WO2013183315A1 - シールリングおよびシールリングの製造方法 - Google Patents
シールリングおよびシールリングの製造方法 Download PDFInfo
- Publication number
- WO2013183315A1 WO2013183315A1 PCT/JP2013/050583 JP2013050583W WO2013183315A1 WO 2013183315 A1 WO2013183315 A1 WO 2013183315A1 JP 2013050583 W JP2013050583 W JP 2013050583W WO 2013183315 A1 WO2013183315 A1 WO 2013183315A1
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- WIPO (PCT)
- Prior art keywords
- material layer
- seal ring
- brazing
- filler metal
- brazing material
- Prior art date
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Classifications
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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
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
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- 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
- H05K5/00—Casings, cabinets or drawers for electric apparatus
- H05K5/06—Hermetically-sealed casings
- H05K5/066—Hermetically-sealed casings sealed by fusion of the joining parts without bringing material; sealed by brazing
-
- 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
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3006—Ag as the principal constituent
-
- 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
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/302—Cu as the principal constituent
-
- 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
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3053—Fe as the principal constituent
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- 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
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/013—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium
-
- 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
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/018—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of a noble metal or a noble metal alloy
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
- C22C38/105—Ferrous alloys, e.g. steel alloys containing cobalt containing Co and Ni
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
- C22C5/08—Alloys based on silver with copper as the next major constituent
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16J—PISTONS; CYLINDERS; SEALINGS
- F16J15/00—Sealings
- F16J15/02—Sealings between relatively-stationary surfaces
- F16J15/06—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces
- F16J15/064—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces the packing combining the sealing function with other functions
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16J—PISTONS; CYLINDERS; SEALINGS
- F16J15/00—Sealings
- F16J15/02—Sealings between relatively-stationary surfaces
- F16J15/06—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces
- F16J15/08—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces with exclusively metal packing
- F16J15/0806—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces with exclusively metal packing characterised by material or surface treatment
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/02—Containers; Seals
- H01L23/10—Containers; Seals characterised by the material or arrangement of seals between parts, e.g. between cap and base of the container or between leads and walls of the container
-
- 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
-
- 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
- H01L2924/0001—Technical content checked by a classifier
- H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
-
- 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
- H01L2924/15—Details of package parts other than the semiconductor or other solid state devices to be connected
- H01L2924/161—Cap
- H01L2924/1615—Shape
- H01L2924/16195—Flat cap [not enclosing an internal cavity]
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- 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
- Y10T29/00—Metal working
- Y10T29/49—Method of mechanical manufacture
- Y10T29/49998—Work holding
Definitions
- the present invention relates to a seal ring used for an electronic component storage package and a method for manufacturing the seal ring.
- Japanese Patent Laid-Open No. 2006-49595 discloses a paste made of a mixture of a silver-based brazing powder containing Ag, Cu and Sn and a medium on one surface of a base material made of an Fe—Ni—Co alloy plate. After the coating, a silver brazing clad material including a base material layer made of an Fe—Ni—Co alloy and a silver brazing material layer is formed by firing or the like. Thereafter, a method of forming a ring body (seal ring) by punching a silver brazing clad material into a ring shape is disclosed.
- the silver brazing material layer is stretched to form a base. It arrange
- the silver brazing filler metal layer that has been excessively scooped by heat during the manufacture of the electronic component storage package spreads over the lid material. End up. As a result, it can be considered that there is a problem that the silver-based brazing filler metal layer spread on the lid material scatters from the lid material and adheres to the electronic component housed in the electronic component housing package.
- the present invention has been made to solve the above-described problems, and one object of the present invention is to prevent the brazing material layer from excessively scooping up the side surface of the base material layer. It is an object of the present invention to provide a seal ring and a seal ring manufacturing method capable of suppressing the material layer from being scattered and adhering to an electronic component.
- a seal ring according to a first aspect of the present invention is a seal ring used in an electronic component storage package, and is a clad material in which a base material layer and a brazing material layer disposed on one surface of the base material layer are joined. The side brazing material part which covers the side surface of the base material layer in the brazing material layer is removed.
- the seal ring according to the first aspect of the present invention when the brazing filler metal layer of the seal ring is melted by removing the side brazing filler metal portion covering the side surface of the base material layer of the brazing filler metal layer.
- the base material layer includes round corners connecting one surface of the base material layer and the side surface formed in a substantially flat surface shape, At least the side brazing material portion covering the substantially flat side surface is removed. If comprised in this way, since the side surface brazing material part which covers the substantially flat side surface is removed, it can suppress more that a brazing material layer scoops up the side surface of a base material layer excessively.
- the “side surface formed in a substantially flat surface shape” includes a curvature sufficiently larger than the curvature radius of the side surface where a minute unevenness is formed, or a round corner, as well as the flat surface side surface.
- the base material layer mainly includes Fe, Ni, and Co
- the brazing material layer mainly includes Ag and Cu.
- the brazing material layer mainly contains Ag and Cu, and the concentration of Ag in the vicinity of the surface of the brazing material layer is higher than the concentration of Ag inside the brazing material layer. large. If comprised in this way, since Ag has corrosion resistance compared with Cu, it can improve the corrosion resistance of the surface of a brazing material layer by Ag in the surface vicinity of a brazing material layer. Further, since the Ag concentration in the vicinity of the surface of the brazing material layer is large, the color tone of the surface of the brazing material layer can be made closer to silver.
- a method for manufacturing a seal ring according to a second aspect of the present invention is a method for manufacturing a seal ring used in an electronic component storage package, comprising: a base material layer; a brazing material layer bonded to one surface of the base material layer; Of the brazing material layer formed by stretching the brazing material layer when punching the cladding material into the shape of the seal ring, the step of preparing the clad material, the step of punching the cladding material into the shape of the seal ring, And a step of removing a side brazing material portion covering the side surface of the material layer.
- the brazing material layer is formed by extending the brazing material when the cladding material is punched into the shape of the sealing ring.
- the brazing filler metal layer of the seal ring is melted by providing the step of removing the side brazing filler metal portion covering the side surface of the layer, the brazing filler metal layer excessively scoops the side surface of the base material layer through the side brazing filler metal portion. It can suppress going up. Thereby, it is possible to suppress the brazing filler metal layer from being scattered due to heat or the like during manufacture of the electronic component storage package and adhering to the electronic component stored in the electronic component storage package.
- the base material layer includes round corners that connect one surface of the base material layer and the side surface formed in a substantially flat surface shape, and the side surface.
- the step of removing the brazing material portion includes a step of removing at least the side brazing material portion covering the substantially flat side surface of the brazing material layer. If comprised in this way, since the side surface brazing material part which covers the substantially flat side surface will be removed, it can suppress more that a brazing material layer scoops up the side surface of a base material layer excessively.
- the step of removing the side brazing material portion includes a step of removing the side brazing material portion by wet etching. If comprised in this way, compared with the case where a side surface brazing material part is removed by mechanical polishing etc., the minute side surface brazing material part which covers the side surface of a base material layer can be removed reliably.
- the step of removing the side brazing material portion by wet etching includes a step of removing the side brazing material portion by isotropically removing the brazing material layer by wet etching. If comprised in this way, since it is not necessary to perform a complicated etching process in order to selectively remove a side brazing material part, a side brazing material part can be removed easily.
- the step of isotropically removing the brazing material layer by wet etching is performed by wet etching.
- the process includes removing the material part and forming the corners of the brazing material layer into a round shape. If configured in this way, the corners of the brazing filler metal layer will be round and no longer sharp, so when the corners of the brazing filler metal layer come into contact with other members, other members will be damaged. Can be suppressed.
- the step of removing the side brazing material portion by wet etching is such that the brazing material layer is easily etched and the base material layer Including a step of removing the side brazing filler metal portion using an etchant that is difficult to etch. If comprised in this way, a brazing material layer can be selectively etched easily.
- the base material layer mainly contains Fe, Ni, and Co.
- the material layer mainly contains Ag and Cu
- the etching solution contains at least an oxidizing agent that oxidizes the surface of the brazing material layer, an oxide removing agent that removes the oxidized brazing material layer, and water. If comprised in this way, the brazing filler metal layer which mainly contains Ag and Cu can be selectively etched, and a side brazing filler metal part can be removed reliably.
- the etchant includes an oxidant, an oxide remover, and water
- the etchant is an oxidant composed of hydrogen peroxide and an oxide composed of acetic acid.
- a removal agent and water are included at least. If comprised in this way, the brazing material layer which mainly contains Ag and Cu can be etched more selectively, and a side surface brazing material part can be removed more reliably.
- the brazing material layer mainly contains Ag and Cu, and the etching solution of the wet etching is a surface of the brazing material layer.
- a side brazing material comprising: an oxidizing agent that oxidizes, an oxide removing agent that removes the oxidized brazing material layer, water, and a Cu preferential removing agent that preferentially removes Cu on the surface of the brazing material layer
- the Cu concentration on the surface of the brazing filler metal layer is preferentially removed using an etching solution, whereby the concentration of Ag in the vicinity of the surface of the brazing filler metal layer is changed to the Ag inside the brazing filler metal layer.
- the step of making the concentration greater than If comprised in this way since Ag has corrosion resistance compared with Cu, it can improve the corrosion resistance of the surface of a brazing material layer by Ag in the surface vicinity of a brazing material layer. Further, since the Ag concentration in the vicinity of the surface of the brazing material layer is large, the color tone of the surface of the brazing material layer can be made closer to silver. Further, since Cu on the surface of the brazing material layer can be preferentially removed using an etching solution to which a Cu preferential removal agent is added, the concentration of Ag in the vicinity of the surface of the brazing material layer can be easily determined. It is possible to make Ag remain and concentrate in the vicinity of the surface of the brazing filler metal layer by making it larger than the concentration of Ag inside the layer.
- the brazing material layer mainly contains Ag and Cu, and the etching solution of the wet etching is a surface of the brazing material layer.
- a side brazing material comprising: an oxidizing agent that oxidizes, an oxide removing agent that removes the oxidized brazing material layer, water, and a Cu preferential removing agent that preferentially removes Cu on the surface of the brazing material layer
- the process of removing the portion by wet etching is performed by preferentially removing Cu on the surface of the brazing filler metal layer using an etching solution, so that the concentration of Ag in the vicinity of the brazing filler metal layer surface is wet etched on the side brazing filler metal portion.
- the step of making the concentration higher than the concentration of Ag in the brazing material layer before removal by the step is included.
- the concentration of Ag in the vicinity of the surface of the brazing filler metal layer can be increased more than before the wet etching, so that the corrosion resistance of the surface of the brazing filler metal layer can be improved and the surface of the brazing filler metal layer can be improved. Can be brought closer to silver. Further, by using an etching solution to which a Cu preferential removal agent is added, the concentration of Ag in the vicinity of the surface of the brazing material layer is easily made larger than the concentration of Ag before the side brazing material portion is removed by wet etching. can do.
- the Cu preferential removing agent is preferably composed of a strong acid.
- the Ag oxide formed by the oxidant is difficult to remove, while the Cu oxide is easily removed. Therefore, the Cu preferential removal agent composed of the strong acid is used.
- Cu oxide can be easily removed preferentially. As a result, Cu on the surface of the brazing material layer can be easily removed preferentially.
- the Cu preferential removal agent is composed of a strong acid
- the Cu preferential removal agent is composed of sulfuric acid, which is a strong acid. If comprised in this way, Cu of the surface of a brazing material layer can be removed preferentially more easily.
- the sulfuric acid is preferably added to the etching solution so that the concentration thereof is 0.5 mass% or more of the entire etching solution. If constituted in this way, Cu on the surface of the brazing filler metal layer is surely preferentially removed, and the concentration of Ag in the vicinity of the surface of the brazing filler metal layer is made larger than the concentration of Ag in the brazing filler metal layer. Can do.
- the etching solution includes an oxidizing agent, an oxide removing agent, water, and a Cu preferential removing agent, preferably before and after the step of removing the side brazing material portion by wet etching.
- the solidus of the layer does not change substantially. If comprised in this way, it can suppress that temperature required in order to melt
- the step of removing the side brazing filler metal portion by wet etching This also serves to remove the oxidized brazing filler metal layer remaining on the surface and clean it.
- the process can be simplified, unlike a case where a process for removing the oxidized brazing filler metal layer remaining on the surface of the seal ring and cleaning it is provided separately.
- the manufacturing method of the seal ring including the step of removing the side brazing material portion by wet etching, preferably, prior to the step of removing the side brazing material portion by wet etching, when the cladding material is punched into the shape of the seal ring
- the method further includes the step of removing the minute projections of the formed base material layer, and the step of removing the side brazing filler metal portion by wet etching is a wet etching of the side brazing filler metal portion and the foreign matter adhering when the minute projections are removed.
- the present invention it is possible to suppress the brazing material layer from excessively scooping up the side surface of the base material layer, so that the brazing material layer is scattered and stored in the electronic component storage package. It can suppress adhering to an electronic component.
- FIG. 4 is a cross-sectional view taken along line 400-400 in FIG.
- FIG. 4 is an enlarged cross-sectional view taken along line 400-400 in FIG.
- It is sectional drawing which showed the structure of the electronic component storage package by 1st Embodiment of this invention.
- It is a perspective view for demonstrating the manufacturing process of the seal ring by 1st Embodiment of this invention.
- It is the expanded sectional view showing the seal ring after stamping in the manufacturing process of the seal ring by a 1st embodiment of the present invention.
- the seal ring 1 As shown in FIG. 1, the seal ring 1 according to the first embodiment is formed in a rectangular frame shape in plan view.
- the seal ring 1 has a length L1 of about 1.5 mm or more and about 2.0 mm or less in the longitudinal direction (X direction), and about 1.2 mm or more and about 1.6 mm or less in the short direction (Y direction).
- the length L2 is formed.
- the opening of the seal ring 1 has a length L3 of about 1.3 mm to about 1.6 mm in the X direction and a length L4 of about 0.9 mm to about 1.1 mm in the Y direction. Is formed.
- the seal ring 1 has a base material layer 10 disposed on the upper side (Z1 side) and a brazing filler metal layer 11 disposed on the lower side (Z2 side). It is composed of a clad material.
- the thickness t1 of the base material layer 10 in the Z direction is about 100 ⁇ m or more and about 130 ⁇ m or less
- the thickness t2 of the brazing filler metal layer 11 is about 15 ⁇ m or more and about 30 ⁇ m or less.
- the thickness t3 (t1 + t2) in the Z direction of the seal ring 1 is not less than about 115 ⁇ m and not more than about 160 ⁇ m.
- the base material layer 10 is formed of an Fe—Ni—Co alloy mainly containing approximately 30% by mass of Ni, approximately 17% by mass of Co, and Fe.
- the base material layer 10 has an upper surface 10a on the Z1 side, a lower surface 10b on the Z2 side joined to the brazing material layer 11, and a pair of side surfaces 10c.
- the upper surface 10a, the lower surface 10b, and the pair of side surfaces 10c are all formed in a substantially flat surface shape.
- the base material layer 10 further includes a pair of upper corner portions 10d that connect the upper surface 10a and the side surface 10c, and a pair of lower corner portions 10e that connect the lower surface 10b and the side surface 10c.
- the upper corner portion 10d and the lower corner portion 10e are formed in a round shape having a sufficiently small radius of curvature.
- the lower surface 10b is an example of the “one surface” in the present invention.
- the brazing material layer 11 is formed of silver brazing mainly containing about 85% by mass of Ag and Cu.
- the solid phase line of silver brazing constituting the brazing filler metal layer 11 (temperature at which part of the brazing filler metal layer 11 starts to melt) is about 780 ° C.
- the brazing filler metal layer 11 has a Z1 side upper surface 11a joined to the base material layer 10, a Z2 side lower surface 11b, and a pair of side surfaces 11c. Both the upper surface 11a and the lower surface 11b are formed in a substantially flat surface shape.
- the side surface 11 c is formed so as to be located slightly inside the side surface 10 c of the base material layer 10.
- the brazing material layer 11 is a pair of a pair of upper corner portions 11d that connect the upper surface 11a and the side surface 11c on the base material layer 10 side, and a pair of the lower surface 11b and the side surface 11c that are opposite to the base material layer 10. And a lower corner portion 11e.
- the upper corner portion 11 d is formed so as to be positioned on the lower corner portion 10 e of the base material layer 10. That is, the brazing filler metal layer 11 is formed up to substantially the center A of the lower corner portion 10 e of the base material layer 10, but is not formed on the side surface 10 c of the base material layer 10.
- the upper corner portion 11 d is formed so as to be located inside the side surface 10 c of the base material layer 10, and is configured so as to be located inside the side surface 11 c of the brazing material layer 11.
- the periphery of the boundary between the lower corner portion 10e of the base material layer 10 and the upper corner portion 11d of the brazing material layer 11 is recessed inward from the side surface 10c of the base material layer 10 and the side surface 11c of the brazing material layer 11. It is comprised so that it may become a shape.
- the lower corner 11e is formed in a round shape having a sufficiently small radius of curvature.
- the brazing filler metal layer 11 of the seal ring 1 is a side brazing filler metal portion 11f (described later) that covers at least the substantially flat side surface 10c of the base material layer 10 of the brazing filler metal layer 11. 7) is removed.
- a specific manufacturing process of the seal ring 1 will be described later.
- the electronic component storage package 100 includes a seal ring 1, a base 2 joined to the seal ring 1 below the seal ring 1 (Z2 side), and the seal ring 1. And a lid member 3 joined to the seal ring 1 above (Z1 side).
- the base 2 is formed of ceramics such as alumina and is formed in a box shape.
- the box-shaped base 2 is formed at the center of the base 2, and has a storage part 2 a to which an electronic component 5 such as a crystal resonator is attached via a bump 4, and a frame shape joined to the seal ring 1.
- the upper surface 2b Further, the seal ring 1 and the upper surface 2 b of the base 2 are joined by a molten brazing material layer 11 of the seal ring 1.
- a metallized layer made of W / Ni / Au may be provided on the upper surface 2 b of the base 2.
- the lid member 3 is made of a plate member made of an Fe—Ni—Co alloy.
- the lid member 3 and the base material layer 10 of the seal ring 1 are joined by seam welding.
- a plating layer made of Ni / Au may be provided on the lid member 3.
- the base 2 is formed slightly larger than the seal ring 1.
- the lid member 3 is formed slightly smaller than the seal ring 1 and larger than the opening of the seal ring 1.
- the base material layer 10 formed of an Fe—Ni—Co alloy and the lower surface 10b (see FIG. 6) of the base material layer 10 are joined, and about 85 mass% of Ag and Cu,
- a clad material 200 including a brazing filler metal layer 11 mainly formed of silver brazing is prepared.
- the thickness t1 (see FIG. 6) of the base material layer 10 is about 100 ⁇ m or more and about 130 ⁇ m or less
- the thickness t4 (see FIG. 6) of the brazing material layer 11 in the Z direction is
- the finished seal ring 1 is formed to have a thickness t6 (see FIG. 7) larger than the thickness t2 (see FIG. 3) of the brazing filler metal layer 11.
- the thickness t5 (t1 + t4) in the Z direction of the clad material 200 is larger than the thickness t3 (t1 + t2, see FIG. 3) of the seal ring 1 by the thickness t6.
- the clad material 200 is punched into the shape of the seal ring 1 (two-dot chain line). At this time, the clad material 200 is punched from the brazing material layer 11 side (Z2 side) along the thickness direction (Z direction). Thereby, the seal ring 1a punched in the shape of the seal ring 1 is formed.
- a minute projection (burr) 10f is formed on the upper corner portion 10d of the base material layer 10 of the seal ring 1a.
- a part of the minute protrusion 10f is formed at an acute angle so as to protrude upward (Z1 side) from the upper surface 10a of the base material layer 10.
- a part of the brazing material layer 11 bonded to the lower surface 10 b of the base material layer 10 moves upward (Z1 side) so as to extend to the side surface 10 c of the base material layer 10.
- the side brazing material portion 11 f connected to the brazing material layer 11 is formed on the side surface 10 c of the base material layer 10.
- barrel polishing is performed to remove the minute protrusions 10f formed on the base material layer 10 of the seal ring 1a.
- a plurality of seal rings 1a, a medium made of ceramics, a compound made of chemical powder, and water are put into the barrel.
- the barrel is rotated at a predetermined speed for a predetermined time.
- the fine protrusions 10f are removed, for example, when the medium collides with the fine protrusions 10f of the base material layer 10.
- the seal ring 1a is taken out and washed.
- the minute protrusions 10f of the base material layer 10 are removed, and the seal ring 1b is formed as shown in FIG.
- the upper corner portion 10d of the base material layer 10 is shaped into a round shape having a sufficiently small radius of curvature.
- the lower corner portion 11e of the brazing material layer 11 is also shaped into a slightly round shape.
- the silver brazing forming the brazing filler metal layer 11 of the seal ring 1b has a small hardness, the surface (the lower surface 11b, the side surface 11c) of the foreign matter 6 made of media residue or the like is exposed to the outside of the brazing filler metal layer 11.
- the lower corner portion 11e and the side brazing filler metal portion 11f are attached so as to be embedded.
- wet etching is performed in order to remove the side brazing filler metal portion 11f formed on the brazing filler metal layer 11 of the seal ring 1b.
- a plurality of seal rings 1b and an etching solution of about 10 ° C. or higher and about 30 ° C. or lower are charged into the barrel.
- This etching solution is a stock solution in which an oxidizing agent formed by hydrogen peroxide, an oxide removing agent formed by acetic acid or ammonia, and water are mixed in a predetermined ratio, or water is further added to the stock solution. It is comprised from the dilution liquid which diluted this by the predetermined
- the oxidizing agent has a function of oxidizing Ag and Cu contained in the brazing filler metal layer 11 (see FIG. 7) to form silver oxide and copper oxide, respectively.
- the oxide remover has a function of dissolving and removing silver oxide and copper oxide of the brazing material layer 11. Note that the etching solution is configured so that the silver brazing of the brazing material layer 11 is easily etched and the Fe—Ni—Co alloy of the base material layer 10 (see FIG. 7) is difficult to be etched.
- the barrel is rotated at a predetermined speed for a predetermined time.
- the brazing filler metal layer 11 is isotropically removed, whereby the surface of the brazing filler metal layer 11 is removed by a thickness t6 (see FIG. 7).
- the base material layer 10 is hardly removed.
- the side brazing filler metal portion 11f located on the side surface 10c of the base material layer 10 and having a thickness t7 smaller than the thickness t6 is removed. That is, the portion of the brazing filler metal layer 11 (side brazing filler metal portion 11f) that covers at least the substantially flat side surface 10c of the base material layer 10 is removed. Further, the lower corner portion 11e of the brazing filler metal layer 11 is formed into a round shape by being exposed to the etching solution on both the lower surface 11b side and the side surface 11c side. Further, as the surface exposed to the outside of the brazing material layer 11 is removed, the foreign matter 6 attached to the exposed surface of the brazing material layer 11 is also removed. As a result, the shape of the brazing filler metal layer 11 is formed up to the approximate center A of the lower corner 10e of the base material layer 10 as shown by a two-dot chain line in FIG. The shape is not formed on the top.
- the oxide (silver oxide and copper oxide) remaining on the surface of the brazing filler metal layer 11 is removed by washing with sulfuric acid or the like, and then washed with water (rinsing) and replaced with alcohol, whereby the seal ring 1 shown in FIG. Is manufactured.
- the seal ring 1 is disposed on the upper surface 2b of the base 2 made of ceramics. At this time, the seal ring 1 is arranged so that the lower surface 11b of the brazing filler metal layer 11 of the seal ring 1 contacts the upper surface 2b. Then, the brazing filler metal layer 11 is melted at a brazing temperature equal to or higher than the solidus line of silver brazing (about 780 ° C.) forming the brazing filler metal layer 11. Thereby, the seal ring 1 is joined to the upper surface 2 b of the base 2 by the molten brazing material layer 11. At this time, the side brazing material portion 11 f (see FIG.
- the electronic component 5 is attached to the storage portion 2 a of the base 2 through the bumps 4. Thereafter, seam welding is performed in a state in which the lid member 3 is in contact with the upper surface 10a of the base material layer 10. Thereby, the lid member 3 is welded to the upper surface 10 a of the seal ring 1.
- the brazing filler metal layer 11 is not excessively positioned in the vicinity of the upper surface 10a of the base material layer 10
- the brazing material layer 11 excessively positioned in the vicinity of the upper surface 10a of the base material layer 10 due to heat during seam welding. It is suppressed that a part spreads on the lower surface of the lid member 3.
- part of the brazing material layer 11 is prevented from scattering from the lower surface of the lid member 3 to the electronic component 5.
- the electronic component storage package 100 shown in FIG. 4 is manufactured.
- the side brazing filler metal portion 11f formed on the brazing filler metal layer 11 of the seal ring 1b and covering at least the substantially flat side surface 10c of the base material layer 10 is removed by wet etching.
- the brazing filler metal layer 11 of the seal ring 1 is melted and the base 2 of the electronic component storage package 100 and the seal ring 1 are joined, the brazing filler metal layer 11 is transferred to the side brazing filler metal portion 11f. It is possible to suppress the side 10c of the layer 10 from being crawled excessively.
- the side surface 10c of the base material layer 10 is made smaller than when the side brazing filler metal portion 11f is removed by mechanical polishing or the like.
- the small side brazing filler metal portion 11f that is covered can be reliably removed.
- the brazing filler metal layer 11 is isotropically removed to remove the side brazing filler metal portion 11f and the lower corner portion 11e of the brazing filler metal layer 11 is formed in a round shape. Accordingly, it is not necessary to perform a complicated etching process in order to selectively remove the side brazing filler metal portion 11f, so that the side brazing filler metal portion 11f can be easily removed. Further, since the lower corner portion 11e of the brazing filler metal layer 11 has a round shape and does not have a sharp shape, when the lower corner portion 11e of the sharp brazing filler metal layer 11 comes into contact with another member, the other member Can be suppressed.
- the brazing filler metal layer 11 is easily etched, and the Fe—Ni—Co alloy of the base layer 10 is not easily etched.
- the material layer 11 can be selectively etched.
- the base material layer 10 is formed with the Fe-Ni-Co alloy which mainly contains about 30 mass% Ni, about 17 mass% Co, and Fe, and brazing material layer 11 is formed.
- a silver brazing mainly containing about 85% by mass of Ag and Cu is formed, and an etching solution is formed by using an oxidizing agent formed by hydrogen peroxide, an oxide removing agent formed by acetic acid or ammonia, water, Is a stock solution mixed at a predetermined rate, or a diluted solution obtained by further diluting the stock solution by adding water.
- the brazing filler metal layer 11 formed of silver brazing can be selectively etched to effectively remove the side brazing filler metal portion 11f.
- the side surface brazing material portion is removed by removing the foreign matter 6 attached to the surface of the brazing material layer 11 as the surface exposed to the outside of the brazing material layer 11 is removed by wet etching. Since the foreign material 6 is simultaneously removed during the wet etching for removing 11f, the process can be simplified, unlike the case where a step for removing the foreign material 6 is separately provided.
- etching solution a stock solution was prepared in which acetic acid water containing 25% by mass of acetic acid, hydrogen peroxide water containing 35% by mass of hydrogen peroxide, and water were mixed at a volume ratio of 1: 5: 4. . Thereafter, a 1: 1 diluted solution in which the volume ratio of the stock solution to water was 1: 1 was prepared as an etching solution.
- a side brazing material portion was formed so as to cover the side surface of the base material layer.
- a plurality of foreign matters due to barrel polishing adhered to the surface of the brazing material layer.
- a part of the side brazing material portion covering the side surface of the base material layer is removed, and foreign matter is not observed. This is presumably because the foreign material adhering to the surface portion from which the brazing material layer was removed also moved into the etching solution as the brazing material layer was removed isotropically.
- the removal time of the side brazing filler metal portion increases as the ratio of water is increased to dilute the etching solution.
- the removal time of the side brazing filler metal portion was shortened as the temperature of the etching solution was increased in the etching solution composed of the 1: 1 diluted solution containing the stock solution.
- ammonia water containing 35% by mass of ammonia, hydrogen peroxide containing 35% by mass of hydrogen peroxide, and water are mixed at a volume ratio of 1: 1: 1.
- a prepared ammonia stock solution was prepared. Thereafter, a 1: 4 diluted solution in which the volume ratio of the ammonia stock solution to water was 1: 4 was prepared as an etching solution. It was confirmed that the side brazing filler metal portion was removed even when wet etching was performed using an etching solution containing this ammonia stock solution.
- the surface roughness of the surface of the base material layer and the surface of the brazing material layer before and after wet etching was measured.
- the arithmetic average roughness Ra and the maximum height roughness Rz of the surface of the base material layer and the surface of the brazing material layer were measured using a laser microscope (VK-8700, manufactured by Keyence Corporation).
- VK-8700 manufactured by Keyence Corporation
- the surface roughness of the surface of the base material layer and the surface of the brazing material layer hardly changed before and after wet etching.
- the surface of the base material layer and the surface of the brazing material layer are hardly roughened by wet etching.
- the seal ring 1 of Example 1 and the seal ring 1b of Comparative Example 1 are brought into contact with the Fe—Ni—Co alloy plate 8 on which Ni plating and Au plating are laminated, and the brazing material layer 11. Arranged. Then, the brazing filler metal layer 11 is melted at a brazing temperature equal to or higher than the solid phase line (about 780 ° C.) of the silver brazing forming the brazing filler metal layer 11, and the seal ring 1 (1b) and the Fe—Ni—Co alloy plate 8 are melted. And were joined. Thereafter, the molten state of the brazing filler metal layer 11 was observed using a scanning electron microscope.
- the brazing material layer 11 As the molten state of the brazing material layer shown in FIGS. 10 and 11, in Example 1 shown in FIG. 10, the brazing material layer 11 hardly crawls up on both side surfaces 10 c of the base material layer 10.
- the scooping portion 11g of the brazing material layer 11 is formed so as to cover more than half of both side surfaces 10c of the base material layer 10 and to extend to the vicinity of the upper surface 10a of the side surface 10c. .
- the amount of creeping of the brazing filler metal layer 11 in Example 1 is sufficiently smaller than the amount of creeping of the brazing filler metal layer 11 in Comparative Example 1, and the brazing filler metal layer 11 in Example 1 is the upper surface of the side surface 10c.
- the brazing filler metal layer 11 of the seal ring 1 was melted on the Fe—Ni—Co alloy plate 8 on which Ni plating and Au plating were laminated.
- the brazing filler metal layer 11 of the seal ring 1 is melted on the upper surface 2a (see FIG. 4) of the base 2 made of ceramics, the brazing filler metal layer 11 is considered to be in the same molten state.
- the concentration of Ag in the vicinity of the surface of the brazing material layer 311 is higher than the concentration of Ag in the interior 11 g of the brazing material layer 311. The case where it is large will be described.
- the seal ring 301 according to the second embodiment differs from the first embodiment in that the surface of the brazing filler metal layer 311 (the lower surface 11b, the pair of side surfaces 11c, the pair of upper corner portions 11d and the pair of lower corner portions 11e) and The concentration of Ag in the vicinity thereof is configured to be about 90% by mass or more. This concentration is higher than the Ag concentration (about 85% by mass) of the brazing material itself (the brazing material before wet etching) of the brazing material layer 311 and the Ag concentration (about 85% by mass) in the inner 11g of the brazing material layer 311. It is comprised so that it may become.
- the structure of the other seal ring 301 of 2nd Embodiment is the same as that of the said 1st Embodiment.
- a base material layer 10 formed of an Fe—Ni—Co alloy and a silver solder mainly containing about 85 mass% of Ag and Cu are used.
- a seal ring 1 a punched into the shape of the seal ring 1 is formed from the clad material 200 including the formed brazing material layer 11.
- barrel polishing is performed to remove the fine protrusions 10f formed on the base material layer 10 of the seal ring 1a, and as shown in FIG. 7, the seal ring 1b from which the fine protrusions 10f of the base material layer 10 are removed.
- wet etching is performed to remove the side brazing filler metal portion 11f formed in the brazing filler metal layer 11 of the seal ring 1b. Specifically, a plurality of seal rings 1b and an etching solution of about 10 ° C. or higher and about 30 ° C. or lower are charged into the barrel.
- a stock solution in which an oxidizing agent formed by hydrogen peroxide, an oxide removing agent formed by acetic acid or ammonia, and water are mixed at a predetermined ratio, or water is used. Furthermore, unlike the first embodiment in which a diluted solution obtained by diluting the stock solution at a predetermined ratio is used as an etching solution, a solution obtained by adding a strong acid made of dilute sulfuric acid to the stock solution or the diluted solution is used as an etching solution. Use. The diluted sulfuric acid is added to the etching solution so that the concentration of the diluted sulfuric acid is about 0.5% by mass or more of the entire etching solution.
- the diluted sulfuric acid it is preferable to add the diluted sulfuric acid to the etching solution so that the concentration of the diluted sulfuric acid is about 0.5% by mass or more and 1.0% by mass or less of the entire etching solution, More preferably, it is added to the etching solution so as to have a concentration of not less than 1.0% and not more than 1.0% by mass.
- This dilute sulfuric acid has a function of preferentially removing copper oxide among oxides (silver oxide and copper oxide) of the brazing filler metal layer 311 (see FIG. 3) formed of hydrogen peroxide.
- copper oxide is preferentially removed from the silver oxide by sulfuric acid on the surface of the brazing filler metal layer 311 (the lower surface 11b, the pair of side surfaces 11c, the pair of upper corner portions 11d, and the pair of lower corner portions 11e). Since it is consumed, the oxidation rate of Cu increases with the removal rate of copper oxide. As a result, Cu is preferentially removed.
- the barrel is rotated at a predetermined speed for a predetermined time.
- the brazing filler metal layer 311 is isotropically removed while the base material layer 10 is hardly removed.
- Cu in the vicinity of the surface of the brazing material layer 311 is preferentially removed, and the concentration of Ag in the vicinity of the surface of the brazing material layer 311 becomes about 90 mass% or more.
- the concentration of Ag in the vicinity of the surface of the brazing material layer 311 increases.
- the solidus line of silver brazing (the temperature at which a part of the brazing material layer 311 starts to melt) before and after the wet etching does not substantially change at about 780 ° C. That is, although the Ag concentration in the vicinity of the surface of the brazing material layer 311 is increased, the solidus line of the silver brazing does not substantially change at about 780 ° C.
- the oxide (silver oxide and copper oxide) remaining on the surface of the brazing material layer 311 is almost removed in the wet etching, unlike the first embodiment, the oxidation remaining on the surface of the brazing material layer 311.
- Direct washing with water (rinsing) and substitution with alcohol are performed without performing the step of removing the product by washing with sulfuric acid or the like. Thereby, the seal ring 301 shown in FIG. 3 is manufactured.
- the side brazing filler metal portion 11f formed on the brazing filler metal layer 311 of the seal ring 1b and covering at least the substantially flat side surface 10c of the base material layer 10 is removed by wet etching.
- the brazing material layer 311 from creeping up the side surface 10c of the base material layer 10 excessively along the side brazing material portion 11f.
- a Cu solution near the surface of the brazing filler metal layer 311 is used by using, as an etchant, a solution obtained by adding a strong acid composed of dilute sulfuric acid having a concentration of about 0.5 mass% or more to the stock solution or the diluted solution.
- a strong acid composed of dilute sulfuric acid having a concentration of about 0.5 mass% or more to the stock solution or the diluted solution.
- the Ag concentration (about 85% by mass) of the brazing material itself (the brazing material before wet etching) of the brazing material layer 311 and the concentration of Ag in the inner 11 g of the brazing material layer 311 about By increasing the Ag concentration in the vicinity of the surface of the brazing filler metal layer 311 to 85% by mass), Ag has more corrosion resistance than Cu.
- the corrosion resistance of the surface of the brazing material layer 311 can be further improved. Further, since the Ag concentration in the vicinity of the surface of the brazing material layer 311 is large, the color tone of the surface of the brazing material layer 311 can be made closer to silver. Moreover, since Cu on the surface of the brazing filler metal layer 311 can be preferentially removed using an etching solution to which a Cu preferential removal agent is added, the concentration of Ag in the vicinity of the surface of the brazing filler metal layer 311 can be easily set. It is possible to make Ag remain and concentrate near the surface of the brazing material layer 311 by making it larger than the concentration of Ag in the inside 11 g of the brazing material layer 311.
- the Cu oxide can be reliably removed preferentially. It is easy to preferentially remove Cu on the surface of the brazing material layer 311.
- the silver brazing solid line (brazing filler metal) constituting the brazing brazing filler metal layer 311 is used.
- the temperature at which a part of the layer 311 starts to melt) can be configured to hardly change at about 780 ° C., so that the brazing filler metal layer 311 has a higher solidus (about 780 ° C.). An increase in the temperature required to melt the layer 311 can be suppressed.
- a process for removing silver oxide and copper oxide remaining on the surface of the heel seal ring 311 and cleaning (generally, the surface of the seal ring 311 is cleaned with sulfuric acid). Since it is not necessary to separately provide a cleaning step), the step can be simplified.
- Example 2 acetic acid water containing 25% by mass of acetic acid, hydrogen peroxide water containing 35% by mass of hydrogen peroxide, and water were used at 1: 5: 4.
- a stock solution mixed at a volume ratio was prepared.
- a 1: 4 diluted solution in which the volume ratio of the stock solution to water was 1: 4 was prepared as an etching solution.
- the seal ring 1b and the etching solution were put into the barrel, and the barrel was rotated at a predetermined speed, and then cleaning and the like were performed. This obtained the seal ring 1 (refer FIG. 3) of Example 2.
- FIG. 3 the seal ring 1 (refer FIG. 3) of Example 2.
- Example 3 a solution obtained by adding dilute sulfuric acid as a strong acid to the 1: 4 diluted solution was used as an etching solution. In that case, it adjusted so that the density
- the concentration of Cu is higher after wet etching than before wet etching (Comparative Example 2).
- the concentration of Ag was reduced. This is because with acetic acid (oxide remover) alone, the rate at which Ag oxide (silver oxide) is removed is faster than the rate at which Cu oxide (copper oxide) is removed, and Ag is relatively low. This is probably because it was removed preferentially.
- the concentration of Cu and Ag in the depth direction of the brazing filler metal layer is determined by an Auger electron spectrometer. It was measured.
- the concentration of Ag gradually increased from the inside of the brazing material layer toward the surface.
- the concentration of Cu gradually decreased from the inside of the brazing material layer toward the surface. From this result, by adding sulfuric acid to the etching solution, Cu on the surface of the brazing filler metal layer can be removed preferentially. As a result, the concentration of Ag in the vicinity of the surface of the brazing filler metal layer can be reduced. It has been found that Ag can be retained and concentrated at the surface of the brazing filler metal layer above the concentration.
- the solidus became slightly higher as the concentration of sulfuric acid added to the etching solution increased.
- the solidus lines of the brazing material layers of Examples 3 to 6 were within 1.5 ° C. (776.1 ° C.) of the solidus line (776.0 ° C.) of the brazing material layer before wet etching (Comparative Example 2). (Example 4) It is above 777.4 degreeC (Example 6) or less), and it is thought that there is almost no temperature difference. As a result, it was confirmed that the solidus line of the brazing material layer hardly changed before and after wet etching.
- Example 3 the oxygen concentration on the surface of the brazing filler metal layer was smaller than in Comparative Example 2.
- wet etching is performed using an etching solution to which 0.7% by mass of sulfuric acid is added as in Example 3, compared with the case where wet etching is not performed as in Comparative Example 2, wet etching is performed. It was later found that oxidation of the surface of the brazing material layer was suppressed. This is because in the seal ring 301 of Example 3, Ag that is relatively less oxidized than Cu that is relatively easily oxidized is present on the surface of the brazing filler metal layer, and the oxidation of the surface of the brazing filler metal layer is suppressed. It is thought that. From this result, by performing wet etching using an etching solution to which sulfuric acid is added as in Example 3, it is possible to suppress the oxidation of the surface of the brazing filler metal layer. It has been found that the corrosion resistance can be improved.
- the side brazing filler metal portion 11f of the brazing filler metal layer 11 is removed by wet etching
- the present invention is not limited to this.
- the side brazing material portion may be removed by a method other than wet etching such as dry etching.
- the brazing material layer 11 showed the example formed to the approximate center A of the lower side corner
- this invention is not limited to this.
- the brazing material layer may be formed on the lower corner of the base material layer and up to the region near the side surface of the base material layer. Further, the brazing material layer may be formed only on the lower surface of the base material layer without being formed on the lower corner portion of the base material layer.
- an oxidant formed by hydrogen peroxide, an oxide remover formed by acetic acid or ammonia, and water are mixed at a predetermined ratio.
- an oxidizing agent other than hydrogen peroxide may be used, and an acid or base other than acetic acid or ammonia may be used as the oxide removing agent.
- ammonium fluoride may be used as an oxide remover.
- an example using an etching solution in which the silver brazing of the brazing material layer 11 is easily etched and the Fe—Ni—Co alloy of the base material layer 10 is not easily etched is shown.
- the present invention is not limited to this.
- an etchant that etches the Fe—Ni—Co alloy of the base material layer to some extent may be used. Thereby, it is possible to omit the step of performing barrel polishing for removing the minute protrusions or to shorten the time for performing barrel polishing.
- examples using silver brazing mainly containing about 85% by mass of Ag and Cu are shown, but the present invention is not limited to this.
- a silver solder mainly containing about 72% by mass of Ag and Cu may be used.
- a brazing material containing Sn other than Ag and Cu may be used. In this case, since the solidus line of the brazing material can be reduced, the brazing temperature can be lowered.
- the brazing material includes Sn, it is preferable to include Sn in an amount of about 6% by mass or less in order to prevent the rolling from becoming difficult when forming the clad material.
- the strong acid composed of dilute sulfuric acid is used as the solution added to the stock solution or the diluent, but the present invention is not limited to this.
- a strong acid other than sulfuric acid such as hydrochloric acid may be added to the stock solution or the diluted solution.
- a solution other than a strong acid may be used as the Cu preferential removal agent.
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Abstract
Description
まず、図1~図3を参照して、本発明の第1実施形態によるシールリング1の構造を説明する。
次に、図3、図4、図7、図10および図11を参照して、本発明の第1実施形態の効果を確認するために行ったエッチング状態の観察、金属溶出量測定、および、ろう材層の溶融状態の観察について説明する。
まず、ウェットエッチングの処理時間を異ならせた場合の、ろう材層の状態の変化を観察した。この観察では、上記第1実施形態のシールリング1b(図7参照)を用いた。また、エッチング液として、酢酸を25質量%含有する酢酸水と、過酸化水素を35質量%含有する過酸化水素水と、水とを1:5:4の体積比で混合した原液を準備した。その後、原液と水との体積比が1:1となる1:1希釈液を作製してエッチング液とした。そして、シールリング1bとエッチング液とをバレルに投入して、バレルを所定の速度で回転させた。その後、所定の処理時間ごとに側面ろう材部分11f(図7参照)付近のエッチング状態を、走査型電子顕微鏡(S-3400N、日立ハイテクノロジーズ社製)を用いて観察した。
次に、基材層を形成するFe-Ni-Co合金のエッチング液への溶出量と、ろう材層を形成する85質量%のAgとCuとを主に含む銀ろうのエッチング液への溶出量とを測定した。具体的には、上記シールリング1bと、エッチング液(上記原液と水との体積比が1:1となる1:1希釈液)とをバレルに投入して、バレルを所定の速度で1時間回転させた。これにより、シールリング1bのろう材層がほとんど溶解した。そして、エッチング液に含まれるAg、Cu、Fe、NiおよびCoを、ICP発光分析装置を用いて測定した。
次に、ろう材層の溶融状態を観察した。このろう材層の溶融状態の観察では、側面ろう材部分11f(図7参照)が除去された実施例1のシールリング1(図3参照)と、側面ろう材部分11fが除去されていない比較例1のシールリング(シールリング1b、図7参照)とにおいて、ろう材層11を溶融させた際のろう材層11の溶融状態の観察を行った。
次に、図3を参照して、本発明の第2実施形態によるシールリング301の構造を説明する。この第2実施形態によるシールリング301では、上記第1実施形態のシールリング1とは異なり、ろう材層311の表面近傍におけるAgの濃度が、ろう材層311の内部11gにおけるAgの濃度よりも大きい場合について説明する。
次に、図3、図7および図12~図15を参照して、本発明の第2実施形態の効果を確認するために行ったろう材層の表面での濃度の測定、ろう材層の深さ方向での濃度の測定、固相線の測定、および、耐食性試験について説明する。
まず、ろう材層の表面でのCuおよびAgの濃度を測定した。この測定では、Fe-Ni-Co合金により形成された基材層10と、85質量%のAgと15質量%のCuとからなる銀ろうにより形成されたろう材層11とを備えるシールリング1b(図7参照)を準備した。そして、比較例2のシールリングとして、ウェットエッチングを行わずに、シールリング1bをそのまま用いた。一方、実施例2および3では、シールリング1bに対してウェットエッチングを行った。
次に、上記実施例3のシールリング301を用いて、オージェ電子分光装置により、ろう材層の深さ方向(ろう材層311の表面に対して直交する方向)でのCuおよびAgの濃度を測定した。
次に、ウェットエッチング前後でのろう材層の固相線の変化を確認するために固相線の測定を行った。この固相線の測定では、上記した比較例2および実施例3に加えて、上記1:4希釈液に添加する硫酸の濃度を各々異ならせたエッチング液を用いてウェットエッチングを行うことによって、実施例4~6のシールリング301を製造した。ここで、実施例4、5および6では、それぞれ、硫酸の濃度がエッチング液全体の0.3質量%、0.5質量%および1.0質量%になるように調整した。なお、実施例4~6におけるウェットエッチングの条件は、上記実施例3の条件と同一である。そして、示差熱分析(DTA)法を用いて、比較例2のシールリング1bおよび実施例3~6のシールリング301におけるろう材層の固相線(ろう材層の一部が溶け始める温度)を測定した。
次に、耐食性試験を行った。この耐食性試験では、上記した比較例2のシールリング1bおよび実施例3のシールリング301を、85℃および85%Rh(相対湿度)の恒温恒湿条件下で1000時間放置する恒温恒湿試験を行った。そして、恒温恒湿試験後の比較例2のシールリング1bおよび実施例3のシールリング301の表面を、電子線マイクロアナライザ(Electron Probe MicroAnalyser:EPMA)を用いて観察した。そして、ろう材層の表面におけるO(酸素)の濃度(存在比)、Cuの濃度およびAgの濃度を求めた。
6 異物
10 基材層
10b 下面(一方表面)
10c 側面
10f 微小突起
11、311 ろう材層
11f 側面ろう材部分
11g 内部
100 電子部品収納用パッケージ
200 クラッド材
Claims (20)
- 電子部品収納用パッケージ(100)に用いられるシールリング(1)であって、
基材層(10)と、
前記基材層の一方表面(10b)に配置されたろう材層(11)とが接合されたクラッド材から構成され、
前記ろう材層のうちの前記基材層の側面(10c)を覆う側面ろう材部分(11f)が除去されている、シールリング。 - 前記基材層は、前記基材層の前記一方表面と略平坦面状に形成された前記側面とを接続する丸形状の角部(10e)を含み、
前記ろう材層のうちの前記略平坦面状の側面を覆う前記側面ろう材部分が少なくとも除去されている、請求項1に記載のシールリング。 - 前記基材層は、FeとNiとCoとを主に含み、
前記ろう材層は、AgとCuとを主に含む、請求項1に記載のシールリング。 - 前記ろう材層は、AgとCuとを主に含み、
前記ろう材層の表面近傍におけるAgの濃度は、前記ろう材層の内部(11g)におけるAgの濃度よりも大きい、請求項1に記載のシールリング。 - 電子部品収納用パッケージ(100)に用いられるシールリング(1)の製造方法であって、
基材層(10)と前記基材層の一方表面(10b)に接合されるろう材層(11)とのクラッド材(200)を準備する工程と、
前記クラッド材を前記シールリングの形状に打ち抜く工程と、
前記クラッド材を前記シールリングの形状に打ち抜く際に前記ろう材層が延伸して形成された、前記ろう材層のうちの前記基材層の側面(10c)を覆う側面ろう材部分(11f)を除去する工程とを備える、シールリングの製造方法。 - 前記基材層は、前記基材層の前記一方表面と略平坦面状に形成された前記側面とを接続する丸形状の角部(10e)を含み、
前記側面ろう材部分を除去する工程は、前記ろう材層のうちの前記略平坦面状の側面を覆う前記側面ろう材部分を少なくとも除去する工程を含む、請求項5に記載のシールリングの製造方法。 - 前記側面ろう材部分を除去する工程は、前記側面ろう材部分をウェットエッチングにより除去する工程を含む、請求項5に記載のシールリングの製造方法。
- 前記側面ろう材部分を前記ウェットエッチングにより除去する工程は、前記ろう材層を前記ウェットエッチングにより等方的に除去することにより、前記側面ろう材部分を除去する工程を含む、請求項7に記載のシールリングの製造方法。
- 前記ろう材層を前記ウェットエッチングにより等方的に除去する工程は、前記ウェットエッチングにより、前記側面ろう材部分を除去するとともに、前記ろう材層の角部(11e)を丸形状に形成する工程を含む、請求項8に記載のシールリングの製造方法。
- 前記側面ろう材部分を前記ウェットエッチングにより除去する工程は、前記ろう材層がエッチングされやすく、かつ、前記基材層がエッチングされにくいエッチング液を用いて、前記側面ろう材部分を除去する工程を含む、請求項7に記載のシールリングの製造方法。
- 前記基材層は、FeとNiとCoとを主に含み、
前記ろう材層は、AgとCuとを主に含み、
前記エッチング液は、前記ろう材層の表面を酸化させる酸化剤と、酸化された前記ろう材層を除去する酸化物除去剤と、水とを少なくとも含む、請求項10に記載のシールリングの製造方法。 - 前記エッチング液は、過酸化水素により構成される前記酸化剤と、酢酸により構成される前記酸化物除去剤と、前記水とを少なくとも含む、請求項11に記載のシールリングの製造方法。
- 前記ろう材層は、AgとCuとを主に含み、
前記ウェットエッチングのエッチング液は、前記ろう材層の表面を酸化させる酸化剤と、酸化された前記ろう材層を除去する酸化物除去剤と、水と、前記ろう材層の表面のCuを優先的に除去するためのCu優先除去剤とを含み、
前記側面ろう材部分を前記ウェットエッチングにより除去する工程は、前記エッチング液を用いて前記ろう材層の表面におけるCuを優先的に除去することにより、前記ろう材層の表面近傍におけるAgの濃度を、前記ろう材層の内部(11g)におけるAgの濃度よりも大きくする工程を含む、請求項7に記載のシールリングの製造方法。 - 前記ろう材層は、AgとCuとを主に含み、
前記ウェットエッチングのエッチング液は、前記ろう材層の表面を酸化させる酸化剤と、酸化された前記ろう材層を除去する酸化物除去剤と、水と、前記ろう材層の表面のCuを優先的に除去するためのCu優先除去剤とを含み、
前記側面ろう材部分を前記ウェットエッチングにより除去する工程は、前記エッチング液を用いて前記ろう材層の表面におけるCuを優先的に除去することにより、前記ろう材層の表面近傍におけるAgの濃度を、前記側面ろう材部分を前記ウェットエッチングにより除去する前の前記ろう材層におけるAgの濃度よりも大きくする工程を含む、請求項7に記載のシールリングの製造方法。 - 前記Cu優先除去剤は、強酸により構成されている、請求項13に記載のシールリングの製造方法。
- 前記Cu優先除去剤は、前記強酸である硫酸により構成されている、請求項15に記載のシールリングの製造方法。
- 前記エッチング液には、前記硫酸が前記エッチング液全体の0.5質量%以上の濃度になるように添加されている、請求項16に記載のシールリングの製造方法。
- 前記側面ろう材部分を前記ウェットエッチングにより除去する工程の前後で前記ろう材層の固相線は略変化しない、請求項13に記載のシールリングの製造方法。
- 前記側面ろう材部分を前記ウェットエッチングにより除去する工程は、前記シールリングの表面に残った酸化された前記ろう材層を取り除いて洗浄する工程を兼ねる、請求項13に記載のシールリングの製造方法。
- 前記側面ろう材部分を前記ウェットエッチングにより除去する工程に先立って、前記クラッド材を前記シールリングの形状に打ち抜く際に形成された前記基材層の微小突起(10f)を除去する工程をさらに備え、
前記側面ろう材部分をウェットエッチングにより除去する工程は、前記側面ろう材部分と、前記微小突起を除去する際に付着する異物(6)とを前記ウェットエッチングにより除去する工程を含む、請求項7に記載のシールリングの製造方法。
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KR20170091684A (ko) * | 2015-01-29 | 2017-08-09 | 히타치 긴조쿠 가부시키가이샤 | 기밀 밀봉용 덮개재 및 전자 부품 수납 패키지 |
EP3252807A4 (en) * | 2015-01-29 | 2018-08-08 | Hitachi Metals, Ltd. | Cover material for hermetic sealing and electronic component-containing package |
KR101941805B1 (ko) * | 2015-01-29 | 2019-01-23 | 히타치 긴조쿠 가부시키가이샤 | 기밀 밀봉용 덮개재 및 전자 부품 수납 패키지 |
JP2017076913A (ja) * | 2015-10-15 | 2017-04-20 | エスアイアイ・クリスタルテクノロジー株式会社 | パッケージ及び圧電振動子 |
JP2021068888A (ja) * | 2019-10-23 | 2021-04-30 | 日立金属株式会社 | ろう材付き基材の製造方法およびろう材付き基材 |
JP7127673B2 (ja) | 2019-10-23 | 2022-08-30 | 日立金属株式会社 | ろう材付き基材の製造方法 |
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TW201409634A (zh) | 2014-03-01 |
US20180213668A1 (en) | 2018-07-26 |
JP6070702B2 (ja) | 2017-02-01 |
US20150342072A1 (en) | 2015-11-26 |
JPWO2013183315A1 (ja) | 2016-01-28 |
US10188010B2 (en) | 2019-01-22 |
KR20150023236A (ko) | 2015-03-05 |
CN104364895B (zh) | 2017-09-26 |
US9961791B2 (en) | 2018-05-01 |
KR101676149B1 (ko) | 2016-11-14 |
CN104364895A (zh) | 2015-02-18 |
TWI612629B (zh) | 2018-01-21 |
HK1204149A1 (en) | 2015-11-06 |
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