接合面未施加銀鍍敷的)SiC晶片與銅基板接合，結果未能於銀接合層接合(接合面未施加銀鍍敷的)SiC晶片。另，針對該銀接合層以與實施例1同樣的方法求算微晶徑(Dx)，結果，(111)面之微晶徑得84nm。
[比較例3] 使用與比較例1同樣的接合材4並將正式燒成時的荷重改為15MPa，除此以外以與實施例1同樣的方法製作(銅基板上接合有接合面施有銀鍍敷之SiC晶片的)接合體1，並觀察銀接合層有無空隙，求出銀接合層厚度。其結果，於銀接合層未察有空隙，且銀接合層厚度為36μm。又，針對該接合體1，以與實施例1同樣的方法進行冷熱衝擊試驗後，觀察銀接合層有無空隙，並求算銀接合層之龜裂進展率。其結果，於接合體1之銀接合層表面的四隅確認有空隙，龜裂進展率為57%，高於30%，故接合體1之銀接合層的接合不佳。
另，使用接合材4並將正式燒成時的荷重改為15MPa，除此以外以與實施例1同樣的方法製作(銅基板上接合有銅塊的)接合體2並求算抗剪強度，得49MPa，接合強度很低。又，使用接合材4並將正式燒成時的荷重改為15MPa，除此以外以與實施例1同樣的方法，試著隔著銀接合層將(接合面未施加銀鍍敷的)SiC晶片與銅基板接合，結果未能於銀接合層接合(接合面未施加銀鍍敷的)SiC晶片。另，針對該銀接合層以與實施例1同樣的方法求算微晶徑(Dx)，結果，(111)面之微晶徑得75nm。
[比較例4] 使用與比較例1同樣的接合材4並將正式燒成時的荷重改為30MPa，除此以外以與實施例1同樣的方法製作(銅基板上接合有接合面施有銀鍍敷之SiC晶片的)接合體1，並觀察銀接合層有無空隙，求出銀接合層厚度。其結果，於銀接合層未察有空隙，且銀接合層厚度為33μm。又，針對該接合體1，以與實施例1同樣的方法進行冷熱衝擊試驗後，觀察銀接合層有無空隙，並求算銀接合層之龜裂進展率。其結果，於接合體1之銀接合層表面的四隅確認有空隙，龜裂進展率為38%，高於30%，故接合體1之銀接合層的接合不佳。
另，使用接合材4並將正式燒成時的荷重改為30MPa，除此以外以與實施例1同樣的方法製作(銅基板上接合有銅塊的)接合體2並求算抗剪強度，得133MPa，接合強度很高。又，使用接合材4並將正式燒成時的荷重改為30MPa，除此以外以與實施例1同樣的方法，試著隔著銀接合層將(接合面未施加銀鍍敷的)SiC晶片與銅基板接合，結果未能於銀接合層接合(接合面未施加銀鍍敷的)SiC晶片。另，針對該銀接合層以與實施例1同樣的方法求算微晶徑(Dx)，結果，(111)面之微晶徑得80nm。
[比較例5] 使用與實施例2同樣的(平均一次粒徑60nm的)銀微粒子(銀粒子2)來替代換掉與實施例1同樣的(平均一次粒徑85nm的)銀微粒子(銀粒子1)，並將作為稀釋溶劑所添加之辛二醇(ODO)之量改為0.56g，除此以外以與比較例1同樣的方法製得由銀糊所構成之接合材5，且該銀糊含有81.54質量%之銀粒子2、12.48質量%之第1溶劑(ODO)、5.97質量%之第2溶劑(IPTL-A)及0.01質量%之燒結助劑(DGA)。
針對該接合材5，以與實施例1同樣的方法求算黏度、Ti值、Ag濃度及粒度，結果在25℃下以5rpm測定之黏度得38(Pa・s)，Ti值為4.2，Ag濃度得80.0質量%。又，第1刮痕為15μm以下，第4刮痕為11μm以下，平均粒徑D50 為6μm以下。
另，使用該接合材5並將正式燒成時的荷重改為5MPa，除此以外以與實施例1同樣的方法製作(銅基板上接合有接合面施有銀鍍敷之SiC晶片的)接合體1，並觀察銀接合層有無空隙，求出銀接合層厚度。其結果，於銀接合層未察有空隙，且銀接合層厚度為33μm。又，針對該接合體1，以與實施例1同樣的方法進行冷熱衝擊試驗後，觀察銀接合層有無空隙，並求算銀接合層之龜裂進展率。其結果，於接合體1之銀接合層表面的四隅確認有空隙，龜裂進展率為100%，高於30%，故接合體1之銀接合層的接合不佳。
另，使用接合材5並將正式燒成時的荷重改為5MPa，除此以外以與實施例1同樣的方法製作(銅基板上接合有銅塊的)接合體2並求算抗剪強度，得31MPa，接合強度很低。又，使用接合材5並將正式燒成時的荷重改為5MPa，除此以外以與實施例1同樣的方法，試著隔著銀接合層將(接合面未施加銀鍍敷的)SiC晶片與銅基板接合，結果未能於銀接合層接合(接合面未施加銀鍍敷的)SiC晶片。另，針對該銀接合層以與實施例1同樣的方法求算微晶徑(Dx)，結果，(111)面之微晶徑得68nm。
[比較例6] 使用與比較例5同樣的接合材5並將正式燒成時的荷重改為30MPa，除此以外以與實施例1同樣的方法製作(銅基板上接合有接合面施有銀鍍敷之SiC晶片的)接合體1，並觀察銀接合層有無空隙，求出銀接合層厚度。其結果，於銀接合層未察有空隙，且銀接合層厚度為34μm。又，針對該接合體1，以與實施例1同樣的方法進行冷熱衝擊試驗後，觀察銀接合層有無空隙，並求算銀接合層之龜裂進展率。其結果，於接合體1之銀接合層表面的四隅確認有空隙，龜裂進展率為53%，高於30%，故接合體1之銀接合層的接合不佳。
另，使用接合材5並將正式燒成時的荷重改為30MPa，除此以外以與實施例1同樣的方法製作(銅基板上接合有銅塊的)接合體2並求算抗剪強度，得128MPa，接合強度很高。又，使用接合材5並將正式燒成時的荷重改為30MPa，除此以外以與實施例1同樣的方法，試著隔著銀接合層將(接合面未施加銀鍍敷的)SiC晶片與銅基板接合，結果未能於銀接合層接合(接合面未施加銀鍍敷的)SiC晶片。另，針對該銀接合層以與實施例1同樣的方法求算微晶徑(Dx)，結果，(111)面之微晶徑得84nm。
[比較例7] 使用與實施例1同樣的(平均一次粒徑85nm的)銀微粒子(銀粒子1)41.0g及與實施例2同樣的(平均一次粒徑60nm的)銀微粒子(銀粒子2)41.0g，來替代與實施例1同樣的(平均一次粒徑85nm的)銀微粒子(銀粒子1)82.0g，並將作為稀釋溶劑所添加之辛二醇(ODO)之量改為1.13g，除此以外以與比較例1同樣的方法製得由銀糊所構成之接合材6，且該銀糊含有40.54質量%之銀粒子1、40.54質量%之銀粒子2、12.98質量%之第1溶劑(ODO)、5.93質量%之第2溶劑(IPTL-A)及0.01質量%之燒結助劑(DGA)。
針對該接合材6，以與實施例1同樣的方法求算黏度、Ti值、Ag濃度及粒度，結果在25℃下以5rpm測定之黏度得29(Pa・s)，Ti值為3.7，Ag濃度得80.1質量%。又，第1刮痕為20μm以下，第4刮痕為14μm以下，平均粒徑D50 為6μm以下。
另，使用該接合材6，以與實施例1同樣的方法製作(銅基板上接合有接合面施有銀鍍敷之SiC晶片的)接合體1，並觀察銀接合層有無空隙，求出銀接合層厚度。其結果，於銀接合層未察有空隙，且銀接合層厚度為38μm。又，針對該接合體1，以與實施例1同樣的方法進行冷熱衝擊試驗後，觀察銀接合層有無空隙，並求算銀接合層之龜裂進展率。其結果，於接合體1之銀接合層表面的四隅確認有空隙，龜裂進展率為93%，高於30%，故接合體1之銀接合層的接合不佳。
另，使用接合材6，以與實施例1同樣的方法製作(銅基板上接合有銅塊的)接合體2並求算抗剪強度，得32MPa，接合強度很低。又使用接合材6，以與實施例1同樣的方法，試著隔著銀接合層將(接合面未施加銀鍍敷的)SiC晶片與銅基板接合，結果未能於銀接合層接合(接合面未施加銀鍍敷的)SiC晶片。另，針對該銀接合層以與實施例1同樣的方法求算微晶徑(Dx)，結果，(111)面之微晶徑得86nm。
該等實施例及比較例之結果列於表1~表3。
[表1]
[表2]
[表3]
如從表1~表3可知，如同實施例1~3之接合體，只要銀接合層之抗剪強度為60MPa以上且該銀接合層之(111)面的微晶徑為78nm以下，即可藉由即使反覆進行冷熱循環也不易產生大型龜裂的銀接合層，將電子零件接合至基板上。另從比較例1~4之比較可知，如果提高接合時的壓力，銀接合層厚度會變薄、抗剪強度提高，但銀接合層之(111)面的微晶徑會變得大於78nm，且龜裂進展率高過30%。而且如比較例1~7可知，若於接合材添加燒結助劑作為添加劑，可促進燒結並提高銀接合層之抗剪強度，但銀接合層之(111)面的微晶徑會變得大於78nm，且龜裂進展率高過30%。又如從比較例1及比較例5之比較可知，若縮小接合材之銀微粒子的粒徑，銀接合層之抗剪強度雖會變高，但銀接合層之(111)面的微晶徑會變得大於78nm，且龜裂進展率高過30%。
10‧‧‧基板
12‧‧‧銀接合層
14‧‧‧電子零件
圖1係概略顯示本發明之接合體之實施形態一例，即隔著銀接合層將電子零件接合至基板上之接合體的截面圖。

Claims (8)

  1. 一種接合體，其特徵在於：隔著含有銀之燒結體的銀接合層於基板上接合有電子零件；在前述接合體中，銀接合層之抗剪強度為60MPa以上且該銀接合層之(111)面的微晶徑為78nm以下。
  2. 如請求項1之接合體，其中前述電子零件之與銀接合層的接合面業經貴金屬鍍敷。
  3. 如請求項1之接合體，其中前述電子零件之與銀接合層的接合面業經銀鍍敷。
  4. 如請求項1之接合體，其中前述電子零件為SiC晶片。
  5. 如請求項1之接合體，其中前述基板為銅基板。
  6. 一種接合材，係由含有銀微粒子之銀糊所構成；其特徵在於：將該接合材塗佈於銅基板上，在大氣環境中施加10MPa之荷重並同時以120秒鐘升溫至280℃後，在280℃下保持180秒鐘進行燒成，使接合材中之銀燒結而形成銀接合層，此時銀接合層之抗剪強度為60MPa以上且該銀接合層之(111)面的微晶徑為78nm以下。
  7. 如請求項6之接合材，其中前述銀微粒子之平均一次粒徑為1~100nm。
  8. 如請求項6之接合材，其中前述接合材含有平均一次粒徑0.2~10μm的銀粒子。
TW107110271A 2017-03-28 2018-03-26 接合材及使用其之接合體 TW201840416A (zh)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2017063351A JP2018165387A (ja) 2017-03-28 2017-03-28 接合材およびそれを用いた接合体
JP2017-063351 2017-03-28

Publications (1)

Publication Number Publication Date
TW201840416A true TW201840416A (zh) 2018-11-16

Family

ID=63675645

Family Applications (1)

Application Number Title Priority Date Filing Date
TW107110271A TW201840416A (zh) 2017-03-28 2018-03-26 接合材及使用其之接合體

Country Status (7)

Country Link
US (1) US20200035637A1 (zh)
EP (1) EP3590633A4 (zh)
JP (1) JP2018165387A (zh)
KR (1) KR20190128714A (zh)
CN (1) CN110582362A (zh)
TW (1) TW201840416A (zh)
WO (1) WO2018181083A1 (zh)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7249759B2 (ja) * 2018-11-08 2023-03-31 日本特殊陶業株式会社 接合体
CN109979828A (zh) * 2019-04-10 2019-07-05 重庆三峡学院 一种碳化硅功率器件芯片键合方法
US11938543B2 (en) * 2021-04-09 2024-03-26 Heraeus Deutschland GmbH & Co. KG Silver sintering preparation and the use thereof for the connecting of electronic components
CN115846656B (zh) * 2022-12-08 2024-08-06 河南科技大学 一种碳化硅颗粒的预处理方法、碳化硅颗粒增强铝基复合材料及其制备方法

Family Cites Families (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5502434B2 (ja) * 2008-11-26 2014-05-28 三ツ星ベルト株式会社 無機素材用接合剤及び無機素材の接合体
KR101623449B1 (ko) * 2009-07-14 2016-05-23 도와 일렉트로닉스 가부시키가이샤 금속 나노 입자를 이용한 접합재 및 접합 방법
JP5824201B2 (ja) 2009-09-11 2015-11-25 Ｄｏｗａエレクトロニクス株式会社 接合材およびそれを用いた接合方法
KR101664991B1 (ko) * 2010-03-15 2016-10-11 도와 일렉트로닉스 가부시키가이샤 접합재 및 이것을 이용한 접합방법
JP4928639B2 (ja) * 2010-03-15 2012-05-09 Ｄｏｗａエレクトロニクス株式会社 接合材およびそれを用いた接合方法
WO2011155055A1 (ja) * 2010-06-11 2011-12-15 Ｄｏｗａエレクトロニクス株式会社 低温焼結性接合材および該接合材を用いた接合方法
KR20130129392A (ko) * 2010-11-22 2013-11-28 도와 일렉트로닉스 가부시키가이샤 접합재료, 접합체, 및 접합방법
KR101725181B1 (ko) * 2011-06-10 2017-04-10 도와 일렉트로닉스 가부시키가이샤 접합재 및 이것을 이용하여 작성된 접합체
WO2013018645A1 (ja) * 2011-07-29 2013-02-07 戸田工業株式会社 銀微粒子並びに該銀微粒子を含有する導電性ペースト、導電性膜及び電子デバイス
KR101609497B1 (ko) * 2012-01-20 2016-04-05 도와 일렉트로닉스 가부시키가이샤 접합재 및 그것을 이용한 접합 방법
TWI455264B (zh) * 2012-02-04 2014-10-01 Lextar Electronics Corp 晶片接合結構及晶片接合的方法
JP6216709B2 (ja) * 2012-03-05 2017-10-18 ナミックス株式会社 銀微粒子焼結体
JP6087425B2 (ja) * 2013-05-08 2017-03-01 国立大学法人大阪大学 接合方法
JP6118192B2 (ja) * 2013-06-21 2017-04-19 Ｄｏｗａエレクトロニクス株式会社 接合材およびそれを用いた接合方法
JP6171645B2 (ja) * 2013-07-12 2017-08-02 ヤマハ株式会社 熱電変換モジュール
JP5992961B2 (ja) * 2014-06-25 2016-09-14 Ｄｏｗａエレクトロニクス株式会社 接合材およびそれを用いた接合方法
JP2017052668A (ja) * 2015-09-09 2017-03-16 三菱マテリアル株式会社 組成物、接合体の製造方法

Also Published As

Publication number Publication date
JP2018165387A (ja) 2018-10-25
CN110582362A (zh) 2019-12-17
EP3590633A4 (en) 2020-12-02
US20200035637A1 (en) 2020-01-30
WO2018181083A1 (ja) 2018-10-04
EP3590633A1 (en) 2020-01-08
KR20190128714A (ko) 2019-11-18

Similar Documents

Publication Publication Date Title
TW201840416A (zh) 接合材及使用其之接合體
CN109789482B (zh) 接合材料及使用该接合材料的接合方法
JP6884285B2 (ja) 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
JP5416153B2 (ja) 導電性ペースト、及びその製造方法、並びに導電接続部材
KR101800155B1 (ko) 접합재 및 그것을 사용한 접합 방법
JP6423416B2 (ja) 焼結が難しい貴金属表面および非貴金属表面上に酸化銀が被覆された焼結ペースト
JP6900150B2 (ja) 接合材およびそれを用いた接合方法
CN109074897B (zh) 接合材料及使用该接合材料的接合方法
JP6561100B2 (ja) 表面処理銅微粒子の製造方法
KR20190103155A (ko) 접합재 및 이것을 이용한 접합 방법
JP6662619B2 (ja) 接合材およびそれを用いた接合方法
KR102354209B1 (ko) 접합재 및 그것을 사용한 접합 방법
KR102359193B1 (ko) 접합재 및 그것을 사용한 접합 방법
WO2021039874A1 (ja) 低温焼結性接合ペースト及び接合構造体
JP2021138991A (ja) 接合材、接合材の製造方法及び接合方法
JP2020164895A (ja) 接合材及び接合方法
WO2017188206A1 (ja) 接合材およびそれを用いた接合方法
JP7487011B2 (ja) 接合材、接合材の製造方法及び接合方法
Maeda et al. Low-temperature metal–metal bonding process using leaf-like aggregates composed of CuO nanoparticles
TW202339873A (zh) 銀微粒子組成物