US20100031848A1 - Alloy nanoparticles of sn-cu-ag, preparation method thereof and ink or paste using the alloy nanoparticles - Google Patents

Alloy nanoparticles of sn-cu-ag, preparation method thereof and ink or paste using the alloy nanoparticles Download PDF

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Publication number
US20100031848A1
US20100031848A1 US12/437,945 US43794509A US2010031848A1 US 20100031848 A1 US20100031848 A1 US 20100031848A1 US 43794509 A US43794509 A US 43794509A US 2010031848 A1 US2010031848 A1 US 2010031848A1
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Prior art keywords
alloy nanoparticles
nanoparticles
salt
alloy
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Abandoned
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US12/437,945
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English (en)
Inventor
Kwi-Jong Lee
Hyuck-Mo Lee
Hyun-Joon Song
Yun-Hwan Jo
Ji-Chan Park
Jung-Up Bang
Dong-Hoon Kim
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Samsung Electro Mechanics Co Ltd
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Samsung Electro Mechanics Co Ltd
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Assigned to SAMSUNG ELECTRO-MECHANICS CO., LTD. reassignment SAMSUNG ELECTRO-MECHANICS CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: LEE, HYUCK-MO, JO, YUN-HWAN, BANG, JUNG-UP, PARK, JI-CHAN, SONG, HYUN-JOON, KIM, DONG-HOON, Lee, Kwi-jong
Publication of US20100031848A1 publication Critical patent/US20100031848A1/en
Priority to US13/495,887 priority Critical patent/US8496873B2/en
Abandoned 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C13/00—Alloys based on tin
    • 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
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/52—Electrically conductive inks
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12708—Sn-base component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12708—Sn-base component
    • Y10T428/12715—Next to Group IB metal-base component

Definitions

  • the present invention relates to Sn—Cu—Ag alloy nanoparticles, a preparation method thereof and ink or paste using the alloy nanoparticles.
  • Nanoparticles which are particles having a particle size of nano scale, exhibit a number of special properties such as optical, electrnic and magnetic propertites that differ significantly from those observed in bulk material due to size-dependent properties such as quantum confinement effect and a very high surface area to volume ratio.
  • Nanoparticle research is currently an area of intense scientific research in catalytic, electronic and magnetic, optical, and medical fields due to such special properties. Nanoparticles are a bridge between bulk materials and molecular structures and preparation of nanoparticles can be classified into two methods, “top-down approach” and “bottom-up approach”.
  • the top-down approach involves the breaking down of bulk materials. It may easily control size of nanoparticles but may be difficult to provide nanoparticles having a size of less than 50 nm.
  • the bottom-up approach which implies assembling single atoms and molecules into larger nanosutructures, has currently more attention and involves generally a colloid liquid phase synthesis when nanoparticles are formed from chemical molecular or atom precursors.
  • Sn—Pb solder materials especially a material having a low melting temperature (m.p. 183° C.) and including 63/37 Sn/Pb, have been generally used to join a substrate and electronic elements of circuit boards embaded in electronic devices.
  • wastes can contain Pb (lead) found in Sn—Pb solder materials and cause environmental pollusion, development on lead-free solder materials has been significantly growing.
  • the Ag—Cu—Sn family among such Pb-free solders has the most promise as the main replacement of Sn—Pb solder.
  • Most of Ag—Cu—Sn solder materials have composition with 95 wt % or less of Sn.
  • the melting temperature is an important factor as the solder material.
  • the invention is to provide a method to increase the content of Sn to lower melting temperature of alloy nanoparticles and at the same time to exhibit electrical conductivity and stability.
  • An aspect of the invention is to provide Sn—Cu—Ag alloy nanoparticles which exhibit good electrical conductivity and low calcinating temperature, a manufacturing method thereof and materials such as ink or paste using the alloy nanoparticles.
  • Another aspect of the invention is to provide alloy nanoparticles including Sn in the range of from more than 95 wt % to 99.9 wt % or less and at least one chosen from the group consisting of Ag and Cu in the range of from 0.1 wt % or more to less than 5 wt %.
  • size of alloy nanoparticles may be in the range of 5 to 300 nm and such alloy nanoparticles have a melting temperature of 150 to 250° C.
  • Another aspect of the invention is to provide ink or paste using the alloy nanoparticles.
  • Another aspect of the invention is to provide a method for manufacturing alloy nanoparticles, the method including: dissolving a Sn salt and a surfactant in a solvent; forming Sn nanoparticles by adding a reducing agent into the solution; and forming Sn—Cu nanoparticles by adding a Cu salt to the solution including the reducing agent.
  • the method may further include forming Sn—Cu—Ag alloy nanoparticles by adding a Ag salt after the Sn—Cu nanoparticles are formed.
  • the solvent may be at least one alcohol chosen from ethylene glycol, diethylene glycol, tetraethylene glycol, and 1-5-pentandiol.
  • the tin salt may be at least one tin salt chosen from Sn(NO 3 ) 2 , SnCl 2 , SnBr 2 , SnI 2 , Sn(OH) 2 , SnSO 4 , Sn(CH 3 COO) 2 , Sn(CH 3 COCHCOCH 3 ) 2 and the like.
  • the forming Sn nanoparticles by adding a reducing agent into the solution may be conducted at a temperature of 100 to 260° C.
  • the forming Sn—Cu alloy nanoparticles by adding a copper salt may be conducted within 3 to 60 mins after the Sn nanoparticles are formed by adding a reducing agent into the solution.
  • the copper salt may be at least one copper salt chosen from Cu(NO 3 ) 2 , CuCl 2 , CuBr 2 , CuI 2 , Cu(OH) 2 , CuSO 4 , Cu(CH 3 COO) 2 , Cu(CH 3 COCHCOCH 3 ) 2 and the like.
  • the copper salt may be added directly to the solution or after it is dissolved in a solvent.
  • the Sn—Cu alloy nanoparticles may include Sn in the range of from more than 95 wt % to 99.9 wt % or less and Cu in the range of from 0.1 wt % or more to less than 5 wt %.
  • a silver salt may be added to provide Sn—Cu—Ag alloy nanoparticles after the Sn—Cu alloy nanoparticles are formed.
  • the silver salt may be at least one silver salt chosen from AgNO 3 , AgCl, AgBr, AgI, AgOH, Ag 2 SO 4 , AgCH 3 COO, AgCH 3 COCHCOCH 3 and the like.
  • the silver salt may be added directly to the solution or after it is dissolved in a solvent.
  • the forming Sn—Cu—Ag alloy nanoparticles by adding a silver salt may be conducted within 3 to 60 mins after the Sn—Cu nanoparticles are formed.
  • the Sn—Cu—Ag alloy nanoparticles may include Sn in the range of from more than 95 wt % to 99.9 wt % or less and Ag and Cu in the range of from 0.1 wt % or more to less than 5 wt %.
  • FIG. 1 is a flow chart illustrating a method of manufacturing alloy nanoparticles according to an embodiment of the invention.
  • FIG. 2 is a flow chart illustrating a method of manufacturing alloy nanoparticles according to another embodiment of the invention.
  • FIG. 3 is a transmission electron microscopy (TEM) result of the alloy nanoparticles according to an embodiment of the invention.
  • FIG. 4 is a differential scanning calorimetry (DSC) analysis result of the alloy nanoparticles according to Example 1.
  • FIG. 5 is a transmission electron microscopy (TEM) result of the alloy nanoparticles according to Example 2.
  • the alloy nanoparticles including 95 wt % or more of Sn and a small amount of Cu and Ag and being suitable for forming metal inks or printed circuit patterns with lower calcinating temperature and having high electrical conductivity, electrical reliability and oxidation resistance, is provided.
  • the alloy nanoparticles including Sn in the range of from more than 95 wt % to 99.9 wt % or less is provided.
  • the melting temperatures of pure Ag, pure Sn, pure Cu is 961° C., 232° C., and 1085° C., respectively.
  • the melting temperature of the alloy nanoparticles cannot be lowered to 250° C. or less and thus, it cannot be used as a solder material since a low melting temperature of 150 to 250° C. is required in order to be used as the solder material.
  • the melting temperature of alloy nanoparticles is higher than 250° C., it may cause thermal deformation of boards.
  • it is lower than 150° C. it may be difficult to remove any organic component in the alloy nanoparticles.
  • size of the alloy nanoparticles may be 1 ⁇ m or less, preferably in the range of 5 nm to 300 nm. Even though alloys have the same composition, their melting temperatures may vary with the particle size. The smaller the particle size is the greater total surface area of particles to volum ratio is. Such result shows significant differences in thermodynamic characteristics. As the particle size gets smaller, surface area per unit volume significantly increases. Thus, energy state of particles becomes unstable so that it may be affected by the surface energy which is high. When particles transform from the solid state to the liquid state, surface area tends to be minimized through rearrangement of surface atoms in the liquid state unlike the solid state. It may lower the surface energy by reducing surface atoms having high energy. Therefore, the liquid state of nanoparticles can be stablized and the melting temperature gets lowered.
  • the alloy nanoparticles of the invention may be used as metal ink or paste and such ink or paste including the alloy nanoparticles may be manufactured by known methods to a person skilled in the art.
  • ink or paste may be manufactured by dispersing alloy nanoparticles including Ag, Cu and Sn in a solvent and adding a dispersing agent and other additives.
  • Such ink or paste may further include a hardening initiator, a hardening accelerator, a coloring agent and the like and further include an additive to control the viscosity.
  • Such hardening agent or hardening accelerator may be water soluble or soluble by adding an emulsifying agent.
  • a method for manufacturing alloy nanoparticles may include dissolving a Sn salt and a surfactant in a solvent (S 101 ), forming Sn nanoparticles by adding a reducing agent into the solution (S 102 ), and forming Sn—Cu alloy nanoparticles by adding a copper salt to the solution including the reducing agent (S 103 ).
  • the method according to another embodiment of the invention may produce Sn—Cu—Ag alloy nanoparticles by further including forming Sn—Cu—Ag alloy nanoparticles by adding a silver salt (S 204 ) after the forming Sn—Cu alloy nanoparticles (S 103 , S 203 ).
  • the metal salt may be added in order according to relative reduction speed of the metal salt.
  • a metal salt having low reduction activity is successively reduced to produce particles having high crystallity.
  • the metal salt having the most reduction activity may be the Sn salt in the alloy nanoparticles manufacturing described above.
  • the Cu salt may be next and the Ag salt is less reductive than the Cu salt. Therefore, the Sn salt, the Cu salt and the Ag salt may be added in order.
  • the Sn salt and a surfactant may be first dissolved in a solvent (S 101 , S 201 ).
  • the surfactant may be added to reduce the surface tension of particles.
  • the surfactant may be an amphiphilic material possessing both hydrophilic and hydrophobic properties in one molecular.
  • the surfactant is classified into anionic, cationic, zwitterionic(dual charge) and non-ionic and examples may include polyvinyl pyrrolidone (PVP), polyethylenimide (PEI), polymethyl vinyl ether (PMVE), polyvinyl alcohol (PVA), polyoxyethylene alkyl phenyl ether, polyoxyethylene sorbitanmonostearate and derivatives thereof, but it is not limited thereto.
  • the surfactant may be added alone or in a combination of 2 or more.
  • the solvent may be any solvent used in the reduction reaction of metal salts without any limitation and examples may include ethylene glycol, di(ethylene) glycol, tetra(ethylene) glycol, and 1,5-pentandiol, etc.
  • the solvent may be added alone or in a combination of 2 or more.
  • Sn salt examples include Sn(NO 3 ) 2 , SnCl 2 , SnBr 2 , SnI 2 , Sn(OH) 2 , SnSO 4 , Sn(CH 3 COO) 2 and Sn(CH 3 COCHCOCH 3 ) 2 , etc. but it is not limited thereto.
  • the Sn salt may be added directly or as a solution dissolved in a solvent.
  • a reducing agent may be added to the result solution to form Sn nanoparticles (S 102 , S 202 ).
  • the reducing agent may be any agent used in the solution phase reduction and known to a person skilled in the art without any limitation. Examples may include a strong reducing agent such as NaBH 4 , NH 2 NH 2 , LiAlH 4 , LiBEt 3 H and the like and a polyol such as ethylene glycol, tri(ethylene) glycol, tetra(ethylene) glycol and the like and an amine.
  • the forming Sn nanoparticles by adding the reducing agent (S 102 ) may be performed at a temperature of 100° C. to 260° C., preferably 150 to 250° C. When the temperature is lower than 100° C., unreacted compounds may be remained. On the other hand when it is higher than 260° C., over growth of particles may occur.
  • the Cu salt may be added to form Sn—Cu alloy nanoparticles (S 103 ).
  • the Cu salt may include Cu(NO 3 ) 2 , CuCl 2 , CuBr 2 , CuI 2 , Cu(OH) 2 , CuSO 4 , Cu(CH 3 COO) 2 and Cu(CH 3 COCHCOCH 3 ) 2 , etc. but it is not limited thereto.
  • the Cu salt may be added directly or as a solution dissolved in a solvent.
  • the forming Sn—Cu alloy nanoparticles may be performed within 3 to 60 min after the Sn nanoparticles are formed. When it is performed later than 60 min, each metal may be formed into its own particles so that uniformed alloy cannot be formed. On the other hand, when it is performed within less than 3 min, the other metal salt can be added before the previous metal salt gets reduced which means no more successive reduction of metal salts.
  • the Ag salt may be added after Sn—Cu alloy nanoparticles are formed (S 103 , S 203 ) as shown in FIG. 2 .
  • the Ag salt may include AgNO 3 , AgCl, AgBr, AgI, AgOH, Ag 2 SO 4 , AgCH 3 COO and AgCH 3 COCHCOCH 3 but it is not limited thereto.
  • the Ag salt may be added alone or in a combination of 2 or more.
  • the Agu salt may be added directly or as a solution dissolved in a solvent.
  • the forming Sn—Cu—Ag alloy nanoparticles may be performed within 3 to 60 min after the Sn—Cu alloy nanoparticles are formed. When it is performed later than 60 min, each metal may be formed into its particles so that uniformed alloy cannot be formed. On the other hand, when it is performed within less than 3 min, the other metal salt can be added before the previous metal salt gets reduced which means no more successive reduction of metal salts.
  • Such produced alloy nanoparticles may be isolated and purified by washing to increase the purity.
  • reaction solution was further reacted for 10 min to provide dispersion including alloy nanoparticles having 99.3 wt % Sn-0.7 wt % Cu.
  • Ethanol was added to the dispersion and the mixture was then performed for the centrifugation (8000 rpm, 20 min) 3 times to remove excess amount of remaing surfactant and other organic materials to finally provide target alloy nanoparticle powder.
  • FIG. 3 is a transmission electron microscopy (TEM) result of the alloy nanoparticles according to Example 1 and determines that the alloy nanoparticles having size of 30 nm and 99.3 Sn-0.7 Cu (weight ratio) are formed. It is also noted that dispersion stability is excellent.
  • TEM transmission electron microscopy
  • FIG. 4 is is a differential scanning calorimetry (DSC) analysis result of the alloy nanoparticles according to Example 1. It shows a peak at 225° C. which is closer to 227° C. which is the melting temperature of alloy nanoparticles having 99.3 Sn-0.7 Cu (weight ratio). Thus, it is determined that the alloy nanoparticles having 99.3 Sn-0.7 Cu (weight ratio) is properly formed.
  • DSC differential scanning calorimetry
  • the reaction solution was performed for another 10 min and then Ag(NO) 3 sonicated in 1,5-pentanediol was added.
  • the reaction solution was further reacted for 10 min to provide dispersion including alloy nanoparticles having 96.5 wt % Sn-3.0 wt % Ag-0.5 wt % Cu(weight ratio).
  • Ethanol was added to the dispersion and the mixture was then performed for the centrifugation (8000 rpm, 20 min) 3 times to remove excess amount of remaing surfactant and other organic materials to finally provide target alloy nanoparticle powder.
  • FIG. 5 is a transmission electron microscopy (TEM) result of the alloy nanoparticles according to Example 2. It is determined that alloy nanoparticles having 96.5 Sn-3.0 Ag-0.5 Cu (weight ratio) are formed.

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  • Engineering & Computer Science (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Conductive Materials (AREA)
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US20110215279A1 (en) * 2010-03-04 2011-09-08 Lockheed Martin Corporation Compositions containing tin nanoparticles and methods for use thereof
CN103146250A (zh) * 2013-03-01 2013-06-12 溧阳市新力机械铸造有限公司 一种纳米银锡铜合金导电油墨的制备方法
CN103146251A (zh) * 2013-03-01 2013-06-12 溧阳市新力机械铸造有限公司 一种纳米金-锡-铜合金导电油墨的制备方法
CN103194116A (zh) * 2012-01-09 2013-07-10 深圳市纳宇材料技术有限公司 一种油墨、透明导电线路及透明导电线路的制备方法
JP2015004121A (ja) * 2013-05-22 2015-01-08 株式会社豊田中央研究所 金属ナノ粒子ペースト、それを含有する接合材料、及びそれを用いた半導体装置
US9011570B2 (en) 2009-07-30 2015-04-21 Lockheed Martin Corporation Articles containing copper nanoparticles and methods for production and use thereof
US9072185B2 (en) 2009-07-30 2015-06-30 Lockheed Martin Corporation Copper nanoparticle application processes for low temperature printable, flexible/conformal electronics and antennas
US9378861B2 (en) 2009-11-30 2016-06-28 Lockheed Martin Corporation Nanoparticle composition and methods of making the same
CN106475711A (zh) * 2016-10-21 2017-03-08 中国计量大学 一种纳米锡银铜焊粉的制备工艺
US9620786B2 (en) 2012-04-23 2017-04-11 Lg Chem, Ltd. Method for fabricating core-shell particles and core-shell particles fabricated by the method
US9695521B2 (en) 2010-07-19 2017-07-04 Universiteit Leiden Process to prepare metal nanoparticles or metal oxide nanoparticles
US10544483B2 (en) 2010-03-04 2020-01-28 Lockheed Martin Corporation Scalable processes for forming tin nanoparticles, compositions containing tin nanoparticles, and applications utilizing same
CN110919022A (zh) * 2019-08-19 2020-03-27 张博成 一种表面修饰纳米铜微粒的制备方法
CN110961826A (zh) * 2019-12-25 2020-04-07 哈尔滨工业大学 一种纳米imc均匀增强锡基合金接头的制备方法
CN110977238A (zh) * 2019-12-25 2020-04-10 哈尔滨工业大学 一种纳米imc均匀增强锡基焊料及其制备方法
CN111015010A (zh) * 2019-12-27 2020-04-17 苏州优诺电子材料科技有限公司 一种性能稳定的焊锡膏及其制备方法
CN112372174A (zh) * 2020-09-24 2021-02-19 南昌航空大学 耐高温服役的复合钎料、焊膏及其焊接方法与电子基板
CN112475313A (zh) * 2020-11-11 2021-03-12 昆明理工大学 一种通过化学反应制备纳米级焊料添加剂的方法

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JP5425664B2 (ja) * 2010-03-01 2014-02-26 国立大学法人宇都宮大学 金ナノ粒子及びその製造方法
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