CN106715039A - Sealing paste, brazing material and production method thereof, sealing lid member and production method thereof, and package sealing method - Google Patents
Sealing paste, brazing material and production method thereof, sealing lid member and production method thereof, and package sealing method Download PDFInfo
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- CN106715039A CN106715039A CN201580051707.8A CN201580051707A CN106715039A CN 106715039 A CN106715039 A CN 106715039A CN 201580051707 A CN201580051707 A CN 201580051707A CN 106715039 A CN106715039 A CN 106715039A
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- powder
- sealing
- lid
- soldered joint
- slurry
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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
- 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
-
- 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
-
- 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
- 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
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
This sealing paste contains a starting material powder and a binder, the starting material powder containing 5-40 mass% of a low melting point metal powder having a 0.5-20.0 [mu]m average particle diameter and a melting point or liquidus temperature of less than 240 DEG C, 40-90 mass% of an Ag powder having an average particle diameter of 0.1-10.0 [mu]m, and 5-50 mass% of a Cu powder having an average particle diameter of 0.1-10.0 [mu]m. The sealing paste can easily form a brazing material, the alloy composition of said brazing material can be changed easily, and the sealing paste can reliably seal a package hermetically without resulting in cracking.
Description
Technical field
Make the present invention relates to a kind of sealing slurry, soldered joint material and packaging body encapsulating method, more particularly to one kind
The free degree is high with supply, the sealing slurry of the easy mixed powder slurry of composition control, soldered joint material and its manufacture method,
Sealing lid material and its manufacture method and packaging body encapsulating method.
The application is advocated based on Japanese patent application filed in 31 days October in 2014 2014-222900, in August, 2015
Japanese patent application filed in 24 days No. 2015-164700 and Japanese patent application 2015- filed in 29 days October in 2015
The priority of No. 213467, and its content is quoted herein.
Background technology
Typically, the solder with the fusing point less than 450 DEG C is used as sealing material, or using with more than 450 DEG C
Fusing point brazing material.And, in order to use lid material sealed package, quilt as described in Patent Document 1 is also sandwiched sometimes
Referred to as the material of sealing ring implements the material of Nickel Plating Treatment or close as encapsulant in the sealing of lid material or packaging body
Seal ring sealing in itself implements the material of nickel plating.In addition, also using glass or resin sometimes as encapsulant.
The quality %Sn (tin) of Pb (lead) -63 or quality %Cu (copper) of Sn-3 mass %Ag (silver) -0.5 can be used in wlding
Deng unleaded wlding, Pb-10 mass %Sn or Au (gold) -20 quality %Sn high-temperature solder.Can mainly make as brazing material
Ag solderings are used, such as headed by Ag-28 mass %Cu, Ag-22 mass %Cu-17 mass %Zn (zinc) -5 quality %Sn or is contained
There are the Ag brazing alloys of Cd (cadmium) or Ni.There are cobalt or 42 alloys etc. as sealing ring or lid material, to these implementation Nickel Plating Treatments.
As the Sealing Method using sealing ring, when using wlding, solder plate and sealing ring circlewise will be processed sometimes
Sandwich together between lid material and packaging body, melted and sealed using stove or baking oven, or using soldering paste etc. in lid material shape
After solder frame circlewise, sealed with packaging body.When on the other hand, using Ag solderings, the Ag prickers of ring-type will be punched into
Welding plate, sandwiches between lid material and packaging body together with sealing ring, is only made close using seamed bonding machine or laser-beam welding machine etc.
Envelope portion locally turns into the condition of high temperature and melts and seal Ag solderings or be formed at the nickel plating of sealing ring.
Using in the Sealing Method of sealing ring, sealing ring turns into padded coaming, and seamed welding is being used therefore, it is possible to relax
Deng thermal shock when sealing or mechanical stress.
But, during using Ag solderings with being sealed with welding with the sealing ring of nickel plating, it is necessary to be sandwiched in lid material with encapsulation
Sealed after between body, the efficiency of contraposition etc. is poor, bothered very much.
It is therefore proposed that have one kind Ag brazing alloys are done powdered and slurried, be printed on lid material, be heat-treated and
The method for forming sealing frame.
Have disclosed in patent document 2, in the sealing metal paste containing metal dust and organic solvent, with
It is more than 99.9 weight % comprising purity as metal dust, average grain diameter is 0.1 μm~1.0 μm of bronze, silver powder, platinum powder
Or the sealing metal paste of the ratio allotment of the weight % of metal dust 85~93, the weight % of organic solvent 5~15 of palladium powder.Make
It is, using the encapsulating method of the metal paste, to record and coat abutment part or cap member and make its dry metal paste,
After using 80~300 DEG C of sintering as sinter from metal powder, sinter from metal powder is heated while abutment portion of pressurizeing
The method of part and cap member.
Described metal paste is the gold of the independent metal powder using bronze, silver powder, platinum powder or palladium powder in patent document 2
Category slurry, is not the metal paste for making these metallic alloying.
Have disclosed in patent document 3 and contain the base material being made up of low thermal expansion metal base and be bonded on the base material at least
The silver brazing clad material of the low form silver system utilizingthebrazing material layer on surface.The silver system utilizingthebrazing material layer is by coating by low temperature
After mixing the slurry of the medium being made up of solvent and binding agent in the metal dust that type silver system brazing material is constituted, carry out
Heat and rapidly cooled and solidified after melting metal powder, and further rolling processing and formed.Specific silver system brazing material can
Enumerate silver-copper-tin alloy, silver-copper-indium alloy, silver-copper-kirsite.By the silver brazing clad material by Punching Technology etc.
Given size is processed into, packaging body sealing lid material is consequently formed.
Have that a kind of will to contain be not that silver is brazing material but the pulp-like soldering of Au and Sn disclosed in patent document 4
Material compositions are printed on the one side of cap, are then heated with the temperature more than fusing point of Sn and below the fusing point of Au,
It is consequently formed the cap of fusion Au-Sn brazing materials, and the technology that the cap is overlapped packaging body and fused.
Patent document 1：Japanese Unexamined Patent Publication 9-293799 publications
Patent document 2：Japanese Unexamined Patent Publication 2008-28364 publications
Patent document 3：Japanese Unexamined Patent Publication 2006-49595 publications
Patent document 4：Japanese Unexamined Patent Publication 2003-163299 publications
But the situation of Ag soldering slurries is, must be carried out with the high temperature more than fusing point of Ag solderings when sealing frame is formed
After heat treatment, soldering is carried out during sealing again.Being additionally, since the powder of Ag brazing alloys carries out making powder, it is desirable to
When being made up of different-alloy, it is necessary to manufacture alloy again, make powder treatment, cause very big trouble.
And, the seamed welding of the so-called vertical masonry joint method of sealing ring is not used or uses method of laser welding, electron beam welding
Method etc. and when being sealed, sealing is locally turned into the condition of high temperature and is sealed, therefore with thermal shock or mechanically stressed
And it is also easy to produce cracking in bonding layer or packaging body.
The content of the invention
Soldered joint material can be easily formed it is an object of the invention to provide one kind, and can easily change its soldered joint
The alloy composition of material, and do not produce cracking and be capable of sealing slurry, the soldered joint of reliably gas-tight seal packaging body
Material and its manufacture method, sealing lid material and its manufacture method and packaging body encapsulating method.
Sealing of the invention includes material powder and binding agent with slurry, and the material powder contains more than 5 mass % 40
The average grain diameter of below quality % is less than more than 0.5 μm 20.0 μm and the low melting point of fusing point or liquidus temperature less than 240 DEG C
Metal dust, Ag powder and 5 matter that the average grain diameter of below the mass % of more than 40 mass % 90 is less than more than 0.1 μm 10.0 μm
The average grain diameter for measuring below the mass % of more than % 50 is less than more than 0.1 μm 10.0 μm of Cu powder.
In sealing slurry of the invention, the average grain diameter of the metal powder with low melting point is preferably the Ag powder
Less than more than 1 times 10 times of average grain diameter and less than more than 1 times 10 times of the average grain diameter for the Cu powder.
In sealing slurry of the invention, the average grain diameter of the metal powder with low melting point is preferably greater than the Ag powder
Average grain diameter and the Cu powder average grain diameter.
And, in sealing slurry of the invention, blending ratio preferably 50 matter of more than 2 mass % of the binding agent
Amount below %.
And, in sealing slurry of the invention, the metal powder with low melting point can be used and be selected from Sn, In, Sn-Ag-
One or more of Cu solder alloys, Sn-Cu solder alloys, Sn-Bi solder alloys and Sn-In solder alloys.
Have in the manufacture method of soldered joint material of the invention：The sealing slurry is coated on the slurry on carrier
Material painting process and heat treatment step, the heat treatment step will be coated on the sealing slurry of the carrier with described low
The melt temperature of melting point metals heated and made the liquid phase of the low-melting-point metal the Ag powder and the Cu powder it
Between permeate after cool and solidify, be consequently formed the binder course that the Ag powder and the Cu powder are formed by the low-melting-point metal
And the soldered joint material of the porosity more than 10% being concatenated.In addition, the soldered joint material is in order to ensure intensity and sealing
Property, is preferably formed into the porosity below 35%.
Soldered joint material of the invention, with Ag powder, average grain that average grain diameter is less than more than 0.1 μm 10.0 μm
Footpath is less than more than 0.1 μm 10.0 μm of Cu powder and the low-melting-point metal shape by fusing point or liquidus temperature less than 240 DEG C
Into and for link the binder course of the Ag powder and the Cu powder, the porosity is more than 10%, and quality ratio is, described
Ag powder is below the mass % of more than 40 mass % 90, and the Cu powder is below the mass % of more than 5 mass % 50, the combination
Layer is below the mass % of more than 5 mass % 40.
The manufacture method of sealing lid material of the invention has：The sealing slurry is coated on the slurry on the surface of lid
Material painting process and heat treatment step, the heat treatment step is the sealing slurry that will be coated on the lid with described
The melt temperature of low-melting-point metal is heated and is made the liquid phase of the low-melting-point metal in the Ag powder and the Cu powder
Between permeate after cool and solidify, be consequently formed the combination that the Ag powder and the Cu powder are formed by the low-melting-point metal
Layer and the soldered joint material of the porosity more than 10% that is concatenated.In addition, the soldered joint material is preferably formed into the porosity
Less than 35%.
In manufacture method of the sealing of the invention with lid material, after the heat treatment step, there can be removal by remaining
The binding agent removing step of the binding agent in the soldered joint material, and, the binding agent removing step is to have：With
Cleaning fluid cleans the cleaning treatment of soldered joint material；And it is heat-treated the drying of the cleaned soldered joint material
Treatment.
In manufacture method of the sealing with lid material, in the slurry painting process, multiple lids are being formed
The sealing slurry is coated with the plate surface of size, and after the heat treatment step, can be had the sheet material
It is divided into the singualtion operation of the lid.
Sealing lid material of the invention has：Lid；And it is located at the soldered joint material of the top surface.
Packaging body encapsulating method of the invention is the packaging body encapsulating method by brazing alloy bonding packaging body and lid,
It has slurry painting process, heat treatment step and alloying step, and the slurry painting process applies the sealing with slurry
Cloth is on the surface of the lid；The heat treatment step will be coated on the sealing slurry of the lid with the low melting point
The melt temperature of metal is heated and the liquid phase of the low-melting-point metal is oozed between the Ag powder and the Cu powder
Cooling and solidifying after thoroughly, be consequently formed the Ag powder and the Cu powder by binder course that the low-melting-point metal is formed quilt
The soldered joint material of the porosity more than 10% of link；The alloying step, the encapsulation is overlapped by the lid
The state heating of body melts the soldered joint material and carries out alloying, so as to as the brazing alloy.In addition, the pricker
Welding condensation material is preferably formed into the porosity below 35% in order to ensure intensity and sealing etc..
In packaging body encapsulating method of the invention, between the heat treatment step and the alloying step, can have
There is removal to remain in the binding agent removing step of the binding agent in the soldered joint material, and, the binding agent removing step
There can be the cleaning treatment that the soldered joint material is cleaned with cleaning fluid, and be heat-treated the cleaned soldering and connect
The drying and processing of condensation material.
In packaging body encapsulating method of the invention, in the slurry painting process, multiple lids are being formed
The sealing slurry is coated with the plate surface of size, and after the heat treatment step, can be had the sheet material
It is divided into the singualtion operation of the lid.
In packaging body encapsulating method of the invention, after the singualtion operation, there can be the table to the lid
Implement the electroplating processes operation of metal plating in face.Metal plating treatment is implemented as the metallization of lid, and is divided into lid
Laggard row metal electroplating processes, so as to metal plating can be implemented to the side wall of lid, and can effectively prevent side wall corrosion and
Get rusty.
Packaging body encapsulating method of the invention is the encapsulation engaged in packaging body overlap lid and by brazing alloy
Body encapsulating method, it carries out slurry painting process, heat treatment step and alloying step, and the slurry painting process will be described close
Envelope slurry is coated on carrier；The heat treatment step will be coated on the sealing slurry of the carrier with the eutectic
The melt temperature of point metal is heated and is made the liquid phase of the low-melting-point metal between the Ag powder and the Cu powder
Cooled and solidified after infiltration, be consequently formed the Ag powder and the Cu powder by binder course that the low-melting-point metal is formed
The soldered joint material of the porosity more than 10% being concatenated；The soldered joint material is layered in institute by the alloying step
After stating between packaging body and the lid, heating melts the soldered joint material and carries out alloying, so as to as the pricker
Solder alloy.In addition, the soldered joint material is preferably formed into the porosity below 35%.
The material powder for being blended in sealing slurry of the invention contains the eutectic of fusing point or liquidus temperature less than 240 DEG C
Point metal dust and fusing point are higher than the Ag powder of the metal powder with low melting point and the material powder of Cu powder.Also, as described above
The sealing slurry that the average grain diameter or fit rate of each metal dust, the fit rate of binding agent are managed is with the molten of low-melting-point metal
Melt temperature heating, thus the soldered joint material of gained is the soldered joint material of the gained in heat treatment step, makes eutectic
During point metal powders melt, fusing point is direct higher than the Ag powder of low-melting-point metal and the major part of Cu powder with solid remaining, should
The liquid phase of low-melting-point metal is permeated and is cooled and solidified between the Ag powder and Cu powder of these solids, thus Ag powder and Cu powder
End turns into the state of mutually bonding by the binder course that low-melting-point metal is formed.Now, before being heated by heat treatment step
Exist and formed at metal powder with low melting point many spaces, thus, soldered joint material is formed as the porous of the porosity more than 10%
Structure.
If the material powder of sealing slurry will be blended in as silver brazing alloy powder, when formation soldered joint material
When, it is necessary to it is heated to more than the melt temperature of silver brazing alloy (liquidus temperature).Soldered joint material use of the invention is low
The liquid-phase sintering of melting point metals powder and formed with (the being less than 240 DEG C) heating of the melt temperature of low-melting-point metal, therefore stove etc.
Energy-conservation need not be realized using the equipment of high temperature.
Also, when using soldered joint material of the invention and sealed package with lid, even if using there is seam weld
The sealing that only makes of connection or method of laser welding, electron beam welding method etc. is partially formed in the encapsulating method of the condition of high temperature, soldering
The vesicular structure of grafting material can relax thermal shock or mechanical stress, therefore can prevent bonding layer or packaging body from producing cracking.And
And, soldered joint material makes Ag and Cu and low-melting point metal alloy to be heated to the melt temperature of Ag powder and Cu powder,
Thereby, it is possible to reliably gas-tight seal packaging body and lid.
And, sealing slurry of the invention can be coated on the surface of carrier or lid by the method for printing etc., therefore
The soldered joint material (sealing frame) of desired shape can easily be formed.Soldered joint of the invention is formed on the surface of lid
During material, soldered joint material is fixed on the surface of lid by the low-melting-point metal for melting, therefore can hold on the surface of lid
The soldered joint material of stabilization is easily formed, and when lid is operated in the absence of the situation of soldered joint material falls back.And, to press from both sides
The state for being firmly bonded to the soldered joint material of sealing lid material and overlapping packaging body implements alloying step, therefore can be simultaneously
Alloying and the sealing of soldered joint material are carried out, thus it is efficient.
Being blended in the material powder combination of sealing slurry of the invention has various metals powder, therefore can easily change each
The fit rate of metal dust or combination, and can easily change alloy composition.
When the average grain diameter of the Ag powder and Cu powder that are blended in sealing slurry is less than 0.1 μm, the soldering for being formed connects
The porosity of condensation material gets lower than 10%, it is difficult to obtain relaxing the effect of thermal shock or mechanical stress.On the other hand, Ag powder
And the average grain diameter of Cu powder more than 10 μm when, the porosity of the soldered joint material for being formed becomes big, and sealing is deteriorated.This hair
The porosity of bright involved soldered joint material is preferably more than 10% and less than 35%.If the porosity of soldered joint material
More than 35%, then there is the possibility of sealing reduction.
When the average grain diameter of metal powder with low melting point is less than 0.5 μm, the porosity of the soldered joint material for being formed also becomes
10% must be less than, it is difficult to obtain relaxing the effect of thermal shock or mechanical stress, the average grain diameter of metal powder with low melting point is more than 20 μ
During m, the porosity of the soldered joint material for being formed becomes big, and sealing is deteriorated.
When the containing ratio of Ag powder is less than 40 mass % in material powder entirety, from Ag, Cu and low-melting-point metal
Eutectic composition significantly deviates, therefore sealing reduction, during more than 90 mass %, when for the cleaning for removing binding agent residue,
It is possible to be peeled off from lid for being bonded to soldered joint material etc., and because expensive Ag is more, cost uprises.
The containing ratio of the Cu powder in material powder entirety be it is more than 5 mass % outside the scope of below 50 mass % when,
When i.e., less than 5 mass % or more than 50 mass %, significantly deviate from the eutectic composition of Ag, Cu and low-melting-point metal, therefore sealing
Property reduce.
When the containing ratio of the metal powder with low melting point in material powder entirety is less than 5 mass %, because of the formation of binder course
Insufficient and be possible to when cleaning be peeled off from lid for being bonded to soldered joint material etc., during more than 40 mass %, superfluous is low
Melting point metals can also be remained (after alloying) after sealing, with eutectic temperature (such as Ag- than Ag, Cu and low-melting-point metal
The eutectic temperature of Cu-Sn) the low melting point temperature region of low fusing point can be produced in sealing, therefore with expect at least 450 DEG C with
On fusing point conversely, a part for sealing be possible to low-melting-point metal fusing point (less than soldered joint material melting temperature
Degree) melting.And, when the containing ratio of this metal powder with low melting point is more than 40 mass %, from being total to for Ag, Cu and low-melting-point metal
Crystalline substance composition significantly deviates, and sealing is also reduced.
When binding agent is less than 2 mass % or binding agent more than 50 mass %, even if being kneaded with material powder, it is also difficult to formed
It is suitable to the pulp-like of printing process.And, when especially binding agent is more than 50 mass %, keep the binding agent of Ag powder and Cu powder
Shape is unable to maintain that by thermal softening, it is difficult to soldered joint material is formed desired shape.
According to the present invention, brazing alloy composition can be easily changed, by the soldered joint material with porous structure
Cracking will not be produced, being capable of reliably gas-tight seal packaging body.
Brief description of the drawings
The schematic diagram of the composition of Figure 1A involved to illustrate the invention sealing slurry.
The schematic diagram of the composition of Figure 1B involved to illustrate the invention soldered joint material.
Fig. 2 is to represent that the surface in carrier involved in the present invention is coated with the top view of the state of sealing slurry.
Fig. 3 is to represent that the surface in lid material involved in the present invention forms the sealing lid material of soldered joint material
Top view.
Fig. 4 is the stravismus of the significant points of the sheet material of the state of the printing coating sealing slurry for representing involved in the present invention
Figure.
Fig. 5 A are the front view of the operation that sealing lid material is layered in packaging body for representing involved in the present invention.
Fig. 5 B are bonded on the main view of the operation of packaging body by the expression sealing lid material that will be laminated involved in the present invention
Figure.
Specific embodiment
Hereinafter, refer to the attached drawing explanation embodiments of the present invention.
The composition ＞ of ＜ sealing slurries
First, the manufacture method for soldered joint material of the invention involved in the present invention or encapsulating method are illustrated
Sealing slurry 20.
As shown in Figure 1A, sealing slurry 20 is that hybrid adhesive 25 is formed in material powder, and the material powder contains
There are the metal powder with low melting point 23 of fusing point or liquidus temperature less than 240 DEG C and fusing point higher than the Ag of metal powder with low melting point 23
Powder 21 and Cu powder 22.
It is less than more than 0.1 μm 10.0 μm and below the mass % of more than 40 mass % 90 that material powder contains average grain diameter
Ag powder 21, contains the Cu powder that average grain diameter is less than more than 0.1 μm 10.0 μm and below the mass % of more than 5 mass % 50
22, contain the metal powder with low melting point that average grain diameter is less than more than 0.5 μm 20.0 μm and below the mass % of more than 5 mass % 40
23, and these Ag powder 21, Cu powder 22 and metal powder with low melting point 23 are suitably mixed in above-mentioned number range.
And, each containing ratio of these Ag powder 21, Cu powder 22 and metal powder with low melting point 23 is the ratio relative to material powder
Rate.
Be can be used as metal powder with low melting point 23 and closed selected from Sn, In, Bi, Sn-Ag-Cu solder alloy, Sn-Cu solders
One or more of gold, Sn-Bi solder alloys, Sn-In solder alloys.In addition, the Sn-Ag- as metal powder with low melting point 23
Any one of Cu solder alloys, Sn-Cu solder alloys, Sn-Bi solder alloys, Sn-In solder alloys contain Sn, for example, turn into
The ratio of components of 96.5 mass %Sn-3.0 mass %Ag-0.5 mass %Cu, 99.3 mass %Sn-0.7 mass Cu etc..
Binding agent 25 is made up of above rosin, activating agent, solvent, thixotropic agent, at least one of other additives.
Sealing with slurry 20 by by binding agent 25 with the ratio (ratio in slurry of below the mass % of more than 2 mass % 50
Rate) mix with material powder and constitute.
In addition, when the average grain diameter of Ag powder 21 and Cu powder 22 is less than 0.1 μm, being formed using sealing slurry 20
The porosity of soldered joint material is less than 10%, it is difficult to obtain relaxing the effect of thermal shock or mechanical stress.On the other hand, Ag powder
When the average grain diameter of end 21 and Cu powder 22 is more than 10 μm, the porosity of the soldered joint material for being formed becomes big, and sealing becomes
Difference.
And, when the average grain diameter of metal powder with low melting point 23 is less than 0.5 μm, the stomata of the soldered joint material for being formed
Rate also gets lower than 10%, it is difficult to obtain relaxing the effect of thermal shock or mechanical stress.The average grain of metal powder with low melting point 23
When footpath is more than 20 μm, the porosity of the soldered joint material for being formed becomes big, and sealing is deteriorated.
The average grain diameter of metal powder with low melting point 23 more than 0.5 μm in less than 20.0 μm of scope, with Ag powder 21 and
The average grain diameter of Cu powder 22 is identical, or is preferred more than it.Specifically, the average grain diameter of metal powder with low melting point 23 is Ag
Less than more than 1 times 10 times of the average grain diameter of powder 21 and Cu powder 22 are preferred, and less than more than 1 times 5 times is it is further preferred that 1.25
Less than 5 times is even more preferably more than times.
Sealing reduction when the containing ratio of the Ag powder 21 in material powder entirety is less than 40 mass %, more than 90 matter
During amount %, can be peeling when for the cleaning for removing binding agent residue, cost is further uprised.And, Cu powder 22
Containing ratio be it is more than 5 mass % outside the scope of below 50 mass % when, i.e. it is close during less than 5 mass % or more than 50 mass %
Envelope property is reduced.And, when the containing ratio of metal powder with low melting point 23 is less than 5 mass %, can be peeling during cleaning, more than 40
During quality %, low melting point temperature region can be produced, so as to a part under the melt temperature less than brazing alloy, may be caused molten
Melt.And, when the containing ratio of metal powder with low melting point 23 is more than 40 mass %, sealing is also reduced.
Binder phase for sealing with the containing ratio of slurry 20 less than 2 mass % or more than 50 mass % when, even if with
Material powder is kneaded, it is also difficult to form the pulp-like for being suitable to print engineering method.Especially, when binding agent is more than 50 mass %, soldering
When grafting material is formed, binding agent can be squeezed except Ag powder and Cu powder, cause to be difficult to the soldered joint of the shape to form desired
Material.
The composition and manufacture method ＞ of ＜ soldered joint materials
The method of the manufacture soldered joint of above sealing slurry 20 material 4 is used in reference to Fig. 2 explanations.
The manufacture method of soldered joint material 4 has：Described sealing slurry 20 is printed and is coated with carrier 3
Slurry painting process；It is coated at heat of the sealing of carrier 3 with slurry 20 with the melt temperature heating of metal powder with low melting point 23
Science and engineering sequence；And the binding agent removing step of binding agent is removed after the heat treatment step.
＜ slurry painting process ＞
Prepare the carrier 3 of the ceramic substrate that will not merge of brazing material etc., on the surface of the carrier 3, shape as desired
Shape, for example, be directed at the sealing described in frame-shaped or sheet the printing coating of the shape of the peripheral part Chong Die with the packaging body of top surface
With slurry 20 (Fig. 2).Sealing slurry 20 can also be spued on supply to carrier 3 by point gum machine etc..
[heat treatment step]
Carrier 3 to being coated with sealing slurry 20 implements low temperature reflow treatment, forms soldered joint material 4.It is specific and
Speech, will be coated on the sealing slurry 20 of carrier 3 and is heated to contained low melting point gold in sealing slurry 20 in a nitrogen environment
Belong to more than the melt temperature of powder 23 is more than the fusing point or liquidus temperature of metal powder with low melting point 23 and less than Ag's and Cu
The temperature that fusing point, Ag powder 21 and Cu powder 22 are not melted, melts metal powder with low melting point 23.As long as the heat treatment makes eutectic
Point metal dust 23 is melted, therefore can carry out reflow (heat treatment) come real by the stove or baking oven for general wlding
Apply.More specifically, metal powder with low melting point 23 be Sn powder when, more than the fusing point (232 DEG C) of Sn and Ag fusing point (961
DEG C) and the following temperature of fusing point (1083 DEG C) of Cu within the scope of, with the fusing point of low-melting-point metal plus 10 DEG C~30 DEG C of temperature
It is heat-treated.
If metal powder with low melting point 23 is melted, the refractory metal Ag powder 21 not melted at a temperature of the heat treatment
Spread all over the liquid phase of low-melting-point metal between Cu powder 22.Also, make the liquid phase of low-melting-point metal in Ag powder 21 and Cu powder
Cooled down and solidified low-melting-point metal after being permeated between 22, thus, as shown in Figure 1B, formed the binder course 24 of low-melting-point metal
Interlink refractory metal powder (Ag powder 21 with Cu powder 22) state soldered joint material 4.Now, also sometimes one
Part low-melting-point metal carries out alloying with refractory metal, but the major part of refractory metal is directly residual with original powder
Deposit, therefore multiple spaces 41 are formed at metal powder with low melting point 23 by being heat-treated to exist before heating, the shape of soldered joint material 4
Loose structure as the porosity more than 10%.
In this way, in heat treatment step, relative to sealing slurry 20 in the Ag powder 21 being made up of refractory metal
With Cu powder 22, low-melting-point metal is melted, and as liquid condition, is immersed between refractory metal powder 21,22, carries out liquid phase burning
Knot.Thus, it is possible to form soldered joint material 4 with low heat-treatment temperature.At this moment, low-melting-point metal and high-melting-point will not be turned into
The brazing alloy of metal.
[binding agent removing step]
As described above, being mixed with binding agent 25 in sealing slurry 20.Therefore, by cleaning after heat treatment step
Liquid removal remains in the residue (cleaning treatment) of the binding agent 25 of soldered joint material 4.Now, soldered joint material is peeled off from carrier
After material 4, individually cleaning soldered joint material 4.Cleaning fluid can be used Arakawa Chemical Industries, Ltd. systems
Precise part cleaning agent (Pine Alpha Series) etc..
After removing the residue (cleaning treatment) of binding agent 25 by cleaning fluid, as needed, can also implement residual for reducing
Stay in the treatment of the organic components of the inside of soldered joint material 4.This is processed as example to soldered joint material 4 with 300 DEG C
Implement the heat treatment of less than 24 hours more than 0.1 hour below 1200 DEG C of the above, preferably with 600 DEG C of heat treatments of implementation 9 hours,
The drying and processing for making organic components gasify and removing.
The ＜ sealings composition and manufacture method ＞ of lid material
It is separately fabricated to being coated with sealing slurry 20 on carrier 3 in the manufacture method of described soldered joint material 4
The situation of soldered joint material 4 is illustrated, but can also be used for packaging body 5 and lid 1 sealing (with reference to Fig. 5 A,
Fig. 5 B) soldered joint material 4 be previously formed in the surface of lid 1, composition makes lid 1 be integrally formed with soldered joint material 4
Sealing lid material 6.
With reference to the method that Fig. 3 explanations manufacture sealing lid material 6.
The sealing manufacture method of lid material 6, by the substitution of carrier 3 in the manufacture method (Fig. 2) of the soldered joint material 4
Into beyond lid 1, the manufacture method with the soldered joint material 4 is identical, has：The printing of sealing slurry 20 is coated on lid
The slurry painting process on the surface of body 1；The sealing of lid 1 will be coated on slurry 20 with the melt temperature of metal powder with low melting point 23
The heat treatment step for being heated；And the binding agent removal of binding agent 25 is removed after the surface of lid 1 forms soldered joint material 4
Operation.
[slurry painting process]
Cobalt, 42 alloys etc. can be used as the material of lid 1, surface is implemented with nickel plating (metal plating).In the lid 1
Described sealing slurry 20 is printed on surface the frame-shaped for being coated into such as shape of the alignment peripheral part Chong Die with packaging body.Separately
Outward, at this point it is possible to carry out discharge supply by point gum machine etc. and be coated with sealing slurry 20 in lid 1.
[heat treatment step]
Then, low temperature reflow treatment is implemented in the lid 1 for being coated with sealing slurry 20.Specifically, in nitrogen environment
Under, it is coated with the lid 1 of sealing slurry 20 and is heated to the molten of contained metal powder with low melting point 23 in sealing slurry 20
Melt more than temperature i.e. fusing point, Ag powder 21 of the fusing point or liquidus temperature of metal powder with low melting point 23 less than Ag and Cu
And the temperature that Cu powder 22 is not melted, melt metal powder with low melting point 23.Also, make the liquid phase of low-melting-point metal in Ag powder
Cooled down after being permeated between 21 and Cu powder 22, so that low-melting-point metal solidifies.Thus, can be constituted on the surface of lid 1 and be provided with pricker
The sealing lid material 6 of condensation material 4 is welded, the soldered joint material 4 has Ag powder 21 and Cu powder 22 by low melting point gold
The loose structure of the porosity more than 10% for belonging to the binder course 24 for being formed and being concatenated.The soldered joint material 4 being thusly-formed is
The state on the surface of lid 1 is fixed on, therefore will not be come off from lid 1 during operation sealing lid material 6.
[binding agent removing step]
As described above, being mixed with binding agent 25 in sealing slurry 20.Therefore, heat treatment step is removed by cleaning fluid
The residue of the binding agent 25 for remaining afterwards.
Now, as needed, after the cleaning treatment of binding agent, can also implement to remain in soldered joint material for reduction
The operation of the organic components of 4 inside (is for example implemented 0.1 hour to soldered joint material with less than more than 300 DEG C 1200 DEG C
Heat treatment below the above 24 hours, preferably implements the heat treatments of 9 hours with 600 DEG C, organic components is gasified and removes
Drying and processing).
Many sealings of ＜ manufacture method ＞ of lid material
In manufacture method of the sealing with lid material 6, except being implemented at heat with slurry 20 in the coating sealing of each lid 1
Beyond reason, as shown in figure 4, can also prepare the sheet material 2 of the size that can form multiple lids 1 in advance, form many on the surface of sheet material 2
After individual soldered joint material 4, split the sheet material 2 and carry out the multiple lids 1 of monolithic chemical conversion, the thus multiple sealings of disposable manufacture are used
Lid material 6.
Now, the manufacture method of sealing lid material has：Sealing slurry 20 is printed the slurry for being coated on the surface of sheet material 2
Painting process；The sealing that sheet material 2 will be coated on is formed with slurry 20 so that the melt temperature of metal powder with low melting point is heated
The heat treatment step of soldered joint material 4；The binding agent of binding agent 25 is removed after the surface of sheet material 2 forms soldered joint material 4
Removing step；And cutting sheet material 2 and be divided into the singualtion operation of sealing lid material 6.And, as needed, in monolithic chemical industry
After sequence, can also have the electroplating processes operation for implementing metal plating to the surface of sealing lid material 6.
[slurry painting process]
The sheet material 2 of the size that preparation can arrange multiple lids 1 and be formed, on the surface of the sheet material 2, by described sealing
The position of the peripheral part of the packaging body 5 on the surface for overlapping sealing lid material 6 is directed at slurry 20, printing is coated into frame-shaped and (saves
Sketch map shows).At this time it is also possible to be supplied by the discharge that point gum machine etc. is carried out and be coated with sealing slurry 20 in sheet material 2.As plate
The material of material 2, can be used cobalt, 42 alloys etc., and nickel plating (metal plating) is implemented with the two sides on surface or one side.
[heat treatment step]
Sheet material 2 (lid 1) to being coated with sealing slurry 20 implements low temperature reflow treatment.Specifically, in nitrogen ring
Under border, it is coated with the sheet material 2 of sealing slurry 20 and is heated to contained metal powder with low melting point 23 in sealing slurry 20
More than melt temperature it is fusing point, the Ag powder of the fusing point or liquidus temperature of metal powder with low melting point 23 less than Ag and Cu
The temperature that 21 and Cu powder 22 is not melted, melts metal powder with low melting point 23.Also, make the liquid phase of low-melting-point metal in Ag powder
Cooled down after being permeated between end 21 and Cu powder 22, so that low-melting-point metal solidifies.Thus, can be in the surface shape of sheet material 2 (lid 1)
Into soldered joint material 4 (Fig. 4), the soldered joint material 4 is to pass through low-melting-point metal with Ag powder 21 and Cu powder 22
The binder course 24 of formation and the loose structure of the porosity more than 10% that is concatenated.The soldered joint material 4 being thusly-formed be by
The state on the surface of sheet material 2 (lid 1) is fixed on, therefore will not be come off from lid during operation sheet material 2 (lid 1).
[binding agent removing step]
As described above, being mixed with binding agent 25 in sealing slurry 20.Therefore, heat treatment step is removed by cleaning fluid
The residue (cleaning treatment) of the binding agent 25 for remaining afterwards.Cleaning fluid can be used Arakawa Chemical Industries, Ltd.
Precise part cleaning agent (Pine Alpha Series) processed etc..
Now, after the residue (cleaning treatment) of binding agent 25 is removed by cleaning fluid, as needed, can also implement for dropping
Treatment of the low-residual in the organic components of the inside of soldered joint material 4.This be processed as example to soldered joint material 4 with
Less than more than the 300 DEG C 1200 DEG C heat treatments for implementing less than 24 hours more than 0.1 hour, preferably with 600 DEG C of heat of implementation 9 hours
Treatment, the drying and processing for making organic components gasify and removing.
[singualtion operation]
Then, cutting is formed with the sheet material 2 of soldered joint material 4, so that monolithic is melted into each lid 1 (sealing lid material 6).
[electroplating processes operation]
As described above, being implemented with nickel plating on the surface of sheet material 2, but soldered joint material 4 can also be formed with cutting
Sheet material 2 so that after monolithic is melted into each lid 1 (sealing lid material 6), to its whole implementation nickel plating (metal plating).Thus,
Cut surface (side) to lid 1 (sealing lid material 6) implements nickel plating, can prevent the side wall in lid 1 (sealing lid material 6)
Generation is corroded or is got rusty.On nickel plating, can be formed by electroless plating, electrolysis plating, thickness can be several μm.And,
Beyond nickel plating, can also implement other metal platings.
＜ packaging body encapsulating methods ＞
Then, the packaging body encapsulating method of lid is engaged with reference to Fig. 5 A, Fig. 5 B explanation packaging body.
The encapsulating method has：Described sealing slurry 20 is printed the slurry painting process for being coated on the surface of lid 1；
The heat treatment step that the sealing of lid 1 is heated with slurry 20 with the melt temperature of metal powder with low melting point 23 will be coated on；
The binding agent removing step of binding agent 25 is removed after the surface of lid 1 forms soldered joint material 4；And after binding agent 25 being removed
Lid 1 overlap packaging body 5, heating melting soldered joint material 4 and carry out alloying, be formed as brazing alloy, thus make
Lid 1 is bonded on the alloying step of packaging body 5, and alloying step is added in manufacture method of the described sealing with lid 6
And constitute.Packaging body encapsulating method has singualtion operation and electroplating processes operation as needed.Therefore, sealed in packaging body
In the explanation of method, slurry painting process, heat treatment step, binding agent removing step, singualtion operation and electroplating processes are omitted
The explanation of operation, only explanation uses and is provided with the sealing lid material 6 of soldered joint material 4 on the surface of lid 1 and is packaged body 5
With the alloying step of the engagement of lid 1.
[alloying step]
As shown in Fig. 5 A arrows, the lap seal lid material 6 in the way of making soldered joint material 4 contact packaging body 5 is such as schemed
Shown in 5B, heated by the state of the pressure with Additional provisions, melt, cool and solidify soldered joint material 4, so that lid
Body 1 is bonded on packaging body 5.Packaging body 5 is made up of ceramics etc., and such as Gold plated Layer is formed with as leading on the composition surface with lid 1
Metal layer.
The heating means of soldered joint material 4 have：Using baking oven or conveyer belt stove etc. with the fusing point of brazing material more than
Temperature processed fusion process (heating Sealing Method), seamed welding (resistance welding method), method of laser welding, electron beam weldering
Connection, ultrasonic bonding etc..
For example in seamed welding, as shown in Figure 5 B, overlapped in the way of the resistance brazing grafting material 4 of packaging body 5 close
Envelope lid material 6, circular electrode 11 is abutted from sealing with the top of the lid 1 of lid material 6, is circulated with the state of the pressure of Additional provisions
Electric current, while making circular electrode 11 be moved along the peripheral part of lid 1.By joule corresponding with the current value of circular electrode 11
Heat and make the partial melting of soldered joint material 4, by appropriate setting electric current value, transient heating to refractory metal powder (Ag powder
End 21 and Cu powder 22) fusing point more than temperature and melt soldered joint material 4.
In method of laser welding or electron beam welding method, diagram is omitted, but can be by being overlapped with by sealing lid material 6
In the state of packaging body 5, to engagement surface irradiation laser or electron beam, transient heating soldered joint material 4.
In this way, being melted by making refractory metal powder 21,22, also comprising low-melting-point metal, soldered joint material 4 is whole
Body turns into molten condition, and brazing alloy is formed by contained each metal, terminates sealing.For example, for example as Ag, Cu, low
Melting point metals and in the soldered joint material 4 containing Sn, as Ag-Cu-Sn systems brazing alloy, engageable lid 1 and packaging body
5。
In the alloying step, using seamed welding, method of laser welding, electron beam welding method etc. only make sealing into
For local high-temperature state heating means when, the part of sealing local heating successively, thus in the heating part and not plus
Hot part produces thermal shock or mechanically stressed.From this point, soldered joint material 4 is by stomata of the inside with space
The loose structure of rate more than 10%, thermal shock or mechanical stress when can relax welding.It is therefore possible to prevent in packaging body 5 and lid
Bonding layer or packaging body 5 between body 1 produce cracking, and packaging body 5 can be made gas-tight seal with lid 1.If in addition, soldered joint
The porosity of material 4 becomes big, then sealing reduction, therefore the porosity preferably is set into less than 35%.
Soldered joint material 4 is formed as the loose structure with space internally, but soldered joint material 4 is heated to
The melt temperature of Ag powder 21 and Cu powder 22 and when Ag and Cu and low-melting-point metal is melted and is alloyed, i.e. by each
Welding is planted along the peripheral part of lid 1 during heating soldering grafting material 4, the puddle of soldered joint material 4 can be successively
It is mobile, thus with the puddle movement and space inside soldered joint material 4 can make packaging body by extrusion to outside
5 is reliably gas-tight seal with lid 1.
When the soldered joint material 4 is used for into such as substrate with by engagement of carrying object etc., i.e. the sealing with packaging body 5
Purposes is different, without it is gas-tight seal when, be not necessarily intended to alloying step.Do not make in soldered joint material 4 Ag and Cu with it is low
Melting metal alloys, or make a part of alloying, and, can also retain loose structure and engage substrate with by carrying object.
Also, in this way, in the method that engagement lid 1 and packaging body 5 are sealed, soldered joint is pre-formed in lid 1
Material 4, therefore the easy surface for being formed in lid 1 of soldered joint material 4 of stabilization, soldering when operation sealing is with lid material 6 can be made
Grafting material 4 will not come off from lid 1, so as to easily operate.And, as described above, sealing slurry 20 is can be by printing
Deng method be coated on the surface of carrier 3 or lid 1, can easily form the (sealing of soldered joint material 4 of desired shape
Frame).Also, the formation operation of 4 pairs of lids 1 of soldered joint material can be carried out by the heat treatment in low temperature, more efficient.
And, the sealing lid material 6 after heat treatment step is overlapped into packaging body 5 to clamp soldered joint material 4
State implements alloying step, thus can simultaneously carry out alloying and the sealing of soldered joint material 4, therefore more efficient.
And, the material powder of sealing slurry 20 is blended in, various metals powder is contained because of combination, therefore can hold
The fit rate or species of each metal dust are easily changed, alloy composition can be easily changed.
And, when the material powder that will be blended in sealing slurry is set to silver brazing alloy powder, connect when soldering is formed
During condensation material, it is necessary to be heated to more than the melt temperature of silver brazing alloy (liquidus temperature), but the soldering of present embodiment
Grafting material 4 can utilize the liquid-phase sintering of low-melting-point metal, and be come with melt temperature (being less than 240 DEG C) heating of low-melting-point metal
Formed, therefore stove etc. need not use the equipment of high temperature specification, it is possible to decrease machining energy.
And, packaging body encapsulating method can also be used：By the soldered joint material 4 of pre-production be layered in packaging body 5 with
After between lid 1, the method (omitting diagram) for melting soldered joint material 4 and carrying out alloying is heated.That is, it is close in the packaging body
In encapsulation method, slurry painting process, heat treatment step and alloying step are carried out；The slurry painting process is by sealing slurry
20 coatings are on carrier 3；The heat treatment step will be coated on the sealing of carrier 3 with slurry 20 with the melting temperature of low-melting-point metal
Degree is heated and cooling and solidifying after being made the liquid phase of low-melting-point metal permeate between Ag powder 21 and Cu powder 22, is consequently formed
The soldering of the porosity more than 10% that Ag powder 21 and Cu powder 22 are concatenated by the binder course 24 that low-melting-point metal is formed
Grafting material 4；The alloying step, after soldered joint material 4 is layered between packaging body 5 and lid 1, heating melting soldering
Grafting material 4 and carry out alloying, be formed as brazing alloy.
Embodiment
On embodiment 1~9, comparative example 1~11, packaging body and the sample of lid (sealing lid material) for testing are
Each 100.The ceramics (oxidation aluminum) that packaging body is 3.2mm × 2.5mm using planar dimension, thickness is 0.5mm, as metal
Plating (metal layer) forms 0.5 μm of Gold plated Layer on 5 μm of nickel coating.Lid using planar dimension be 3.1mm ×
2.4mm, thickness are the cobalt panel of 0.1mm, and 0.1 μm is formed on 5 μm of nickel coating as metal plating (metal layer)
Gold plated Layer.
The sealing slurry of each sealing of embodiment 1~9 and comparative example 1~10 lid material is formed by the mixing shown in table 1
Ratio, the material powder of each metal dust mixing of average grain diameter and binding agent mix and make.SAC305 in table 1 is Sn-3
The Sn-Ag-Cu solder alloys of quality %Ag-0.5 mass %Cu.Then, it is real after these sealing slurries being coated on into each lid
Apply the heat treatment of 240 DEG C of maximum temperature and form soldered joint material to form sealing lid material, in order to remove binding agent, cleaning
Lid material is used in sealing.
On each metal dust, in the particle diameter that will be determined using laser diffraction, scattering formula particle size distribution device
Between value footpath (D50) as average grain diameter.
The rolling stock of the silver brazing alloy without loose structure has been used in the soldered joint material of comparative example 11
(BAg-8：72 mass %Ag-28 mass %Cu).
In the soldered joint material that the sealing lid material of these embodiments 1~9 and comparative example 1~11 is formed, with its group
Into mixed powder (material powder) solid density as ρ 1, Archimedes is passed through with the density of the soldered joint material after cleaning
When the density that method is determined is as ρ 2, the porosity is calculated using the formula of the porosity (%)=(ρ 1- ρ 2)/ρ 1.
In addition, the soldered joint material of comparative example 7 and comparative example 10 is peeling in binding agent removing step.And,
The soldered joint material of comparative example 8 shape in heat treatment step crumbles, it is impossible to keep its shape.Therefore, these comparative examples 7,
8th, 10 soldered joint material cannot carry out the measure of the porosity and record the porosity with "-".
Then, each lid (sealing lid material) is overlapped into packaging body and is implemented with seam welding, be hermetically sealed.
Afterwards, near with (× 50 times) junction surfaces of the observation packaging body with lid of stereomicroscope, no cracking has been checked.And
And, being set to qualified (OK) for ceramic packaging body no cracking near junction surface produces being set to unqualified (NG) (table 2) for cracking.
And, the gas-tight seal experiment based on test of being bubbled in He leak-testings and liquid is implemented to each 100 samples, according to
The leakage number of generation checks airtight fraction defective.It is airtight in test both sides if sealing assessment is bubbled in He leak-testings and liquid
Fraction defective be less than 2%, be set to qualified (OK), in the test of at least one party airtight fraction defective be more than 2% be set to it is unqualified
(NG) (table 2).
These results are shown in table 2.
[table 1]
[table 2]
| Cracking | Sealing | |
| Embodiment 1 | OK | OK |
| Embodiment 2 | OK | OK |
| Embodiment 3 | OK | OK |
| Embodiment 4 | OK | OK |
| Embodiment 5 | OK | OK |
| Embodiment 6 | OK | OK |
| Embodiment 7 | OK | OK |
| Embodiment 8 | OK | OK |
| Embodiment 9 | OK | OK |
| Comparative example 1 | OK | NG |
| Comparative example 2 | OK | NG |
| Comparative example 3 | OK | NG |
| Comparative example 4 | OK | NG |
| Comparative example 5 | OK | NG |
| Comparative example 6 | OK | NG |
| Comparative example 7 | - | - |
| Comparative example 8 | - | - |
| Comparative example 9 | NG | OK |
| Comparative example 10 | - | - |
| Comparative example 11 | NG | OK |
From table 1 and table 2 it will be apparent that, the use of containing average grain diameter is less than more than 0.1 μm 10.0 μm as material powder
And 40 more than mass % below 90 mass % Ag powder, be less than more than 0.1 μm 10.0 μm and 5 mass % containing average grain diameter
The Cu powder of below the mass % of the above 50, containing average grain diameter be less than more than 0.5 μm 20.0 μm and more than 5 mass % 40 matter
Measure the sealing slurry of the metal powder with low melting point of below %, the pricker with the loose structure that the set porosity is more than 10%
Any one does not produce cracking in the sealing lid material of the embodiment 1~9 for welding condensation material, and, the air-tightness of packaging body is high
And can be sealed well.
The Ag powder of sealing slurry and the average grain diameter of Cu powder are blended in less than 0.1 μm, metal powder with low melting point
Average grain diameter (comparative example 9), the porosity of the soldered joint material formed using the sealing slurry when being less than 0.5 μm
It is that, less than 10%, the bonding layer or packaging body of packaging body and lid generate cracking in itself.On the other hand, Ag powder and Cu powder
Average grain diameter more than 10 μm when (comparative example 1), the porosity of the soldered joint material for being formed becomes big, and sealing is deteriorated.And
And, when the average grain diameter of metal powder with low melting point is more than 20 μm (comparative example 2), the porosity of the soldered joint material for being formed
Become big, sealing is also deteriorated.
When the containing ratio of Ag powder is less than 40 mass % (comparative example 3), sealing reduction, (ratio during more than 90 mass %
Compared with example 10), stripping is generated in binding agent removing step.The containing ratio of Cu powder be the mass % of more than 5 mass % 50 with
Under scope outside when, i.e. (comparative example 4,10) or (comparative example 5,7), sealing meeting during more than 50 mass % during less than 5 mass %
Reduce.When the containing ratio of metal powder with low melting point is less than 5 mass % (comparative example 7,10), produced in binding agent removing step
Peel off, during more than 40 mass % (comparative example 6), sealing can be reduced.
And, the present invention is not limited to above-mentioned implementation method, is not departing from the range of order of the invention, can add each
Plant change.
Industrial applicability
It is made up of the alloy that can easily change soldered joint material, the soldered joint material with loose structure can
Do not produce cracking and reliably gas-tight seal packaging body.
Symbol description
1- lids, 2- sheet materials, 3- carriers, 4- soldered joint materials, 5- packaging bodies, 6- sealing lid materials, 11- rollers electricity
Pole, 20- sealing slurries, 21-Ag powder, 22-Cu powder, 23- metal powder with low melting point, 24- binder courses, 25- binding agents,
41- spaces.
Claims (18)
1. a kind of sealing slurry, it is characterised in that comprising material powder and binding agent,
The material powder contain the average grain diameter of more than 5 mass % below 40 mass % for less than more than 0.5 μm 20.0 μm and
Metal powder with low melting point, the average grain diameter of below the mass % of more than 40 mass % 90 of fusing point or liquidus temperature less than 240 DEG C
For the average grain diameter of less than more than 0.1 μm 10.0 μm of Ag powder and below the mass % of more than 5 mass % 50 is more than 0.1 μm
Less than 10.0 μm of Cu powder.
2. sealing slurry according to claim 1, it is characterised in that
The average grain diameter of the metal powder with low melting point is less than more than 1 times 10 times of the average grain diameter of the Ag powder and is institute
State the average grain diameter of Cu powder less than more than 1 times 10 times.
3. sealing slurry according to claim 1, it is characterised in that
The average grain diameter of the metal powder with low melting point is more than the average grain diameter of the Ag powder and the average grain of the Cu powder
Footpath.
4. sealing slurry according to claim 1, it is characterised in that
The blending ratio of the binding agent is below the mass % of more than 2 mass % 50.
5. sealing slurry according to claim 1, it is characterised in that
The metal powder with low melting point is to be closed selected from Sn, In, Sn-Ag-Cu solder alloy, Sn-Cu solder alloys, Sn-Bi solders
One or more of gold and Sn-In solder alloys.
6. a kind of manufacture method of soldered joint material, it is characterised in that have：
Slurry painting process, the sealing slurry described in claim 1 is coated on carrier；And
Heat treatment step, the sealing that will be coated on the carrier is carried out with slurry with the melt temperature of the low-melting-point metal
Heat and cool and solidify after the liquid phase of the low-melting-point metal is permeated between the Ag powder and the Cu powder, thus shape
It is 10% into the porosity that the Ag powder and the Cu powder are concatenated by the binder course that the low-melting-point metal is formed
Soldered joint material above.
7. a kind of soldered joint material, it is characterised in that have：
Ag powder, the average grain diameter of the Ag powder is less than more than 0.1 μm 10.0 μm；
Cu powder, the average grain diameter of the Cu powder is less than more than 0.1 μm 10.0 μm；And
Binder course, low-melting-point metal of the binder course by fusing point or liquidus temperature less than 240 DEG C is formed and for linking
The Ag powder and the Cu powder,
In the soldered joint material, the porosity is more than 10%, and quality ratio is, the Ag powder is more than 40 mass %
Below 90 mass %, the Cu powder is below the mass % of more than 5 mass % 50, and the binder course is 40 matter of more than 5 mass %
Amount below %.
8. it is a kind of to seal with the manufacture method of lid material, it is characterised in that to have：
Slurry painting process, the sealing slurry described in claim 1 is coated on the surface of lid；And
Heat treatment step, the sealing that will be coated on the lid is carried out with slurry with the melt temperature of the low-melting-point metal
Heat and cool and solidify after the liquid phase of the low-melting-point metal is permeated between the Ag powder and the Cu powder, thus shape
It is 10% into the porosity that the Ag powder and the Cu powder are concatenated by the binder course that the low-melting-point metal is formed
Soldered joint material above.
9. it is according to claim 8 to seal with the manufacture method of lid material, it is characterised in that to have：
The binding agent removing step of the binding agent in remaining in the soldered joint material is removed after the heat treatment step.
It is 10. according to claim 9 to seal with the manufacture method of lid material, it is characterised in that
The binding agent removing step has：The cleaning treatment of the soldered joint material is cleaned with cleaning fluid；And heat treatment should
The drying and processing of the cleaned soldered joint material.
The 11. sealings according to claim 8 manufacture method of lid material, it is characterised in that
In the slurry painting process, the sealing is coated with the plate surface of size that can form multiple lids and is used
Slurry,
And with the sheet material to be divided into the singualtion operation of the lid after the heat treatment step.
Lid material is used in a kind of 12. sealings, it is characterised in that had：
Lid；And
It is located at the soldered joint material described in the claim 7 of the top surface.
A kind of 13. packaging body encapsulating methods, it is the packaging body encapsulating method by brazing alloy bonding packaging body and lid, tool
Have：
Slurry painting process, the sealing slurry described in claim 1 is coated on the surface of the lid；
Heat treatment step, the sealing that will be coated on the lid is carried out with slurry with the melt temperature of the low-melting-point metal
Heat and cool and solidify after the liquid phase of the low-melting-point metal is permeated between the Ag powder and the Cu powder, thus shape
It is 10% into the porosity that the Ag powder and the Cu powder are concatenated by the binder course that the low-melting-point metal is formed
Soldered joint material above；And
Alloying step, overlaps the lid state heating melting soldered joint material of the packaging body and enters
Row alloying, so as to as the brazing alloy.
14. packaging body encapsulating methods according to claim 13, it is characterised in that
Between the heat treatment step and the alloying step, remained in removal viscous in the soldered joint material
Tie the binding agent removing step of agent.
15. packaging body encapsulating methods according to claim 14, it is characterised in that
The binding agent removing step has：The cleaning treatment of the soldered joint material is cleaned with cleaning fluid；And heat treatment should
The drying and processing of the cleaned soldered joint material.
16. packaging body encapsulating methods according to claim 13, it is characterised in that
In the slurry painting process, the sealing is coated with the plate surface of size that can form multiple lids and is used
Slurry,
And with the sheet material to be divided into the singualtion operation of the lid after the heat treatment step.
17. packaging body encapsulating methods according to claim 16, it is characterised in that have：
After the singualtion operation, the electroplating processes operation of metal plating is implemented on the surface to the lid.
A kind of 18. packaging body encapsulating methods, it is the packaging body engaged in packaging body overlap lid and by brazing alloy
Encapsulating method, it is characterised in that carry out following operation：
Slurry painting process, the sealing slurry described in claim 1 is coated on carrier；
Heat treatment step, the sealing that will be coated on the carrier is carried out with slurry with the melt temperature of the low-melting-point metal
Heat and cool and solidify after the liquid phase of the low-melting-point metal is permeated between the Ag powder and the Cu powder, thus shape
It is 10% into the porosity that the Ag powder and the Cu powder are concatenated by the binder course that the low-melting-point metal is formed
Soldered joint material above；And
Alloying step, after the soldered joint material is layered between the packaging body and the lid, heating melting institute
State soldered joint material and carry out alloying, so as to as the brazing alloy.
Applications Claiming Priority (7)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2014222900 | 2014-10-31 | ||
| JP2014-222900 | 2014-10-31 | ||
| JP2015-164700 | 2015-08-24 | ||
| JP2015164700 | 2015-08-24 | ||
| JP2015213467A JP6575301B2 (en) | 2014-10-31 | 2015-10-29 | Sealing paste, brazing joint material and method for producing the same, sealing lid material and method for producing the same, and package sealing method |
| JP2015-213467 | 2015-10-29 | ||
| PCT/JP2015/080651 WO2016068272A1 (en) | 2014-10-31 | 2015-10-30 | Sealing paste, brazing material and production method thereof, sealing lid member and production method thereof, and package sealing method |
Publications (2)
| Publication Number | Publication Date |
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| CN106715039A true CN106715039A (en) | 2017-05-24 |
| CN106715039B CN106715039B (en) | 2020-06-12 |
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| CN201580051707.8A Active CN106715039B (en) | 2014-10-31 | 2015-10-30 | Package sealing method |
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| Country | Link |
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| JP (1) | JP6575301B2 (en) |
| KR (1) | KR102203608B1 (en) |
| CN (1) | CN106715039B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109616460A (en) * | 2017-10-04 | 2019-04-12 | 三菱电机株式会社 | Power semiconductor device |
| CN110961831A (en) * | 2018-09-28 | 2020-04-07 | 株式会社田村制作所 | Forming solder and manufacturing method of forming solder |
| CN111926231A (en) * | 2020-08-27 | 2020-11-13 | 湘潭大学 | Method for preparing oxide dispersion strengthening MoNbTaVW refractory high-entropy alloy |
| CN113814504A (en) * | 2021-09-03 | 2021-12-21 | 广州德芯半导体科技有限公司 | Packaging method for non-high-temperature connection temperature sensor |
| CN114450106A (en) * | 2019-10-15 | 2022-05-06 | 千住金属工业株式会社 | Bonding material, method for producing bonding material, and bonded body |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11095104B2 (en) * | 2017-05-05 | 2021-08-17 | Harvey L Frierson | Chord organizer |
| JP7500943B2 (en) * | 2019-10-11 | 2024-06-18 | 株式会社レゾナック | Metal paste for bonding, method for manufacturing bonded body, and bonded body |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0110307A2 (en) * | 1982-11-24 | 1984-06-13 | Samsung Electronics Co., Ltd. | Semiconductor die-attach technique and composition therefor |
| JP2002160090A (en) * | 2000-11-27 | 2002-06-04 | Tanaka Kikinzoku Kogyo Kk | Ag-Cu-In-BASED BRAZING FILLER MATERIAL AND METHOD FOR PRODUCING THE SAME |
| JP2003163299A (en) * | 2001-11-29 | 2003-06-06 | Nippon Filcon Co Ltd | Sealing cap for electronic element package and its manufacturing method as well as method for sealing using the cap |
| CN101087673A (en) * | 2005-01-11 | 2007-12-12 | 株式会社村田制作所 | Solder paste and electronic device |
| CN101529583A (en) * | 2006-09-01 | 2009-09-09 | 千住金属工业株式会社 | Lid for functional part and process for producing the same |
| JP2011096756A (en) * | 2009-10-28 | 2011-05-12 | Kyocera Corp | Package for housing electronic component and electronic device |
| CN103028861A (en) * | 2011-10-06 | 2013-04-10 | 富士通株式会社 | Conductive bonding material, conductor bonding method, and semiconductor device production method |
| WO2014082100A1 (en) * | 2012-11-16 | 2014-05-30 | Ormet Circuits Inc. | Alternative compositions for high temperature soldering applications |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05254949A (en) * | 1992-03-05 | 1993-10-05 | Nippon Cement Co Ltd | Brazing filler metal for joining metal to ceramics and joining method |
| JP3030479B2 (en) * | 1992-04-23 | 2000-04-10 | 日本特殊陶業株式会社 | Ceramic package |
| JP2803636B2 (en) | 1996-04-26 | 1998-09-24 | 日本電気株式会社 | Semiconductor integrated circuit package and method of manufacturing the same |
| JP2006049595A (en) | 2004-08-05 | 2006-02-16 | Tanaka Kikinzoku Kogyo Kk | Silver solder cladding material, and lid and ring for package sealing |
| JP5065718B2 (en) | 2006-06-20 | 2012-11-07 | 田中貴金属工業株式会社 | Hermetic sealing method of piezoelectric element and manufacturing method of piezoelectric device |
| JP6488896B2 (en) * | 2014-06-13 | 2019-03-27 | 三菱マテリアル株式会社 | Package sealing method and sealing paste |
-
2015
- 2015-10-29 JP JP2015213467A patent/JP6575301B2/en not_active Expired - Fee Related
- 2015-10-30 CN CN201580051707.8A patent/CN106715039B/en active Active
- 2015-10-30 KR KR1020177013063A patent/KR102203608B1/en active IP Right Grant
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0110307A2 (en) * | 1982-11-24 | 1984-06-13 | Samsung Electronics Co., Ltd. | Semiconductor die-attach technique and composition therefor |
| US4487638A (en) * | 1982-11-24 | 1984-12-11 | Burroughs Corporation | Semiconductor die-attach technique and composition therefor |
| JP2002160090A (en) * | 2000-11-27 | 2002-06-04 | Tanaka Kikinzoku Kogyo Kk | Ag-Cu-In-BASED BRAZING FILLER MATERIAL AND METHOD FOR PRODUCING THE SAME |
| JP2003163299A (en) * | 2001-11-29 | 2003-06-06 | Nippon Filcon Co Ltd | Sealing cap for electronic element package and its manufacturing method as well as method for sealing using the cap |
| CN101087673A (en) * | 2005-01-11 | 2007-12-12 | 株式会社村田制作所 | Solder paste and electronic device |
| CN101529583A (en) * | 2006-09-01 | 2009-09-09 | 千住金属工业株式会社 | Lid for functional part and process for producing the same |
| JP2011096756A (en) * | 2009-10-28 | 2011-05-12 | Kyocera Corp | Package for housing electronic component and electronic device |
| CN103028861A (en) * | 2011-10-06 | 2013-04-10 | 富士通株式会社 | Conductive bonding material, conductor bonding method, and semiconductor device production method |
| WO2014082100A1 (en) * | 2012-11-16 | 2014-05-30 | Ormet Circuits Inc. | Alternative compositions for high temperature soldering applications |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109616460A (en) * | 2017-10-04 | 2019-04-12 | 三菱电机株式会社 | Power semiconductor device |
| CN109616460B (en) * | 2017-10-04 | 2023-02-24 | 三菱电机株式会社 | Power semiconductor device |
| CN110961831A (en) * | 2018-09-28 | 2020-04-07 | 株式会社田村制作所 | Forming solder and manufacturing method of forming solder |
| US11618108B2 (en) | 2018-09-28 | 2023-04-04 | Tamura Corporation | Molded solder and molded solder production method |
| CN114450106A (en) * | 2019-10-15 | 2022-05-06 | 千住金属工业株式会社 | Bonding material, method for producing bonding material, and bonded body |
| CN114450106B (en) * | 2019-10-15 | 2023-06-06 | 千住金属工业株式会社 | Bonding material, method for producing bonding material, and bonded body |
| CN111926231A (en) * | 2020-08-27 | 2020-11-13 | 湘潭大学 | Method for preparing oxide dispersion strengthening MoNbTaVW refractory high-entropy alloy |
| CN111926231B (en) * | 2020-08-27 | 2021-08-03 | 湘潭大学 | Method for preparing oxide dispersion strengthening MoNbTaVW refractory high-entropy alloy |
| CN113814504A (en) * | 2021-09-03 | 2021-12-21 | 广州德芯半导体科技有限公司 | Packaging method for non-high-temperature connection temperature sensor |
Also Published As
| Publication number | Publication date |
|---|---|
| KR102203608B1 (en) | 2021-01-14 |
| JP2017039163A (en) | 2017-02-23 |
| JP6575301B2 (en) | 2019-09-18 |
| CN106715039B (en) | 2020-06-12 |
| KR20170074913A (en) | 2017-06-30 |
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