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WO2015060245A1 - Pâte d'argent et dispositif à semi-conducteur utilisant cette dernière et procédé de production pour pâte d'argent - Google Patents

Pâte d'argent et dispositif à semi-conducteur utilisant cette dernière et procédé de production pour pâte d'argent Download PDF

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Publication number
WO2015060245A1
WO2015060245A1 PCT/JP2014/077830 JP2014077830W WO2015060245A1 WO 2015060245 A1 WO2015060245 A1 WO 2015060245A1 JP 2014077830 W JP2014077830 W JP 2014077830W WO 2015060245 A1 WO2015060245 A1 WO 2015060245A1
Authority
WO
WIPO (PCT)
Prior art keywords
silver
silver particles
silver paste
paste
protective agent
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/JP2014/077830
Other languages
English (en)
Japanese (ja)
Inventor
石川　大
松本　博
名取　美智子
偉夫 中子
田中　俊明
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Resonac Corp
Original Assignee
Hitachi Chemical Co Ltd
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 Hitachi Chemical Co Ltd filed Critical Hitachi Chemical Co Ltd
Publication of WO2015060245A1 publication Critical patent/WO2015060245A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • 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
    • B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • H10W72/013—
    • H10W72/07331—
    • H10W72/325—
    • H10W72/352—
    • H10W72/884—
    • H10W74/00—
    • H10W90/736—
    • H10W90/756—

Definitions

  • the semiconductor element is die-bonded and bonded by heat curing to obtain a semiconductor device.
  • a method is mentioned.
  • the characteristics required for the silver paste are broadly classified into the contents relating to the construction method at the time of bonding and the contents relating to the physical properties of the silver sintered body after bonding.
  • the silver particles having a particle diameter of 1 ⁇ m to 20 ⁇ m are desirably plate-like silver particles or a mixture of plate-like silver particles and spherical silver particles.
  • the present invention is also a method for producing a silver paste, wherein a silver paste is obtained by mixing silver particles and a solvent, wherein the silver particles have a particle diameter of 1 ⁇ m to 20 ⁇ m and a boiling point under atmospheric pressure.
  • a method for producing a silver paste using silver particles coated with a protective agent having a temperature of less than 130 ° C. and having a particle diameter of 1 nm to 300 nm.
  • 4 is a TG-DTA measurement result of the silver nanoparticles of Comparative Example 1.
  • 4 is a SEM photograph of a connection cross section of a semiconductor member of Comparative Example 1.
  • 4 is a SEM photograph of a connection cross section of a semiconductor member of Comparative Example 2.
  • 10 is a SEM photograph of a connection cross section of a semiconductor member of Comparative Example 3.
  • the silver paste according to this embodiment is a silver paste containing silver particles and a solvent, and the silver particles are silver particles having a particle diameter of 1 ⁇ m to 20 ⁇ m, and a protective material having a boiling point of less than 130 ° C. under atmospheric pressure. And silver particles having a particle diameter of 1 nm to 300 nm coated with an agent.
  • the silver particles used in the present embodiment are particles coated with silver particles having a particle diameter of 1 ⁇ m to 20 ⁇ m (hereinafter “silver microparticles”) and a protective agent having a boiling point of less than 130 ° C. under atmospheric pressure. Silver particles having a diameter of 1 nm to 300 nm (hereinafter “silver nanoparticles”).
  • the shape of the silver microparticle and the silver nanoparticle is not particularly limited, and a shape that increases the filling property when the silver microparticle and the silver nanoparticle are mixed may be used as appropriate.
  • plate-like silver particles, spherical silver particles, a mixture thereof, and the like can be used as appropriate.
  • a silver microparticle and a silver nanoparticle both a single crystal and a polycrystal can be used.
  • the desorption temperature of the protective agent for silver microparticles and silver nanoparticles is preferably 300 ° C. or lower, and 250 ° C. The following is more desirable.
  • the protective agent for silver nanoparticles is an organic compound having a boiling point of less than 130 ° C., desirably an organic compound having a boiling point of 120 ° C. or less, more desirably an organic compound having a boiling point of 110 ° C. or less.
  • the lower limit of the boiling point of the protective agent is not particularly limited, but is, for example, 70 ° C. or higher.
  • the boiling point in this specification means the boiling point under atmospheric pressure (1013 hPa).
  • the mass ratio can be obtained from the mass change before and after the measurement by heating the silver nanoparticles or silver microparticles to a temperature at which the desorption of the protective agent is sufficiently performed.
  • Example 1 silver nanoparticles coated with N, N-dimethylethylenediamine (Tokyo Chemical Industry Co., Ltd., boiling point 107 ° C.) as a protective agent, and silver microparticles (AgC239 (AgC239) coated with dodecanoic acid as a protective agent Fukuda Metal Foil Co., Ltd.)) is used in combination.
  • TG-DTA measurement results of silver nanoparticles and silver microparticles are shown in FIGS. 1 and 2, respectively.
  • FIG. 1 shows that N, N-dimethylethylenediamine on the surface of the silver nanoparticles is desorbed at about 225.degree.
  • FIG. 2 shows that dodecanoic acid on the surface of the silver microparticles is desorbed at about 250 ° C.
  • FIG. 3 shows the results of TG-DTA measurement of a silver paste prepared by mixing these silver particles.
  • the temperature at which the desorption of the organic substance from the silver paste is completed is about 250 ° C., and the weight loss is about 9.5% by weight.
  • the desorption temperature of the organic substance in TG-DTA measurement is 250 ° C., but if it is heated to some degree even at about 200 ° C., the same weight loss (9.5% by weight) as when heated at 250 ° C. is obtained.
  • the silver paste of Example 1 can be sintered at about 200 ° C. with the organic matter completely removed. Also, since the difference in desorption temperature between the protective agent for silver nanoparticles and the protective agent for silver microparticles is as small as 25 ° C., the silver nanoparticles and the silver microparticles can be sintered almost simultaneously, and a dense silver sintered body Can be formed. As a result, the characteristics (die shear strength, volume resistivity and thermal conductivity) of the silver sintered body are also good.
  • the solvent in this embodiment is not particularly limited as long as it is liquid at normal temperature (20 ° C.), and a known solvent can be used.
  • Solvents can be selected from alcohols, aldehydes, carboxylic acids, ethers, esters, amines, monosaccharides, polysaccharides, linear hydrocarbons, fatty acids, aromatics, etc. It is also possible to use a combination of a plurality of the above solvents.
  • the boiling point of the solvent is not particularly limited, but is preferably 100 ° C to 350 ° C, more preferably 130 ° C to 300 ° C, and further preferably 150 ° C to 250 ° C.
  • the boiling point of the solvent is 100 ° C. or higher, it is possible to prevent the solvent from volatilizing at room temperature when the silver paste is used, and as a result, it is possible to ensure the viscosity stability, applicability, and the like of the silver paste.
  • the boiling point of the solvent is 350 ° C. or less, it is possible to suppress the solvent from being evaporated in the silver sintered body at a temperature at which the semiconductor element is connected to the support member. The characteristics can be kept better.
  • silver nanoparticles, silver microparticles, and a solvent are collectively or divided into a stirrer, a separator, What is necessary is just to combine dispersion
  • the method for heating and sintering the silver paste a known method can be used. In addition to external heating by a heater, an ultraviolet lamp, laser, microwave, or the like can be suitably used.
  • the heating temperature of the silver paste is preferably equal to or higher than the temperature at which the protective agent, solvent and additive are desorbed from the system. Specifically, the range of the heating temperature is desirably 150 ° C. or more and 300 ° C. or less, and more desirably 150 ° C. or more and 250 ° C. or less.
  • a general semiconductor member is connected by setting the heating temperature to 300 ° C. or lower, damage to the member can be avoided, and by setting the heating temperature to 150 ° C. or higher, Desorption is likely to occur.
  • the process for heating the silver paste can be appropriately determined.
  • sintering is performed at a temperature exceeding the boiling point of the solvent, pre-heating at a temperature lower than the boiling point of the solvent, and after performing the sintering after volatilizing the solvent to some extent, a denser silver sintered body Easy to get.
  • the rate of temperature increase when heating the silver paste is not particularly limited when sintering is performed below the boiling point of the solvent. In the case of sintering at a temperature exceeding the boiling point of the solvent, it is desirable to set the heating rate to 1 ° C./second or less, or to perform a preheating step.
  • AgC239 (Fukuda Metal Foil Co., Ltd.) was used as the silver microparticles.
  • the treatment for coating AgC239 with dodecanoic acid as a protective agent was performed as follows. That is, first, 100 g of AgC239, 10 g of dodecanoic acid (Wako Pure Chemical Industries, Ltd., boiling point 299 ° C.) and 500 mL of 1-propanol (Wako Pure Chemical Industries, Ltd., boiling point 97 ° C.) were added to the eggplant flask. did. The reaction solution was reacted by heating at 60 ° C. for 3 hours while stirring at about 200 rpm with a magnetic stirrer.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Dispersion Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Conductive Materials (AREA)
  • Manufacturing Of Printed Wiring (AREA)
  • Die Bonding (AREA)

Abstract

La présente invention porte sur une pâte d'argent qui est une pâte d'argent qui contient des particules d'argent et un solvant. Les particules d'argent contiennent des particules d'argent ayant un diamètre de particule de 1-20 μm et des particules d'argent ayant un diamètre de particule de 1-300 nm et qui sont recouvertes d'un agent protecteur qui a un point d'ébullition inférieur à 130 °C sous pression atmosphérique.
PCT/JP2014/077830 2013-10-22 2014-10-20 Pâte d'argent et dispositif à semi-conducteur utilisant cette dernière et procédé de production pour pâte d'argent Ceased WO2015060245A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2013219283A JP6303392B2 (ja) 2013-10-22 2013-10-22 銀ペースト及びそれを用いた半導体装置、並びに銀ペーストの製造方法
JP2013-219283 2013-10-22

Publications (1)

Publication Number Publication Date
WO2015060245A1 true WO2015060245A1 (fr) 2015-04-30

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PCT/JP2014/077830 Ceased WO2015060245A1 (fr) 2013-10-22 2014-10-20 Pâte d'argent et dispositif à semi-conducteur utilisant cette dernière et procédé de production pour pâte d'argent

Country Status (3)

Country Link
JP (1) JP6303392B2 (fr)
TW (1) TWI636514B (fr)
WO (1) WO2015060245A1 (fr)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018049735A (ja) * 2016-09-21 2018-03-29 矢崎総業株式会社 導電性ペースト及びそれを用いた配線板
CN110213883A (zh) * 2019-06-28 2019-09-06 智玻蓝新科技(武汉)有限公司 一种玻璃基电路板导电线路制备工艺
CN111230125A (zh) * 2015-09-07 2020-06-05 日立化成株式会社 接合用铜糊料、接合体的制造方法及半导体装置的制造方法
CN111360270A (zh) * 2015-09-07 2020-07-03 日立化成株式会社 接合体及半导体装置
CN114206526A (zh) * 2019-09-02 2022-03-18 株式会社大阪曹達 银颗粒
US11515280B2 (en) * 2018-04-12 2022-11-29 Panasonic Intellectual Property Management Co., Ltd. Mounting structure and nanoparticle mounting material
CN118248574A (zh) * 2024-05-29 2024-06-25 诚联恺达科技有限公司 一种纳米级银烧结方法、芯片及焊接设备

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SG11201801847SA (en) * 2015-09-07 2018-04-27 Hitachi Chemical Co Ltd Copper paste for joining, method for producing joined body, and method for producing semiconductor device
JP6509770B2 (ja) * 2016-03-31 2019-05-08 Ｊｘ金属株式会社 導電性金属粉ペースト
SG11201906411TA (en) 2017-01-11 2019-08-27 Hitachi Chemical Co Ltd Copper paste for pressureless bonding, bonded body and semiconductor device
JP6624620B1 (ja) * 2018-12-03 2019-12-25 ニホンハンダ株式会社 ペースト状銀粒子組成物、金属製部材接合体の製造方法および金属製部材接合体
CN112935240A (zh) * 2021-01-20 2021-06-11 深圳市先进连接科技有限公司 微纳米复合银膏及其制备方法和气密性器件的封装方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002035554A1 (fr) * 2000-10-25 2002-05-02 Harima Chemicals, Inc. Pate metallique electro-conductrice et procede de production de cette pate
JP2008091250A (ja) * 2006-10-03 2008-04-17 Mitsuboshi Belting Ltd 低温焼成型銀ペースト
JP2012052198A (ja) * 2010-09-02 2012-03-15 Nippon Handa Kk ペースト状銀粒子組成物、金属製部材接合体の製造方法および金属製部材接合体

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6001861B2 (ja) * 2012-01-11 2016-10-05 株式会社ダイセル 銀ナノ粒子の製造方法及び銀ナノ粒子、並びに銀塗料組成物
JP6081231B2 (ja) * 2012-03-05 2017-02-15 ナミックス株式会社 熱伝導性ペースト及びその使用

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002035554A1 (fr) * 2000-10-25 2002-05-02 Harima Chemicals, Inc. Pate metallique electro-conductrice et procede de production de cette pate
JP2008091250A (ja) * 2006-10-03 2008-04-17 Mitsuboshi Belting Ltd 低温焼成型銀ペースト
JP2012052198A (ja) * 2010-09-02 2012-03-15 Nippon Handa Kk ペースト状銀粒子組成物、金属製部材接合体の製造方法および金属製部材接合体

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111230125A (zh) * 2015-09-07 2020-06-05 日立化成株式会社 接合用铜糊料、接合体的制造方法及半导体装置的制造方法
CN111360270A (zh) * 2015-09-07 2020-07-03 日立化成株式会社 接合体及半导体装置
JP2018049735A (ja) * 2016-09-21 2018-03-29 矢崎総業株式会社 導電性ペースト及びそれを用いた配線板
WO2018055848A1 (fr) * 2016-09-21 2018-03-29 矢崎総業株式会社 Pâte électriquement conductrice et tableau de connexions l'utilisant
US11515280B2 (en) * 2018-04-12 2022-11-29 Panasonic Intellectual Property Management Co., Ltd. Mounting structure and nanoparticle mounting material
CN110213883A (zh) * 2019-06-28 2019-09-06 智玻蓝新科技(武汉)有限公司 一种玻璃基电路板导电线路制备工艺
CN114206526A (zh) * 2019-09-02 2022-03-18 株式会社大阪曹達 银颗粒
CN114206526B (zh) * 2019-09-02 2025-04-15 株式会社大阪曹達 银颗粒
CN118248574A (zh) * 2024-05-29 2024-06-25 诚联恺达科技有限公司 一种纳米级银烧结方法、芯片及焊接设备

Also Published As

Publication number Publication date
JP2015082385A (ja) 2015-04-27
TW201528388A (zh) 2015-07-16
TWI636514B (zh) 2018-09-21
JP6303392B2 (ja) 2018-04-04

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