US20090208363A1 - Solder alloy for oxide bonding - Google Patents

Solder alloy for oxide bonding Download PDF

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Publication number
US20090208363A1
US20090208363A1 US11/994,324 US99432406A US2009208363A1 US 20090208363 A1 US20090208363 A1 US 20090208363A1 US 99432406 A US99432406 A US 99432406A US 2009208363 A1 US2009208363 A1 US 2009208363A1
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United States
Prior art keywords
bonding
solder alloy
bal
mass
oxide
Prior art date
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Abandoned
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US11/994,324
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English (en)
Inventor
Minoru Yamada
Nobuhiko CHIWATA
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Proterial Ltd
SOPHIA PRODUCT Co
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Individual
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Filing date
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Assigned to HITACHI METALS, LTD., SOPHIA PRODUCT CO. reassignment HITACHI METALS, LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CHIWATA, NOBUHIKO, YAMADA, MINORU
Publication of US20090208363A1 publication Critical patent/US20090208363A1/en
Abandoned legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
    • B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
    • B23K35/262—Sn as the principal constituent
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • C03C27/04—Joining glass to metal by means of an interlayer
    • C03C27/042—Joining glass to metal by means of an interlayer consisting of a combination of materials selected from glass, glass-ceramic or ceramic material with metals, metal oxides or metal salts
    • C03C27/046—Joining glass to metal by means of an interlayer consisting of a combination of materials selected from glass, glass-ceramic or ceramic material with metals, metal oxides or metal salts of metals, metal oxides or metal salts only
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • C03C27/06—Joining glass to glass by processes other than fusing
    • C03C27/08—Joining glass to glass by processes other than fusing with the aid of intervening metal
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
    • C04B37/023—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used
    • C04B37/026—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used consisting of metals or metal salts
    • 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
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2311/00—Metals, their alloys or their compounds
    • B32B2311/12—Copper
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
    • C04B2237/12—Metallic interlayers
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/32—Ceramic
    • C04B2237/34—Oxidic

Definitions

  • the present invention relates to an optimal solder alloy for bonding to oxide materials such as glass and ceramic. More particularly, the present invention relates to a technical field of welding (sealing) with a lead-free alloy solder to fabricate dual-layer glass, vacuum containers, or sealed glass containers.
  • a method of bonding and welding performed at about 380° C. mainly uses a lead-containing solder or a lead glass material.
  • lead cannot be used any more due to environmental problems.
  • various wax materials and brazing sheets disclosed in “JIS Handbook (3) Non-ferrous metals” it is difficult to supply a material that melts below 400° C. and has good adhesion, and is capable to bond without the problems of contraction and cracking of a glass resulted from the difference between the thermal expansion coefficients of the glass and the wax materials.
  • sealing materials with In (indium) and an In alloy as a metal material have been set forth recently (please see Japanese Patent Early Laid-open Publications No. 2002-020143 and No. 2002-542138). Furthermore, an In-based solder alloy is further set forth, which is formed by adding various elements, such as Al, Ag, Cu, and Zn, into a material with Sn as the principal composition, in addition to a large amount of In (please see Japanese Patent Early Laid-open Publication No. 2000-141078).
  • the materials disclosed in Japanese Patent Early Laid-open Publications No. 2002-020143, No. 2002-542138, and No. 2000-141078 have excellent bonding strength and hermetic sealing capability on oxide materials, such as glass and ceramic.
  • oxide materials such as glass and ceramic.
  • the supply of In that must be added during the application is inadequate; thus, the application of methods in Japanese Patent Early Laid-open Publications No. 2002-020143 and No. 2002-542138 is limited due to high cost.
  • the method in Japanese Patent Early Laid-open Publication No. 2000-141078, in which effects are obtained by adding a small amount of In a great deal of time is demanded for adjusting the compositions as various elements are required to be added besides In (indium).
  • the present invention is directed to provide a lead-free metal solder material, which is a solder alloy merely for bonding to an oxide and capable of realizing excellent bonding strength and hermetic sealing by a composition system as simple as possible, so as to solve the above problems.
  • a ternary Sn-based lead-free solder alloy having the composition balance below can directly bond oxide materials, which are represented by glass, with high bonding strength.
  • the present invention provides a solder alloy for bonding to an oxide, which contains 2.0-15.0 mass % of Ag, more than 0.1-6.0 mass % of Al, and the remainder is composed of Sn and some inevitable impurities.
  • the content of Al is preferably 0.3-3.0 mass %, and more preferably 0.5-3.0 mass %.
  • the content of Ag is preferably 3.0-13.0 mass %, and more preferably more than 5.0-12.0 mass %, and most preferably 6.0-10.0 mass %.
  • a relation between Ag and Al that fits the following equation: 0 ⁇ [(% Ag) ⁇ (% Al) ⁇ 7.8] ⁇ 10 is preferred.
  • the solder alloy for oxide bonding of the present invention is used for bonding glass, for instance, and has an excellent effect.
  • a lead-free and environmental-friendly solder alloy for bonding to an oxide in which the solder alloy of the invention has a simple composition design and requires no complex production process. Further, the solder alloy of the invention has excellent bonding strength and hermetic sealing capability. Furthermore, the operating temperature of the solder alloy for bonding to an oxide of the present invention can be selected from a low heating range of about 230° C.-400° C., for example, for the welding of a dual-layer glass and a glass container, to conserve thermal energy.
  • FIG. 1 is an electron microscope picture showing a cross-section of a bonding between soda glass substrates by using a solder alloy according to an embodiment of the present invention.
  • FIG. 2 is an electron microscope picture showing a cross-section of a bonding between a soda glass and Fe-42% Ni alloy by using a solder alloy according to an embodiment of the present invention.
  • FIG. 3 is an electron microscope picture showing a cross-section of a bonding between aluminum oxide and copper by using a solder alloy according to an embodiment of the present invention.
  • FIG. 4 is a schematic diagram showing a three point bending test for evaluating the bonding strength according to an embodiment of the present invention.
  • FIG. 5 is a schematic diagram showing a leakage test for evaluating the vacuum sealing properties of a bonding surface according to an embodiment of the present invention.
  • compositions of the solder alloy of the present invention are illustrated.
  • the compositions of the solder alloy is presented in “%”, which represents mass percentage (mass %).
  • Al is an indispensable and necessary metal for bonding with an oxide material. That is, in the Sn—Ag-based solder alloy, if varying the contents of Sn and Ag still results with difficulties in bonding with the oxide material, the wettability to the oxide material can be increased by adding Al, so as to enhance the adhesion with the oxide material. The reason is that, Al has a strong tendency to form an oxide material, so Al can easily combine with the oxide, and to increase the wettability to the oxide material. However, if an excessive amount of Al is added, an aluminum oxide material is formed, which will reduce the bonding or increase the metal solidification shrinkage, and the problem of fracturing of the bonded articles (oxide). Therefore, the content of Al, with respect to the content of Ag described below, is more than 0.1% to 6.0%, preferably between 0.5% to 3.0%, and more preferably 0.5% to 1.5%.
  • Ag is the most suitably used to control the amount of Al in Sn.
  • the lead-free metal alloy solder with Al added in Sn of the present invention Ag is an indispensable and necessary metal.
  • Ag is an element that inhibits the formation of an oxide layer of the metal solder, Ag is further an important and necessary element. However, if an excessive amount of Ag is added, a large amount of hard and brittle intermetallic compound is formed in the solder; thus, the bonding strength is reduced.
  • the content of Ag, with respect to the added amount of Al described above is more than 2.0% to 15.0%, preferably 3.0% to 13.0%, more preferably 5.0% to 12.0%, and most preferably 6.0% to 10.0%.
  • the relation between Al and Ag is important and it is preferably to adjust Al and Ag correspondingly. That is, when the dispensation ratio of Al and Ag is optimally controlled according to the present invention so as to optimize the adhesion with the oxide material, and under the condition of controlling the formation of the intermetallic compound of Al and Ag, if excessive Al is added relative to the content of Ag, Al will be segregated, the wettability to the oxide material is reduced. Furthermore, if the amount of Al is small relative to the content of Ag, sufficient wettability might not be obtained as Al, that is capable of increasing the wettability, is entangled with Ag during forming the intermetallic compound.
  • the optimal adjusting index of Ag and Al has been identified that the calculated value of [(% Ag) ⁇ (% Al) ⁇ 7.8] is preferred as a standard. Furthermore, the calculated value preferably satisfies the inequality of 0 ⁇ [(% Ag) ⁇ (% Al) ⁇ 7.8] ⁇ 10, which is effective for increasing the wettability when vacuum sealing is performed by oxide bonding.
  • Sn is an essential element of the solder alloy of the present invention, which can alleviate the thermal expansion coefficient to the oxide material and reduce the melting temperature. Particularly, during the adjustment of the thermal expansion coefficient, the content of Sn is preferably adjusted to the range of 85% to 90%.
  • the solder alloy of the present invention can achieve excellent bonding strength and hermetic sealing by limiting the bonding article as being an oxide material. That is, the solder alloy of the present invention can definitely exert excellent bonding capability on ceramics such as aluminum oxide and glass such as soda lime glass, and to the materials that are not the above oxides. Furthermore, the present invention is not merely used for the bonding between the above oxide materials. As long as at least one article is an oxide material, the other article can be a material that is not an oxide material and a bonding capability can be ensured. For example, the solder alloy of the present invention even has bonding capability on various metals, such as stainless steel, copper, Fe—Ni-based alloy. Even the other article is a material of poor bonding capability, if a surface treatment is applied thereon to provide the bonding capability, the material can also be used without limitation.
  • the supply of the bonding material is preferably performed under a pre-melted condition. That is, when the solder alloy is in a solid state, most of its surface is likely to be oxidized. The oxide layer formed on the surface is the main reason in hindering the solder bonding. However, if the solder alloy is in a pre-melted state, the surface can keep fresh with merely a little oxidation. Therefore, if the bonding material is attached onto the solder alloy after the solder alloy is melted, good bonding strength can be obtained.
  • the bonding material can be used in the following configurations, i.e., the melted solder alloy can be infused between bonding surfaces of the bonding material units in final configuration after combination; alternatively, another bonding material is disposed on the melted solder alloy disposed on a surface of the bonding material.
  • FIG. 1 is an enlarged, cross-sectional view of a bonding of soda glass substrates by using a Sn-7% Ag-0.5% Al solder alloy of the present invention.
  • FIG. 2 is an enlarged cross-section view of a bonding between a soda glass substrate and a Fe-42% Ni alloy by using the same solder alloy of the present invention.
  • FIG. 3 is an enlarged, cross-sectional view of a bonding between an aluminum oxide and copper by using the same solder alloy of the present invention.
  • compositions Sn, Ag, and Al are weighted and melted at high frequency under an Ar (argon) atmosphere.
  • the compositions are then infused into a mold under the same environment, so as to fabricate a solder alloy. Thereafter, the resulting solder alloy is evaluated according to the test methods below. Furthermore, in the evaluation, in order to be welded easily, the solder alloy is cut and processed into small pieces for use.
  • test sheets are prepared, two glass plates are connected by the solder alloy, and a three point bending test is performed thereon.
  • the test sheets are two soda lime glass substrates, which are 3 mm thickness ⁇ 50 mm length ⁇ 25 nun width and bonded by a bonding material of 6 mm length at different positions ( FIG. 4 ). Then, the bonded test sheets are used to perform the three point bending test, in which the bonding sites are striped, and the load is determined when the two glass plates are separated or the test sheets are damaged.
  • the load evaluation test machine is MODEL-1308 manufactured by AIKON ENGINEERING CO., LTD. The test results and the compositions of the used solder alloy are listed in Table 1 together.
  • the solder, alloy of the present invention is required to be a solder alloy “for an oxide bonding”; thus, a sufficient bonding strength must be ensured first. Furthermore, by adjusting a desirable composition of the solder alloy stress relaxation and hermetic sealing of the solder bonding site are provided. Accordingly, the solder alloy of the invention can be applied in many fields. Hereinafter, the properties are evaluated.
  • a soda lime glass substrate of 5 mm thickness ⁇ 40 mm length ⁇ 40 mm is placed on a heating plate and heated to about 380° C. Then, under the ambient atmospheric condition, the solder alloy is coated on a surface of the soda lime glass substrate to about 0.4 mm thick.
  • the internal stress of the glass is determined by polarization compensation method (Senarmont method). The determination is directed to determining the internal stress on the bonding surface of the solder alloy and the internal stress on the surface without being coated with the solder alloy, and obtaining the difference of the stresses as the increment of the internal stress of the glass due to the coating of the solder alloy when the compressive stress is positive.
  • the test results and the compositions of the used solder alloy are listed in Table 2 together.
  • a soda lime glass substrate of 3 mm thickness ⁇ 50 mm length ⁇ 50 mm is heated to 380° C. on a glass, and a solder alloy of about 2 mm width is coated around a surface of the glass substrate. Then, a substrate of the same size, pre-heated to the same temperature and having a 3 mm ⁇ hole at central portion, is laminated on the surface, and the two pieces of glass are bonded. At this time, as a stainless steel foil of about 0.1 mm thickness (about 1 mm angle) is disposed between the glass surfaces as a pad, a container having 0.1 mm height space inside is formed ( FIG. 5 ).
  • the space is vacuumed by a leakage detector (HELLOT700, manufactured by ULVAC) and a helium (He) gas is blown to each bonding site to determine leakage.
  • HELLOT700 manufactured by ULVAC
  • He helium

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Metallurgy (AREA)
  • Structural Engineering (AREA)
  • Joining Of Glass To Other Materials (AREA)
US11/994,324 2005-07-14 2006-07-13 Solder alloy for oxide bonding Abandoned US20090208363A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2005233746 2005-07-14
JP2005-233746 2005-07-14
PCT/JP2006/313983 WO2007007840A1 (ja) 2005-07-14 2006-07-13 酸化物接合用はんだ合金

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US20090208363A1 true US20090208363A1 (en) 2009-08-20

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US11/994,324 Abandoned US20090208363A1 (en) 2005-07-14 2006-07-13 Solder alloy for oxide bonding
US12/712,984 Abandoned US20100147926A1 (en) 2005-07-14 2010-02-25 Method for oxide bonding using solder alloy

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US12/712,984 Abandoned US20100147926A1 (en) 2005-07-14 2010-02-25 Method for oxide bonding using solder alloy

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US (2) US20090208363A1 (zh)
JP (1) JP4669877B2 (zh)
KR (1) KR100930348B1 (zh)
CN (1) CN101198436B (zh)
TW (1) TWI347243B (zh)
WO (1) WO2007007840A1 (zh)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080241552A1 (en) * 2007-03-29 2008-10-02 Hitachi Metals, Ltd. Solder alloy and glass bonded body using the same
US10731233B2 (en) 2015-10-16 2020-08-04 AGC Inc. Composition for bonding

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CN101402514B (zh) * 2007-10-03 2011-09-07 日立金属株式会社 氧化物接合用焊料合金和使用了它的氧化物接合体
KR101173531B1 (ko) * 2009-05-25 2012-08-13 히타치 긴조쿠 가부시키가이샤 땜납 합금 및 이를 이용한 땜납 접합체
KR101108157B1 (ko) 2009-11-19 2012-01-31 삼성모바일디스플레이주식회사 유기 발광 디스플레이 장치
WO2012075724A1 (en) * 2010-12-10 2012-06-14 Luoyang Landglass Technology Co., Ltd. Vacuum glass component
WO2013005312A1 (ja) * 2011-07-06 2013-01-10 有限会社ソフィアプロダクト 酸化物接合材及びこれを用いた接合体
CN103775469A (zh) * 2012-10-23 2014-05-07 浙江喜乐嘉电器有限公司 一种紧固件的防盗结构及恢复工具
JP2016141611A (ja) * 2015-02-04 2016-08-08 旭硝子株式会社 接合用組成物
CN107540247A (zh) * 2017-09-07 2018-01-05 上海耀江实业有限公司 一种真空玻璃真空制作方法
JP7142644B2 (ja) * 2017-11-10 2022-09-27 日本板硝子株式会社 ガラスパネル及びガラスパネルにおける吸引孔の規定方法
JPWO2019093326A1 (ja) * 2017-11-10 2020-11-26 日本板硝子株式会社 溶融金属供給装置、これを用いたガラスパネルの製法及びガラスパネル
CN115397786B (zh) * 2020-04-09 2024-02-20 业纳光学系统有限公司 将玻璃元件热稳定地接合到支撑元件的方法、生产光学装置的方法以及光学装置
CN114131239B (zh) * 2021-12-27 2023-02-28 浙江亚通新材料股份有限公司 一种汽车玻璃焊接用无铅焊料

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Publication number Priority date Publication date Assignee Title
US20080241552A1 (en) * 2007-03-29 2008-10-02 Hitachi Metals, Ltd. Solder alloy and glass bonded body using the same
US7901782B2 (en) * 2007-03-29 2011-03-08 Hitachi Metals, Ltd. Solder alloy and glass bonded body using the same
US10731233B2 (en) 2015-10-16 2020-08-04 AGC Inc. Composition for bonding

Also Published As

Publication number Publication date
CN101198436A (zh) 2008-06-11
JP4669877B2 (ja) 2011-04-13
US20100147926A1 (en) 2010-06-17
KR100930348B1 (ko) 2009-12-08
WO2007007840A1 (ja) 2007-01-18
TWI347243B (en) 2011-08-21
KR20080021080A (ko) 2008-03-06
TW200706298A (en) 2007-02-16
CN101198436B (zh) 2010-10-06
JPWO2007007840A1 (ja) 2009-01-29

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