CN105397340B - Composite soldering system and its method for welding for the adaptive sealing-in of intermediate temperature solid oxide fuel cell - Google Patents
Composite soldering system and its method for welding for the adaptive sealing-in of intermediate temperature solid oxide fuel cell Download PDFInfo
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- CN105397340B CN105397340B CN201511023752.0A CN201511023752A CN105397340B CN 105397340 B CN105397340 B CN 105397340B CN 201511023752 A CN201511023752 A CN 201511023752A CN 105397340 B CN105397340 B CN 105397340B
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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
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/362—Selection of compositions of fluxes
-
- 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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/008—Soldering within a furnace
-
- 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
- B23K35/40—Making wire or rods for soldering or welding
-
- 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
- B23K2101/00—Articles made by soldering, welding or cutting
- B23K2101/36—Electric or electronic devices
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Abstract
Composite soldering system and its method for welding for the adaptive sealing-in of intermediate temperature solid oxide fuel cell, the invention belongs to field of solid oxide fuel, the connection temperature that it will solve existing soldering connection sealing SOFC is higher, the problem of reliability is not enough caused by inter-module coefficient of thermal expansion mismatch.The composite soldering system is made up of preformed layer and intermediate layer, and wherein intermediate layer is using Ag CuO solders as matrix, in the base containing the different glass phase of two kinds of glass transition temperatures.Method for welding：First, Cu thin layers are deposited；2nd, hybrid glass phase is prepared；3rd, hybrid glass phase is added in Ag CuO solders, solder mixed-powder is prepared；4th, the preparation of bonding agent；5th, solder mixed-powder is mixed with bonding agent；6th, composite soldering cream is coated；7th, high temperature brazing is carried out.The present invention increases the plastic deformation ability of composite soldering system by adding two kinds of glass phases, adds the reliability of SOFC sealing batch productions.
Description
Technical field
The invention belongs to SOFC technical field, and in particular to temperature solid-oxide fires during one kind is realized
Expect the composite soldering and its method for welding of the reliable adaptive sealing-in of battery.
Background technology
SOFC (Solid Oxide Fuel Cell, SOFC), is a kind of new energy technology,
Reaction between fuel and oxide is realized by the conduction of ion in the electrolyte, electric energy is directly converted chemical energy into, replaces
For traditional fuel combustion process, it is not necessary to by the energy conversion process of fuel chemical energy → heat energy → mechanical energy → electric energy,
It is a kind of all solid state chemical devices of clean and effective.But higher operation temperature causes SOFC to start time length and seal tired
Difficulty, while high temperature accelerates the reaction between battery component also to influence battery life, is obtained so reduction operation temperature is SOFC
Wide variety of key.Currently, middle temperature (~800 DEG C) SOFC is widely studied, and is expected to obtain big rule
Mould practical application.In solid-oxide fuel cell stack, multiple monocells are joined together to obtain desired voltage
Output, connector is placed between single battery, and repeat unit constitutes battery pile.Realizing the reliable sealing of fuel cell is
SOFC obtains the key used reliably and with long-term.The seal request of battery avoid the mixing between fuel gas and oxidizing gas with
And the leakage of gas.
Good fuel encapsulation needs sealing position keeping good heat endurance and electrical insulating property using process, possesses
The thermal coefficient of expansion matched with battery component, seal process needs to carry out at a lower temperature, it is to avoid high temperature is to battery pack
Part causes damage.Meanwhile, encapsulant will keep the balance between wetability and viscosity, ensure that encapsulant can be filled well
While, it is to avoid the sealing station that trickles is polluted to SOFC.In order to meet these use requirements, substantial amounts of sealing system quilt
Develop.Mainly include glass capsulation, compression seal and soldering connection.But, three of the above encapsulating method all exists intrinsic
Defect, it is impossible to fully meet SOFC use requirement.Recently, research reports a kind of brand-new sealing theory-adaptive close
Envelope, that is, allow encapsulant to produce certain plastic deformation at service temperatures, to eliminate because of the thermal stress that temperature change is produced,
Improve the operational reliability of SOFC battery piles.But the research at present on self-adapting seal is also insufficient, still in exploration rank
Section.
The content of the invention
The invention aims to the connection temperature for solving existing soldering connection sealing SOFC is higher, inter-module thermal expansion system
The problem of reliability is not enough caused by number mismatch, and provide for the compound of the adaptive sealing-in of intermediate temperature solid oxide fuel cell
Solder system and its method for welding.
Composite soldering system of the invention for the adaptive sealing-in of intermediate temperature solid oxide fuel cell is by preformed layer with
Interbed is constituted, and preformed layer is is deposited in cell piece and the Cu thin layers of connector sealing station, and intermediate layer is mixed with Ag powder and CuO powder
Ag-CuO solders be matrix, be in the base 650~700 DEG C of glass phase A and glass added with glass transition temperature
Glass softening temperature is 750~800 DEG C of glass phase B, and CuO content is 1~15mol% wherein in Ag-CuO solders.
The present invention is pressed for the method for welding of the composite soldering system of the adaptive sealing-in of intermediate temperature solid oxide fuel cell
Realized according to following steps：
First, Cu thin layers in vacuum evaporation are distinguished on the sealing surface of connector and cell piece, plated film connector and plating is obtained
Film battery piece；
2nd, by the glass phase A that glass transition temperature is 650~700 DEG C and the glass that glass transition temperature is 750~800 DEG C
Glass phase B mixing is pulverized, and hybrid glass phase is obtained after crossing 300~400 mesh sieves；
3rd, Ag powder and CuO the powder mixing weighed, obtains Ag-CuO solders, then adds step 2 into Ag-CuO solders
Obtained hybrid glass phase, adds absolute ethyl alcohol and carries out ball milling, 300~400 mesh sieves are crossed after drying, solder mixed-powder is obtained；
4th, ethyl cellulose is dissolved in terpinol, obtains terpineol solution of ethyl cellulose bonding agent；
5th, the solder mixed-powder that step 3 is obtained is added in terpineol solution of ethyl cellulose bonding agent, mixed
Uniformly obtain intermediate layer composite soldering cream；
6th, intermediate layer composite soldering cream is coated on the sealing surface of plated film cell piece using the method for silk-screen printing, obtained
To the cell piece for being coated with intermediate layer composite soldering cream；
7th, the sealing surface of plated film connector is fitted dress with the sealing surface for the cell piece for being coated with intermediate layer composite soldering cream
Match somebody with somebody, be then placed in Muffle furnace, 200 DEG C of insulation 30~50min degasification are warming up to first, 300~400 DEG C of insulations are continuously heating to
30~50min plastic removals, then 5~30min is incubated in the range of being warming up to 1000~1050 DEG C, room temperature is then cooled to, in completion
The soldering of the composite soldering system of the adaptive sealing-in of temperature solid-oxide fuel battery；
The content of glass phase A wherein described in step 2 accounts for 1~20wt% of Ag-CuO solders, and glass phase B content is accounted for
CuO content accounts for 1~15mol% of Ag-CuO solders in 1~20wt% of Ag-CuO solders, step 3.
The advantage of adaptive composite soldering system of the present invention is：The two kinds of glass phases added, can be in SOFC
In actual use, soften after reaching corresponding glass softening point temperature, increase the plastic deformation of composite soldering system
Ability, can absorb the thermal stress produced in heating process due to SOFC inter-modules coefficient of thermal expansion mismatch.Addition possesses not
With two kinds of glass phases of softening point, composite soldering system can be allowed to possess post deformation failure deformability, thermal stress is absorbed stage by stage,
Composite soldering system plastic deformation ability is avoided to increase suddenly, the structural stability to SOFC is impacted.And prefabricated Cu is deposited
The purpose of thin layer is, in order to avoid glass phase and by the direct contact of sealing matrix, to soften in use because glass is met
Plastic deformation is produced, can be reduced if glass is mutually appeared on seal interface, after softening and be tightly connected performance, causes the slow of gas
Slow leakage.
Step 7 of the present invention can then quantify technical process using the method for air reaction soldering connection, add SOFC close
The reliability of batch production is sealed, while the method being attached with Muffle furnace in air ambient, reduces manufacturing cost, is had
Good commercial application prospect.
Brief description of the drawings
Fig. 1 is the structural representation of the composite soldering system of the adaptive sealing-in of intermediate temperature solid oxide fuel cell of the present invention
Figure；
Fig. 2 is that analog composite solder system reaches that occurring plastic deformation after glass phase A and B softening temperature absorbs thermal stress
Schematic diagram；
Intermediate temperature solid oxide fuel cell 800 DEG C of high temperature of adaptive sealing-in soldered fitting that Fig. 3 is obtained by embodiment one
Joint shear strength test figure after thermal cycle.
Embodiment
Embodiment one：Present embodiment is used for the compound pricker of the adaptive sealing-in of intermediate temperature solid oxide fuel cell
Material system is made up of preformed layer and intermediate layer, and preformed layer is evaporation in cell piece and the Cu thin layers of connector sealing station, centre
The Ag-CuO solders that layer is mixed using Ag powder and CuO powder as matrix, in the base also added with glass transition temperature be 650~
700 DEG C of glass phase A and glass transition temperature is 750~800 DEG C of glass phase B, CuO content wherein in Ag-CuO solders
For 1~15mol%.
Embodiment two：Present embodiment is 1 from the thickness of the copper lamina unlike embodiment one
~2 μm.
Embodiment three：Present embodiment and glass phase A unlike embodiment one or two addition
Account for 1~20wt% of Ag-CuO solders, glass phase A by mass percentage by 5%~15% Li2O, 25%~35%
SiO2, 15%~25% BeO, 20%~30% B2O3MgO with 10%~15% is constituted.
Embodiment four：Glass phase B's adds unlike one of present embodiment and embodiment one to three
Dosage accounts for 1~20wt% of Ag-CuO solders, and B is by mass percentage by 10%~15%Na for the glass phase2O, 30%~40%
SiO2, 20%~25%CaO, 10%~20%B2O3With 10%~20%Al2O3Composition.
Embodiment five：Present embodiment is used for the compound pricker of the adaptive sealing-in of intermediate temperature solid oxide fuel cell
The method for welding of material system is implemented according to following steps：
First, on the sealing surface of connector 1 and cell piece 2 distinguish vacuum evaporation on Cu thin layers 3, obtain plated film connector and
Plated film cell piece；
2nd, by the glass phase A4 that glass transition temperature is 650~700 DEG C and the glass that glass transition temperature is 750~800 DEG C
Glass phase B5 mixing is pulverized, and hybrid glass phase is obtained after crossing 300~400 mesh sieves；
3rd, Ag powder and CuO the powder mixing weighed, obtains Ag-CuO solders 6, then adds step 2 into Ag-CuO solders
Obtained hybrid glass phase, adds absolute ethyl alcohol and carries out ball milling, 300~400 mesh sieves are crossed after drying, solder mixed-powder is obtained；
4th, ethyl cellulose is dissolved in terpinol, obtains terpineol solution of ethyl cellulose bonding agent；
5th, the solder mixed-powder that step 3 is obtained is added in terpineol solution of ethyl cellulose bonding agent, mixed
Uniformly obtain intermediate layer composite soldering cream；
6th, intermediate layer composite soldering cream is coated on the sealing surface of plated film cell piece using the method for silk-screen printing, obtained
To the cell piece for being coated with intermediate layer composite soldering cream；
7th, the sealing surface of plated film connector is fitted dress with the sealing surface for the cell piece for being coated with intermediate layer composite soldering cream
Match somebody with somebody, be then placed in Muffle furnace, 200 DEG C of insulation 30~50min degasification are warming up to first, 300~400 DEG C of insulations are continuously heating to
30~50min plastic removals, then 5~30min is incubated in the range of being warming up to 1000~1050 DEG C, room temperature is then cooled to, in completion
The soldering of the composite soldering system of the adaptive sealing-in of temperature solid-oxide fuel battery；
The content of glass phase A wherein described in step 2 accounts for 1~20wt% of Ag-CuO solders, and glass phase B content is accounted for
CuO content accounts for 1~15mol% of Ag-CuO solders in 1~20wt% of Ag-CuO solders, step 3.
Web plate used in present embodiment step 6 silk-screen printing, it is necessary to previously prepared printed pattern, printed pattern according to
The actual graphical progress of position to be sealed is prefabricated, and printed pattern and battery position to be sealed strictly are aligned by printing process, it is to avoid pricker
Expect that cream pollutes other positions of fuel cell sheet.
Embodiment six：Present embodiment and vacuum during step one evaporation unlike embodiment five
Degree maintains 5 × 10-2More than Pa, current control is controlled in 10~15V in 120~150A, voltage.Other steps and parameter and tool
Body embodiment five is identical.
Embodiment seven：Present embodiment and step 4 ethyl cellulose unlike embodiment five or six
The content of ethyl cellulose is 2~8wt% in terpineol solution bonding agent.Other steps and parameter and embodiment five or
Six is identical.
Embodiment eight：Step 5 unlike one of present embodiment and embodiment five to seven is by weight
Than for (2~4):The 1 solder mixed-powder for obtaining step 3 is added in terpineol solution of ethyl cellulose bonding agent.It is other
Step and parameter are identical with one of embodiment five to seven.
Embodiment nine：Described in step 6 unlike one of present embodiment and embodiment five to eight
The web plate of 300~400 mesh is used in the method for silk-screen printing, screen thickness is 100~200 μm.Other steps and parameter and tool
One of body embodiment five to eight is identical.
Embodiment ten：Described in step 6 unlike one of present embodiment and embodiment five to nine
The thickness of intermediate layer composite soldering cream is 100~200 μm.One of other steps and parameter and embodiment five to nine phase
Together.
Embodiment one：The present embodiment is used for the composite soldering system of the adaptive sealing-in of intermediate temperature solid oxide fuel cell
Method for welding is realized according to following steps：
First, the Cu thin layers that thickness in vacuum evaporation is 1 μm are distinguished on the sealing surface of connector and cell piece, plated film is obtained
Connector and plated film cell piece；
2nd, the glass phase A that glass transition temperature the is 680 DEG C and glass phase B that glass transition temperature is 780 DEG C is mixed and ground
It is broken, obtain hybrid glass phase after crossing 300 mesh sieves；
3rd, Ag powder and CuO the powder mixing weighed, obtains Ag-CuO solders, then adds step 2 into Ag-CuO solders
Obtained hybrid glass phase, adds absolute ethyl alcohol and carries out ball milling 3 hours, crosses 300 mesh sieves after being dried at 100 DEG C, obtains solder
Mixed-powder；
4th, ethyl cellulose is dissolved in terpinol, obtains terpineol solution of ethyl cellulose bonding agent, wherein ethyl
The addition of cellulose is 2wt%；
5th, it is 2 by weight:The 1 solder mixed-powder for obtaining step 3 is added to terpineol solution of ethyl cellulose
It is well mixed to obtain intermediate layer composite soldering cream in bonding agent；
6th, intermediate layer composite soldering cream is coated using the method for silk-screen printing for 100 μm of 300 mesh web plates using thickness
Onto the sealing surface of plated film cell piece, the thickness for controlling intermediate layer is 100 μm, obtains being coated with the electricity of intermediate layer composite soldering cream
Pond piece；
7th, the sealing surface of plated film connector is fitted dress with the sealing surface for the cell piece for being coated with intermediate layer composite soldering cream
Match somebody with somebody, be then placed in Muffle furnace, 200 DEG C of insulation 30min degasification are warming up to first, be continuously heating to 300 DEG C of insulation 30min rows
Modeling, then be incubated 5min in the range of being warming up to 1000 DEG C, is then cooled to room temperature, complete intermediate temperature solid oxide fuel cell from
Adapt to the soldering of the composite soldering system of sealing-in；
CuO content is 1mol% wherein in step 3 Ag-CuO solders, and glass phase A addition accounts for Ag-CuO solders
1wt%, glass phase B addition account for the 1wt% of Ag-CuO solders.
In order to intuitively show the quality of connection of battery component, by Crofer 22APU ferritic stainless steel (soild oxides
Fuel cell is often with metallic interconnection materials) and cell piece be processed into shearing sample, then to soldered fitting carry out 800 DEG C of thermal cycles cut
Shearing stress is tested, and experimental result is as shown in Figure 3.As a result show, soldered fitting is in 80 Thermal Cycling center tap shear strengths
More than 150MPa is maintained, long term high temperature thermal cycle does not have butt joint performance and causes obvious influence.
Embodiment two：The present embodiment is used for the composite soldering system of the adaptive sealing-in of intermediate temperature solid oxide fuel cell
Method for welding is realized according to following steps：
First, the Cu thin layers that thickness in vacuum evaporation is 1 μm are distinguished on the sealing surface of connector and cell piece, plated film is obtained
Connector and plated film cell piece；
2nd, the glass phase A that glass transition temperature the is 680 DEG C and glass phase B that glass transition temperature is 780 DEG C is mixed and ground
It is broken, obtain hybrid glass phase after crossing 300 mesh sieves；
3rd, Ag powder and CuO the powder mixing weighed, obtains Ag-CuO solders, then adds step 2 into Ag-CuO solders
Obtained hybrid glass phase, adds absolute ethyl alcohol and carries out ball milling 3 hours, crosses 300 mesh sieves after being dried at 100 DEG C, obtains solder
Mixed-powder；
4th, ethyl cellulose is dissolved in terpinol, obtains terpineol solution of ethyl cellulose bonding agent, wherein ethyl
The addition of cellulose is 2wt%；
5th, it is 2 by weight:The 1 solder mixed-powder for obtaining step 3 is added to terpineol solution of ethyl cellulose
It is well mixed to obtain intermediate layer composite soldering cream in bonding agent；
6th, intermediate layer composite soldering cream is coated using the method for silk-screen printing for 100 μm of 300 mesh web plates using thickness
Onto the sealing surface of plated film cell piece, the thickness for controlling intermediate layer is 100 μm, obtains being coated with the electricity of intermediate layer composite soldering cream
Pond piece；
7th, the sealing surface of plated film connector is fitted dress with the sealing surface for the cell piece for being coated with intermediate layer composite soldering cream
Match somebody with somebody, be then placed in Muffle furnace, 200 DEG C of insulation 30min degasification are warming up to first, be continuously heating to 300 DEG C of insulation 40min rows
Modeling, then 10min is incubated in the range of being warming up to 1000 DEG C, room temperature is then cooled to, intermediate temperature solid oxide fuel cell is completed
The soldering of the composite soldering system of adaptive sealing-in；
CuO content is 4mol% wherein in step 3 Ag-CuO solders, and glass phase A addition accounts for Ag-CuO solders
2wt%, glass phase B addition account for the 5wt% of Ag-CuO solders.
Embodiment three：The present embodiment is used for the composite soldering system of the adaptive sealing-in of intermediate temperature solid oxide fuel cell
Method for welding is realized according to following steps：
First, the Cu thin layers that thickness in vacuum evaporation is 1 μm are distinguished on the sealing surface of connector and cell piece, plated film is obtained
Connector and plated film cell piece；
2nd, the glass phase A that glass transition temperature the is 680 DEG C and glass phase B that glass transition temperature is 780 DEG C is mixed and ground
It is broken, obtain hybrid glass phase after crossing 300 mesh sieves；
3rd, Ag powder and CuO the powder mixing weighed, obtains Ag-CuO solders, then adds step 2 into Ag-CuO solders
Obtained hybrid glass phase, adds absolute ethyl alcohol and carries out ball milling 3 hours, crosses 300 mesh sieves after being dried at 100 DEG C, obtains solder
Mixed-powder；
4th, ethyl cellulose is dissolved in terpinol, obtains terpineol solution of ethyl cellulose bonding agent, wherein ethyl
The addition of cellulose is 2wt%；
5th, it is 3 by weight:The 1 solder mixed-powder for obtaining step 3 is added to terpineol solution of ethyl cellulose
It is well mixed to obtain intermediate layer composite soldering cream in bonding agent；
6th, intermediate layer composite soldering cream is coated using the method for silk-screen printing for 100 μm of 400 mesh web plates using thickness
Onto the sealing surface of plated film cell piece, the thickness for controlling intermediate layer is 100 μm, obtains being coated with the electricity of intermediate layer composite soldering cream
Pond piece；
7th, the sealing surface of plated film connector is fitted dress with the sealing surface for the cell piece for being coated with intermediate layer composite soldering cream
Match somebody with somebody, be then placed in Muffle furnace, 200 DEG C of insulation 40min degasification are warming up to first, be continuously heating to 300 DEG C of insulation 40min rows
Modeling, then 15min is incubated in the range of being warming up to 1000 DEG C, room temperature is then cooled to, intermediate temperature solid oxide fuel cell is completed
The soldering of the composite soldering system of adaptive sealing-in；
CuO content is 4mol% wherein in step 3 Ag-CuO solders, and glass phase A addition accounts for Ag-CuO solders
5wt%, glass phase B addition account for the 5wt% of Ag-CuO solders.
Claims (8)
1. the composite soldering system for the adaptive sealing-in of intermediate temperature solid oxide fuel cell, it is characterised in that this is used for middle temperature
The composite soldering system of the adaptive sealing-in of SOFC is made up of preformed layer and intermediate layer, and preformed layer exists for evaporation
The Cu thin layers of cell piece and connector sealing station, the Ag-CuO solders that intermediate layer is mixed using Ag powder and CuO powder as matrix,
It is in the base 650~700 DEG C of glass phase A added with glass transition temperature and glass transition temperature is 750~800 DEG C
CuO content is 1~15mol% in glass phase B, wherein Ag-CuO solders；Glass phase A addition accounts for the 1 of Ag-CuO solders
~20wt%, glass phase A by mass percentage by 5%~15% Li2O, 25%~35% SiO2, 15%~25%
BeO, 20%~30% B2O3MgO with 10%~15% is constituted；Glass phase B addition account for Ag-CuO solders 1~
20wt%, B is by mass percentage by 10%~15%Na for the glass phase2O, 30%~40%SiO2, 20%~25%CaO, 10%
~20%B2O3With 10%~20%Al2O3Composition.
2. the composite soldering system according to claim 1 for the adaptive sealing-in of intermediate temperature solid oxide fuel cell,
It is characterized in that the thickness of the copper lamina is 1~2 μm.
3. the method for welding of the composite soldering system for the adaptive sealing-in of intermediate temperature solid oxide fuel cell, it is characterised in that
It is to follow these steps to realize：
First, Cu thin layers in vacuum evaporation are distinguished on the sealing surface of connector and cell piece, plated film connector and plated film electricity is obtained
Pond piece；
2nd, by the glass phase A that glass transition temperature is 650~700 DEG C and glass phase B that glass transition temperature is 750~800 DEG C
Mixing is pulverized, and hybrid glass phase is obtained after crossing 300~400 mesh sieves；
3rd, Ag powder and CuO the powder mixing weighed, obtains Ag-CuO solders, and step 2 is then added into Ag-CuO solders obtains
Hybrid glass phase, add absolute ethyl alcohol carry out ball milling, after drying cross 300~400 mesh sieves, obtain solder mixed-powder；
4th, ethyl cellulose is dissolved in terpinol, obtains terpineol solution of ethyl cellulose bonding agent；
5th, the solder mixed-powder that step 3 is obtained is added in terpineol solution of ethyl cellulose bonding agent, be well mixed
Obtain intermediate layer composite soldering cream；
6th, intermediate layer composite soldering cream is coated on the sealing surface of plated film cell piece using the method for silk-screen printing, applied
It is covered with the cell piece of intermediate layer composite soldering cream；
7th, the sealing surface of plated film connector is fitted assembling with the sealing surface for the cell piece for being coated with intermediate layer composite soldering cream,
It is then placed in Muffle furnace, 200 DEG C of insulation 30~50min degasification is warming up to first, 300~400 DEG C of insulations 30 are continuously heating to
~50min plastic removals, then 5~30min is incubated in the range of being warming up to 1000~1050 DEG C, room temperature is then cooled to, middle temperature is completed
The soldering of the composite soldering system of the adaptive sealing-in of SOFC；
The content of glass phase A wherein described in step 2 accounts for 1~20wt% of Ag-CuO solders, and glass phase B content accounts for Ag-
CuO content accounts for 1~15mol% of Ag-CuO solders in 1~20wt% of CuO solders, step 3.
4. the composite soldering system according to claim 3 for the adaptive sealing-in of intermediate temperature solid oxide fuel cell
Method for welding, it is characterised in that vacuum maintains 5 × 10 during step one evaporation-2More than Pa, current control 120~
150A, voltage is controlled in 10~15V.
5. the composite soldering system according to claim 3 for the adaptive sealing-in of intermediate temperature solid oxide fuel cell
Method for welding, it is characterised in that in step 4 terpineol solution of ethyl cellulose bonding agent the content of ethyl cellulose be 2~
8wt%.
6. the composite soldering system according to claim 3 for the adaptive sealing-in of intermediate temperature solid oxide fuel cell
Method for welding, it is characterised in that step 5 is (2~4) by weight:The 1 solder mixed-powder for obtaining step 3 is added to second
In base cellulose terpineol solution bonding agent.
7. the composite soldering system according to claim 3 for the adaptive sealing-in of intermediate temperature solid oxide fuel cell
Method for welding, it is characterised in that the web plate of 300~400 mesh, screen thickness are used in the method for the silk-screen printing described in step 6
For 100~200 μm.
8. the composite soldering system according to claim 3 for the adaptive sealing-in of intermediate temperature solid oxide fuel cell
Method for welding, it is characterised in that the thickness of the intermediate layer composite soldering cream described in step 6 is 100~200 μm.
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| CN108258263B (en) * | 2018-01-10 | 2020-04-24 | 哈尔滨工业大学 | Low temperature sealing method for solid oxide fuel cell |
| CN110405379B (en) * | 2018-04-27 | 2020-11-13 | 哈尔滨工业大学 | Ag-CuO-B2O3Brazing filler metal, preparation method thereof and method for connecting sapphire by using brazing filler metal |
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| CN102699561A (en) * | 2012-06-21 | 2012-10-03 | 上海交通大学 | Composite brazing alloy for sealing solid oxide fuel cell and brazing technology of composite brazing alloy |
| CN102699558A (en) * | 2012-06-29 | 2012-10-03 | 哈尔滨工业大学 | Flexible composite middle layer brazing alloy and method of utilizing brazing ceramic and metal |
| CN103343247A (en) * | 2013-07-08 | 2013-10-09 | 深圳市亿铖达工业有限公司 | Method for adding trace elements during preparation of composite lead-free solder |
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| US7794170B2 (en) * | 2005-04-22 | 2010-09-14 | Battelle Memorial Institute | Joint with application in electrochemical devices |
| US7691488B2 (en) * | 2007-06-11 | 2010-04-06 | Battelle Memorial Institute | Diffusion barriers in modified air brazes |
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| JPH0917232A (en) * | 1995-06-30 | 1997-01-17 | Tanaka Kikinzoku Internatl Kk | Conductor paste composition |
| CN102699561A (en) * | 2012-06-21 | 2012-10-03 | 上海交通大学 | Composite brazing alloy for sealing solid oxide fuel cell and brazing technology of composite brazing alloy |
| CN102699558A (en) * | 2012-06-29 | 2012-10-03 | 哈尔滨工业大学 | Flexible composite middle layer brazing alloy and method of utilizing brazing ceramic and metal |
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