CN105195846B - Multi-scale combined method for improving strength of soldered joint made of conductive ceramic base materials - Google Patents
Multi-scale combined method for improving strength of soldered joint made of conductive ceramic base materials Download PDFInfo
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- CN105195846B CN105195846B CN201510702499.5A CN201510702499A CN105195846B CN 105195846 B CN105195846 B CN 105195846B CN 201510702499 A CN201510702499 A CN 201510702499A CN 105195846 B CN105195846 B CN 105195846B
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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
- 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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
-
- 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
- B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
-
- 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
- B23K33/00—Specially-profiled edge portions of workpieces for making soldering or welding connections; Filling the seams formed thereby
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- Chemical & Material Sciences (AREA)
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Abstract
The invention belongs to the field of soldering and relates to a multi-scale combined method for improving the strength of a soldered joint made of conductive ceramic base materials. The method solves the problems that a joint connected through an existing conducive ceramic base material soldering method is low in strength, and the residual stress is large and the reliability is low due to the thermal expansion coefficient difference between the ceramic base materials and metal. The method comprises the steps of 1, surface treatment of a conductive ceramic base metal connecting face, 2, solder preparation, 3, solder placement and 4, vacuum soldering connection. Due to the macro-scale and micro-scale combined effect, the joint stress is relieved to the maximum extent, and the strength reliability of the joint is improved. The compression-shear resistant strength of the obtained soldered joint made of the conducive ceramic base materials is 155-265 MPa, and the strength of the soldered joint is improved by 165-345% compared with a soldered joint adopting a conventional straight interface and no wild phase.
Description
Technical field
The present invention relates to a kind of method that multiple dimensioned joint improves conductivity ceramics sill soldering joint strength.
Background technology
Ceramic material all has extensive with its excellent high-temperature comprehensive property in many extreme harsh environments such as Aeronautics and Astronautics
Application prospect, be the preferred material of current hot-end component.But ceramic material fragility is larger, it is difficult to obtain large scale and complex shape
The structural member of shape, greatly limit the engineer applied of ceramic material, therefore, realize ceramic material itself or with metal material
Be reliably connected becomes one of key technology of ceramic material application.Typically using active soldering method realize ceramic to ceramic with
The connection of ceramic-metal, the method process is simple, it is reproducible, to connector size and dimension strong adaptability.Traditional activated pricker
There is chemical reaction with ceramic surface using it by adding active metallic element (such as Ti, Zr, Hf) in solder in soldering method
Form chemical bond and formed and be reliably connected.But, because ceramics are deposited with the hot expansibility of metal (base material metal or solder)
Thermal mismatching in greatest differences, joint cooling procedure produces residual thermal stress in linkage interface, reduces strength of joint and reliability
Property.
The content of the invention
The present invention is to solve the strength of joint of existing conductivity ceramics sill method for welding connection is low, ceramic based material with
The thermal expansion coefficient difference of metal caused by residual stress is big, reliability is low problem, there is provided a kind of multiple dimensioned joint is improved
The method of conductivity ceramics sill soldering joint strength.
The method that a kind of multiple dimensioned joint of the present invention improves conductivity ceramics sill soldering joint strength, is according to the following steps
Carry out：
First, conductivity ceramics base mother metal joint face surface treatment：
A, using precision WEDM machine technology by conductivity ceramics base mother metal and correspondence connector be connected junction be processed into circular arc
Face, if wherein the thermal coefficient of expansion of conductivity ceramics base mother metal is less than the thermal coefficient of expansion of correspondence connector, conductivity ceramics base mother
Material surface is convex surface, and the surface of correspondence connector is concave surface, and radian is equal；If the thermal coefficient of expansion of conductivity ceramics base mother metal is big
In the thermal coefficient of expansion for corresponding to connector, then conductivity ceramics base mother metal surface is concave surface, corresponds to connector for convex surface, radian phase
Deng；
B, the conductivity ceramics base mother metal joint face after wire cutting processes step a are processed into profile of tooth groove-like structure, its
Middle groove depth is 0.3～3mm, and groove width is 0.3～3mm, and the spacing of two grooves is 0.3～2mm, and groove depth direction is cut with face to be connected
The angle in line direction is 90～150 °；
C, by step b be surface-treated after conductivity ceramics base mother metal and step a surface treatment after corresponding connector polish
Cleaning, then cleaned with acetone and dried, the conductivity ceramics base mother metal after being cleaned and correspondingly connector；
2nd, solder is prepared：Composite soldering includes B sources and the system of eutectic alloy containing Ti, the wherein mol ratio of Ti elements and B element
For (10～1):1；B sources are B, TiB2、ZrB2、HfB2, HfB, BN and B4Any one or a few in C is by arbitrarily than composition
Mixture, the system of eutectic alloy containing Ti is Ti-Ni, Ti-Cu, Ag-Cu-Ti or Ti-Si；If conductivity ceramics base mother metal or correspondence connection
Contain B sources in part, be then not added with B sources or reduce B sources addition；The volume content of TiB whiskers is not low in the soldered fitting of end-product
In 5%；
3rd, solder is placed
The composite soldering of step 2 preparation, terpineol, into mastic, are obtained into composite soldering with ethyl cellulose uniform stirring
The mass ratio of cream, wherein composite soldering, terpineol and ethyl cellulose is 10:(0.2～2):(0.4～3), by composite soldering cream
Between the conductivity ceramics base mother metal being coated on after step one cleaning and the joint face of correspondence connector, component to be welded is obtained final product；Or will
The composite soldering cream of preparation is placed between correspondence connector by getting rid of band or being squeezed into after paper tinsel, obtains component to be welded；
4th, vacuum brazing connection
Component to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to into 5 × 10-4～1 × 10-3Pa, then will be true
Empty soldering oven is warming up to temperature T with the speed of 15 DEG C/min1, and 5min～10min is incubated, then heated up with the speed of 10 DEG C/min
To brazing temperature T2, and 10min～20min is incubated, then it is cooled to 400 DEG C with the speed of 5～10 DEG C/min, it is finally cold with stove
But, that is, the soldering connection of conductivity ceramics sill is completed；Wherein T1=T2- (100 DEG C～200 DEG C), T2Higher than solder liquidus curve temperature
Degree 10%～30%.
The method that a kind of multiple dimensioned joint of the present invention improves conductivity ceramics sill soldering joint strength is according to the following steps
Carry out：
First, conductivity ceramics base mother metal joint face surface treatment：
Conductivity ceramics base mother metal joint face is processed into by profile of tooth groove-like structure by wire cutting, surface-treated leading is obtained
Electroceramics base mother metal, wherein groove depth are 0.3～3mm, and groove width is 0.3～3mm, and the spacing of two grooves is 0.3～2mm, groove depth
Direction is 90～150 ° with the angle of face tangential direction to be connected；Correspondence connector and surface-treated conductivity ceramics base is female
Material polishing cleaning, then cleaned with acetone and dried, the conductivity ceramics base mother metal after being cleaned and correspondingly connector；
2nd, solder is prepared：Composite soldering includes B sources and the system of eutectic alloy containing Ti, the wherein mol ratio of Ti elements and B element
For (10～1):1；B sources are B, TiB2、ZrB2、HfB2, HfB, BN and B4Any one or a few in C is by arbitrarily than composition
Mixture, the system of eutectic alloy containing Ti is Ti-Ni, Ti-Cu, Ag-Cu-Ti or Ti-Si；If conductivity ceramics base mother metal or correspondence connection
Contain B sources in part, be then not added with B sources or reduce B sources addition；The volume content of TiB whiskers is not low in the soldered fitting of end-product
In 5%；
3rd, solder is placed
The composite soldering of step 2 preparation, terpineol, into mastic, are obtained into composite soldering with ethyl cellulose uniform stirring
The mass ratio of cream, wherein composite soldering, terpineol and ethyl cellulose is 10:(0.2～2):(0.4～3), by composite soldering cream
Between the conductivity ceramics base mother metal being coated on after step one cleaning and the joint face of correspondence connector, component to be welded is obtained final product；Or will
The composite soldering cream of preparation is placed between correspondence connector by getting rid of band or being squeezed into after paper tinsel, obtains component to be welded；
4th, vacuum brazing connection
Component to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to into 5 × 10-4～1 × 10-3Pa, then will be true
Empty soldering oven is warming up to temperature T with the speed of 15 DEG C/min1, and 5min～10min is incubated, then heated up with the speed of 10 DEG C/min
To brazing temperature T2, and 10min～20min is incubated, then it is cooled to 400 DEG C with the speed of 5～10 DEG C/min, it is finally cold with stove
But, that is, the soldering connection of conductivity ceramics sill is completed；Wherein T1=T2- (100 DEG C～200 DEG C), T2Higher than solder liquidus curve temperature
Degree 10%～30%；Wherein described conductivity ceramics base mother metal is equal with the thermal coefficient of expansion of corresponding connector.
Preparation method of the present invention has the advantage that：
(1) make full use of the conductive characteristic of conductivity ceramics sill to introduce precision WEDM machine technology in macro-scale to connect it
Junction carries out the Secondary Design processing of the surface texture of various ways, can effectively slow down ceramic/metal linkage interface closely ceramic
The stress concentration of side, and the process is simple is easy to operate, low cost；
(2) micro-scale near the soldering interface and in solder layer can in-situ preparation TiB whiskers simultaneously, while have with
Lower effect：
A. linkage interface is carried out carrying out the secondary operations at interface in microcosmic level, is distributed in the TiB whiskers of near interface
Interface connection area can be increased in micro-scale and effectively slow down the stress collection of the nearly ceramics side of ceramic/metal linkage interface
In, residual stress travel direction can also be reversed；
B. solder layer material is modified, solder layer is changed into the reinforcing of Metal Substrate TiB whisker from original simple metal material
Composite, effectively reduces solder layer thermal coefficient of expansion, reduces residual stress；
C. generated in-situ TiB whiskers can effective twisting joint residual stress direction, reduce the probability that crackle occurs.
(3) by the synergy of macro-scale and micro-scale, joint stress is alleviated to the full extent, improve joint
Strength reliability.The anti-compression shear strength of the conductivity ceramics sill soldered fitting that this method is obtained is 155～265MPa, than adopting
165%～345% is improve with conventional straight interface and without the soldering joint strength for strengthening phase.
Description of the drawings
Fig. 1 is the front view of ZrC conductivity ceramics base mother metals surface-treated in embodiment one；
Fig. 2 is the profile of Fig. 1；
Fig. 3 connects for ZrC conductivity ceramics base mother metal/Nb base material metals after the soldering connection of the conductivity ceramics sill of embodiment one
Head assembling schematic diagram；Wherein a is correspondence connector Nb mother metals, and b is composite soldering, and c is profile of tooth groove-like structure, and d is the conductive potteries of ZrC
Porcelain base mother metal；
Fig. 4 is the conventional straight interface and the soldered fitting assembling schematic diagram without enhancing phase of the contrast of embodiment one, and wherein a is
Correspondence connector Nb mother metals, b is composite soldering, and d is ZrC conductivity ceramics base mother metals.
Specific embodiment
Specific embodiment one：A kind of multiple dimensioned joint of present embodiment improves conductivity ceramics sill soldering joint strength
Method, be to carry out according to the following steps：
First, conductivity ceramics base mother metal joint face surface treatment：
A, using precision WEDM machine technology by conductivity ceramics base mother metal and correspondence connector be connected junction be processed into circular arc
Face, if wherein the thermal coefficient of expansion of conductivity ceramics base mother metal is less than the thermal coefficient of expansion of correspondence connector, conductivity ceramics base mother
Material surface is convex surface, and the surface of correspondence connector is concave surface, and radian is equal；If the thermal coefficient of expansion of conductivity ceramics base mother metal is big
In the thermal coefficient of expansion for corresponding to connector, then conductivity ceramics base mother metal surface is concave surface, corresponds to connector for convex surface, radian phase
Deng；
B, the conductivity ceramics base mother metal joint face after wire cutting processes step a are processed into profile of tooth groove-like structure, its
Middle groove depth is 0.3～3mm, and groove width is 0.3～3mm, and the spacing of two grooves is 0.3～2mm, and groove depth direction is cut with face to be connected
The angle in line direction is 90～150 °；
C, by step b be surface-treated after conductivity ceramics base mother metal and step a surface treatment after corresponding connector polish
Cleaning, then cleaned with acetone and dried, the conductivity ceramics base mother metal after being cleaned and correspondingly connector；
2nd, solder is prepared：Composite soldering includes B sources and the system of eutectic alloy containing Ti, the wherein mol ratio of Ti elements and B element
For (10～1):1；B sources are B, TiB2、ZrB2、HfB2, HfB, BN and B4Any one or a few in C is by arbitrarily than composition
Mixture, the system of eutectic alloy containing Ti is Ti-Ni, Ti-Cu, Ag-Cu-Ti or Ti-Si；If conductivity ceramics base mother metal or correspondence connection
Contain B sources in part, be then not added with B sources or reduce B sources addition；The volume content of TiB whiskers is not low in the soldered fitting of end-product
In 5%；
3rd, solder is placed
The composite soldering of step 2 preparation, terpineol, into mastic, are obtained into composite soldering with ethyl cellulose uniform stirring
The mass ratio of cream, wherein composite soldering, terpineol and ethyl cellulose is 10:(0.2～2):(0.4～3), by composite soldering cream
Between the conductivity ceramics base mother metal being coated on after step one cleaning and the joint face of correspondence connector, component to be welded is obtained final product；Or will
The composite soldering cream of preparation is placed between correspondence connector by getting rid of band or being squeezed into after paper tinsel, obtains component to be welded；
4th, vacuum brazing connection
Component to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to into 5 × 10-4～1 × 10-3Pa, then will be true
Empty soldering oven is warming up to temperature T with the speed of 15 DEG C/min1, and 5min～10min is incubated, then heated up with the speed of 10 DEG C/min
To brazing temperature T2, and 10min～20min is incubated, then it is cooled to 400 DEG C with the speed of 5～10 DEG C/min, it is finally cold with stove
But, that is, the soldering connection of conductivity ceramics sill is completed；Wherein T1=T2- (100 DEG C～200 DEG C), T2Higher than solder liquidus curve temperature
Degree 10%～30%.
Preparation method described in present embodiment has the advantage that：
(1) make full use of the conductive characteristic of conductivity ceramics sill to introduce precision WEDM machine technology in macro-scale to connect it
Junction carries out the Secondary Design processing of the surface texture of various ways, can effectively slow down ceramic/metal linkage interface closely ceramic
The stress concentration of side, and the process is simple is easy to operate, low cost；
(2) micro-scale near the soldering interface and in solder layer can in-situ preparation TiB whiskers simultaneously, while have with
Lower effect：
A. linkage interface is carried out carrying out the secondary operations at interface in microcosmic level, is distributed in the TiB whiskers of near interface
Interface connection area can be increased in micro-scale and effectively slow down the stress collection of the nearly ceramics side of ceramic/metal linkage interface
In, residual stress travel direction can also be reversed；
B. solder layer material is modified, solder layer is changed into the reinforcing of Metal Substrate TiB whisker from original simple metal material
Composite, effectively reduces solder layer thermal coefficient of expansion, reduces residual stress；
C. generated in-situ TiB whiskers can effective twisting joint residual stress direction, reduce the probability that crackle occurs.
(3) by the synergy of macro-scale and micro-scale, joint stress is alleviated to the full extent, improve joint
Strength reliability.The anti-compression shear strength of the conductivity ceramics sill soldered fitting that this method is obtained is 155～265MPa, than adopting
165%～345% is improve with conventional straight interface and without the soldering joint strength for strengthening phase.
Specific embodiment two：Present embodiment from unlike specific embodiment one：Described corresponding connector is
Metal or conductivity ceramics base mother metal.Other are identical with specific embodiment one.
Specific embodiment three：Present embodiment from unlike specific embodiment one or two：Described conductivity ceramics
Base mother metal refers to the ceramic based material with conductive characteristic to be connected with itself or metal_based material.Other and specific embodiment party
Formula one or two is identical.Conductivity ceramics base mother metal is boride-based ceramics, carbide base ceramics, conductive oxidation in present embodiment
The nitride base ceramics of thing base ceramics or conduction.
Specific embodiment four：Unlike one of present embodiment and specific embodiment one to three：Described metal
For titanium alloy, niobium alloy or molybdenum alloy.Other are identical with one of specific embodiment one to three.
Specific embodiment five：Unlike one of present embodiment and specific embodiment one to four：Institute in step one
Any two groove is parallel to each other or interlaced in the profile of tooth groove-like structure stated.Other are one of with specific embodiment one to four
It is identical.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five：Described is compound
The form of solder is powdery, foil-like or lamellar.Other are identical with one of specific embodiment one to five.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment one to six：Institute in step 2
B sources in the composite soldering stated are incorporated in active eutectic solder in the way of powder body ball milling mixing, or by multiple melting
Mode is incorporated in active eutectic solder, or is incorporated into active eutectic solder by plating, magnetron sputtering or electronics evaporation
On outer surface.Other are identical with one of specific embodiment one to six.
Specific embodiment eight：A kind of multiple dimensioned joint of present embodiment improves conductivity ceramics sill soldering joint strength
Method, be to carry out according to the following steps：
First, conductivity ceramics base mother metal joint face surface treatment：
Conductivity ceramics base mother metal joint face is processed into by profile of tooth groove-like structure by wire cutting, surface-treated leading is obtained
Electroceramics base mother metal, wherein groove depth are 0.3～3mm, and groove width is 0.3～3mm, and the spacing of two grooves is 0.3～2mm, groove depth
Direction is 90～150 ° with the angle of face tangential direction to be connected；Correspondence connector and surface-treated conductivity ceramics base is female
Material polishing cleaning, then cleaned with acetone and dried, the conductivity ceramics base mother metal after being cleaned and correspondingly connector；
2nd, solder is prepared：Composite soldering includes B sources and the system of eutectic alloy containing Ti, the wherein mol ratio of Ti elements and B element
For (10～1):1；B sources are B, TiB2、ZrB2、HfB2, HfB, BN and B4Any one or a few in C is by arbitrarily than composition
Mixture, the system of eutectic alloy containing Ti is Ti-Ni, Ti-Cu, Ag-Cu-Ti or Ti-Si；If conductivity ceramics base mother metal or correspondence connection
Contain B sources in part, be then not added with B sources or reduce B sources addition；The volume content of TiB whiskers is not low in the soldered fitting of end-product
In 5%；
3rd, solder is placed
The composite soldering of step 2 preparation, terpineol, into mastic, are obtained into composite soldering with ethyl cellulose uniform stirring
The mass ratio of cream, wherein composite soldering, terpineol and ethyl cellulose is 10:(0.2～2):(0.4～3), by composite soldering cream
Between the conductivity ceramics base mother metal being coated on after step one cleaning and the joint face of correspondence connector, component to be welded is obtained final product；Or will
The composite soldering cream of preparation is placed between correspondence connector by getting rid of band or being squeezed into after paper tinsel, obtains component to be welded；
4th, vacuum brazing connection
Component to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to into 5 × 10-4～1 × 10-3Pa, then will be true
Empty soldering oven is warming up to temperature T with the speed of 15 DEG C/min1, and 5min～10min is incubated, then heated up with the speed of 10 DEG C/min
To brazing temperature T2, and 10min～20min is incubated, then it is cooled to 400 DEG C with the speed of 5～10 DEG C/min, it is finally cold with stove
But, that is, the soldering connection of conductivity ceramics sill is completed；Wherein T1=T2- (100 DEG C～200 DEG C), T2Higher than solder liquidus curve temperature
Degree 10%～30%；Wherein described conductivity ceramics base mother metal is equal with the thermal coefficient of expansion of corresponding connector.
Specific embodiment nine：Present embodiment from unlike specific embodiment eight：Described corresponding connector is
Metal or conductivity ceramics base mother metal.Other are identical with specific embodiment eight.
Specific embodiment ten：Present embodiment from unlike specific embodiment eight or nine：Described conductivity ceramics
Base mother metal refers to the ceramic based material with conductive characteristic to be connected with itself or metal_based material.Other and specific embodiment party
Formula eight or nine is identical.Conductivity ceramics base mother metal is boride-based ceramics, carbide base ceramics, conductive oxidation in present embodiment
The nitride base ceramics of thing base ceramics or conduction.
Specific embodiment 11：Unlike one of present embodiment and specific embodiment eight to ten：Described gold
Belong to for titanium alloy, niobium alloy or molybdenum alloy.Other are identical with one of specific embodiment eight to ten.
Specific embodiment 12：Present embodiment from unlike specific embodiment eight to one of 11：Step one
Described in profile of tooth groove-like structure in any two groove for parallel to each other or interlaced.Other and specific embodiment eight to ten
One of one is identical.
Specific embodiment 13：Present embodiment from unlike specific embodiment eight to 12：Described is compound
The form of solder is powdery, foil-like or lamellar.Other are identical with specific embodiment eight to 12.
Specific embodiment 14：Present embodiment from unlike specific embodiment eight to 13：Institute in step 2
B sources in the composite soldering stated are incorporated in active eutectic solder in the way of powder body ball milling mixing, or by multiple melting
Mode is incorporated in active eutectic solder, or is incorporated into active eutectic solder by plating, magnetron sputtering or electronics evaporation
On outer surface.Other are identical with specific embodiment eight to 13.
The following examples will be further described to the present invention, but not thereby limiting the invention.
Embodiment 1：The method that a kind of multiple dimensioned joint of the present embodiment improves conductivity ceramics sill soldering joint strength, be
Carry out according to the following steps：
First, conductivity ceramics base mother metal joint face surface treatment：
A, the ZrC conductivity ceramics base mother metals and correspondence connector Nb mother metals junction that is connected is added using precision WEDM machine technology
Into arc surface, wherein ZrC mother metals surface is convex surface to work, and the surface of correspondence connector Nb mother metals is concave surface, and the equal circular arc of radian
Radius is 20mm；
B, the ZrC conductivity ceramics base mother metal joint faces after wire cutting processes step a are processed into profile of tooth groove-like structure,
Wherein groove depth is 1.5mm, and groove width is 0.4mm, and the spacing of two grooves is 0.8mm, groove depth direction and face tangential direction to be connected
Angle be 90 °；
C, by step b be surface-treated after ZrC conductivity ceramics base mother metals and step a surface treatment after corresponding connector Nb
Mother metal polishing cleaning, then cleaned with acetone and dried, the conductivity ceramics base mother metal after being cleaned and correspondingly connector；
2nd, solder is prepared：Composite soldering includes TiB2With Ag-Cu-Ti eutectic alloys system, concrete compound method is：Respectively
Weigh Ag, Cu, TiB2、TiH2Powder, its mass percent is respectively：67%th, 24%, 1.5%, 7.5%, by various solder powder
It is sufficiently mixed using ball mill, is obtained composite soldering；
3rd, solder is placed
The composite soldering of step 2 preparation, terpineol, into mastic, are obtained into composite soldering with ethyl cellulose uniform stirring
The mass ratio of cream, wherein composite soldering, terpineol and ethyl cellulose is 10:0.35:1, composite soldering cream is coated on into step
One cleaning after conductivity ceramics base mother metal and correspondence connector joint face between, coating thickness be 200 μm, obtain final product to be welded group
Part；
4th, vacuum brazing connection
Component to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to into 5 × 10-4Pa, then by vacuum brazing furnace
750 DEG C of temperature is warming up to the speed of 15 DEG C/min, and is incubated 10min, then brazing temperature is warming up to the speed of 10 DEG C/min
900 DEG C, and 20min is incubated, then 400 DEG C being cooled to the speed of 5 DEG C/min, last furnace cooling completes conductivity ceramics
The soldering connection of sill.
Wherein the front view of the surface-treated ceramic base ZrC mother metals of step one is as shown in figure 1, profile is as shown in Figure 2.
ZrC conductivity ceramics base mother metal/Nb base material metals joint dress after the soldering connection of the present embodiment conductivity ceramics sill
It is as shown in Figure 3 with schematic diagram.
Conventional straight interface and the soldering processes without enhancing phase as a comparison is as follows：
First, after by ZrC conductivity ceramics base mother metals and the polishing cleaning of Nb mother metals straight joint face, with acetone thoroughly cleaning and dry
It is dry, the ceramic base mother metal after being cleaned and correspondingly connector；
2nd, Ag, Cu, TiH are weighed respectively2Powder, its mass percent is respectively：69.3%th, 26.4%, 4.3%, will be each
Plant solder powder to be sufficiently mixed using ball mill, obtain composite soldering；Composite soldering cream is coated on after step one cleans
Between the joint face of conductivity ceramics base mother metal and correspondence connector, coating thickness is 200 μm, obtains final product component to be welded；
3rd, the part to be welded obtained by step 3 is placed in vacuum drying oven, then by vacuum brazing furnace with the speed of 15 DEG C/min
750 DEG C are warming up to, and are incubated 10min, then 900 DEG C of brazing temperature is warming up to the speed of 10 DEG C/min, and be incubated 20min, so
Afterwards 400 DEG C are cooled to the speed of 5 DEG C/min, last furnace cooling completes the soldering connection of conductivity ceramics sill；Soldering
Joint assembling schematic diagram is as shown in Figure 4.
The joint that the method for improving conductivity ceramics sill soldering joint strength using multiple dimensioned joint is obtained, by room temperature
Static load compression shear tests (loading speed is 0.5mm/s), and it is 221MPa to measure shear strength, and conventional straight interface as a comparison
With without the soldered fitting for strengthening phase, the shear strength under same test condition is only 58MPa, i.e., obtained using the inventive method
Soldered fitting shear strength improves 283%.
The method that a kind of multiple dimensioned joint of embodiment 2, the present embodiment improves conductivity ceramics sill soldering joint strength, be
Carry out according to the following steps：
First, conductivity ceramics base mother metal joint face surface treatment：
A, the conductivity ceramics base ZrC mother metals and correspondence connector Nb mother metals junction that is connected is added using precision WEDM machine technology
Work is convex surface into arc surface, wherein ZrC mother metals surface, and the surface of correspondence connector Nb mother metals is concave surface, and radian is equal, circular arc
Radius is 15mm；
B, the conductivity ceramics base ZrC mother metal joint faces after wire cutting processes step a are processed into profile of tooth groove-like structure,
Wherein groove depth is 1.5mm, and groove width is 0.4mm, and the spacing of two grooves is 0.8mm, groove depth direction and face tangential direction to be connected
Angle be 90 °；
C, by step b be surface-treated after ZrC conductivity ceramics base mother metals and step a surface treatment after corresponding connector Nb
Mother metal polishing cleaning, then cleaned with acetone and dried, the conductivity ceramics base mother metal after being cleaned and correspondingly connector；
2nd, solder is prepared：Composite soldering includes TiB2With Ag-Cu-Ti eutectic alloys system, concrete compound method is：Respectively
Weigh Ag, Cu, TiB2、TiH2Powder, its mass percent is respectively：64.5%th, 20%, 7.2%, 8.3%, by various solders
Powder is sufficiently mixed using ball mill, obtains composite soldering；
3rd, solder is placed
The composite soldering of step 2 preparation, terpineol, into mastic, are obtained into composite soldering with ethyl cellulose uniform stirring
The mass ratio of cream, wherein composite soldering, terpineol and ethyl cellulose is 10:0.35:1, composite soldering cream is coated on into step
One cleaning after conductivity ceramics base mother metal and correspondence connector joint face between, coating thickness be 200 μm, obtain final product to be welded group
Part；
4th, vacuum brazing connection
Component to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to into 5 × 10-4Pa, then by vacuum brazing furnace
750 DEG C of temperature is warming up to the speed of 15 DEG C/min, and is incubated 10min, then brazing temperature is warming up to the speed of 10 DEG C/min
900 DEG C, and 20min is incubated, then 400 DEG C being cooled to the speed of 5 DEG C/min, last furnace cooling completes conductivity ceramics
The soldering connection of sill.
Conventional straight interface and the soldering processes without enhancing phase as a comparison is as follows：
First, after by ZrC conductivity ceramics base mother metals and the polishing cleaning of Nb mother metals straight joint face, with acetone thoroughly cleaning and dry
It is dry, the conductivity ceramics base mother metal after being cleaned and correspondingly connector；
2nd, Ag, Cu, TiH are weighed respectively2Powder, its mass percent is respectively：69.3%th, 26.4%, 4.3%, will be each
Plant solder powder to be sufficiently mixed using ball mill, obtain composite soldering；Composite soldering cream is coated on after step one cleans
Between the joint face of conductivity ceramics base mother metal and correspondence connector, coating thickness is 200 μm, obtains final product component to be welded；
3rd, the part to be welded obtained by step 3 is placed in vacuum drying oven, then by vacuum brazing furnace with the speed of 15 DEG C/min
750 DEG C are warming up to, and are incubated 10min, then 900 DEG C of brazing temperature is warming up to the speed of 10 DEG C/min, and be incubated 20min, so
Afterwards 400 DEG C are cooled to the speed of 5 DEG C/min, last furnace cooling completes the soldering connection of conductivity ceramics sill；
The joint that the method for improving conductivity ceramics sill soldering joint strength using multiple dimensioned joint is obtained, by room temperature
Static load compression shear tests (loading speed is 0.5mm/s), and it is 258MPa to measure shear strength, and conventional straight interface as a comparison
With without the soldered fitting for strengthening phase, the shear strength under same test condition is only 58MPa, i.e., obtained using the inventive method
Soldered fitting shear strength improves 345%.
Embodiment 3：The method that a kind of multiple dimensioned joint of the present embodiment improves conductivity ceramics sill soldering joint strength, be
Carry out according to the following steps：
First, conductivity ceramics base mother metal joint face surface treatment：
Conductivity ceramics base ZrC mother metal joint faces are processed into by profile of tooth groove-like structure by wire cutting, obtain surface-treated
Conductivity ceramics base mother metal, wherein groove depth is 1.5mm, and groove width is 0.4mm, and the spacing of two grooves is 0.8mm, groove depth direction with
The angle of face tangential direction to be connected is 90 °；By correspondence connector and surface-treated conductivity ceramics base mother metal polishing cleaning,
Cleaned with acetone and dried again, the conductivity ceramics base mother metal after being cleaned and correspondingly connector；
2nd, solder is prepared：Composite soldering includes TiB2With Ag-Cu-Ti eutectic alloys system, concrete compound method is：Respectively
Weigh Ag, Cu, TiB2、TiH2Powder, its mass percent is respectively：67%th, 24%, 1.5%, 7.5%, by various solder powder
It is sufficiently mixed using ball mill, is obtained composite soldering；
3rd, solder is placed
The composite soldering of step 2 preparation, terpineol, into mastic, are obtained into composite soldering with ethyl cellulose uniform stirring
The mass ratio of cream, wherein composite soldering, terpineol and ethyl cellulose is 10:0.35:1, composite soldering cream is coated on into step
One cleaning after conductivity ceramics base mother metal and correspondence connector joint face between, coating thickness be 200 μm, obtain final product to be welded group
Part；
4th, vacuum brazing connection
Component to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to into 5 × 10-4Pa, then by vacuum brazing furnace
750 DEG C of temperature is warming up to the speed of 15 DEG C/min, and is incubated 10min, then brazing temperature is warming up to the speed of 10 DEG C/min
900 DEG C, and 20min is incubated, then 400 DEG C being cooled to the speed of 5 DEG C/min, last furnace cooling completes conductivity ceramics
The soldering connection of sill.
Conventional straight interface and the soldering processes without enhancing phase as a comparison is as follows：
First, after by the straight joint face polishing cleaning of two pieces of ZrC conductivity ceramics base mother metals, with acetone thoroughly cleaning and dry,
Conductivity ceramics base mother metal after being cleaned；
2nd, Ag, Cu, TiH are weighed respectively2Powder, its mass percent is respectively：69.3%th, 26.4%, 4.3%, will be each
Plant solder powder to be sufficiently mixed using ball mill, obtain composite soldering；Composite soldering cream is coated on after step one cleans
Between two pieces of conductivity ceramics base mother metal joint faces, coating thickness is 200 μm, obtains final product component to be welded；
3rd, the part to be welded obtained by step 3 is placed in vacuum drying oven, then by vacuum brazing furnace with the speed of 15 DEG C/min
750 DEG C are warming up to, and are incubated 10min, then 900 DEG C of brazing temperature is warming up to the speed of 10 DEG C/min, and be incubated 20min, so
Afterwards 400 DEG C are cooled to the speed of 5 DEG C/min, last furnace cooling completes the soldering connection of conductivity ceramics sill；
The joint that the method for improving conductivity ceramics sill soldering joint strength using multiple dimensioned joint is obtained, by room temperature
Static load compression shear tests (loading speed is 0.5mm/s), and it is 205MPa to measure shear strength, and conventional straight interface as a comparison
With without the soldered fitting for strengthening phase, the shear strength under same test condition is only 76MPa, i.e., obtained using the inventive method
Soldered fitting shear strength improves 171%
The synergy that macro-scale and micro-scale are passed through by above example, the present invention, to the full extent
Joint stress is alleviated, the strength reliability of joint is improved.The resistance to compression of the conductivity ceramics sill soldered fitting that this method is obtained
Intensity is cut for 165～265MPa, than improve 165% using conventional straight interface and without the soldering joint strength for strengthening phase～
345%.
Claims (10)
1. it is a kind of it is multiple dimensioned joint improve conductivity ceramics sill soldering joint strength method, it is characterised in that the method press with
Lower step is carried out：
First, conductivity ceramics base mother metal joint face surface treatment：
A, using precision WEDM machine technology by conductivity ceramics base mother metal and correspondence connector be connected junction be processed into arc surface, its
If in conductivity ceramics base mother metal thermal coefficient of expansion less than correspondence connector thermal coefficient of expansion, conductivity ceramics base mother metal surface
For convex surface, the surface of correspondence connector is concave surface, and radian is equal；If the thermal coefficient of expansion of conductivity ceramics base mother metal is more than correspondence
The thermal coefficient of expansion of connector, then conductivity ceramics base mother metal surface is concave surface, and correspondence connector is convex surface, and radian is equal；
B, the conductivity ceramics base mother metal joint face after wire cutting processes step a are processed into profile of tooth groove-like structure, its bracket groove
Depth is 0.3～3mm, and groove width is 0.3～3mm, and the spacing of two grooves is 0.3～2mm, groove depth direction and face tangent line side to be connected
To angle be 90～150 °；
C, cleaning that the corresponding connector after the conductivity ceramics base mother metal after the surface treatment of step b and the surface treatment of step a is polished,
Cleaned with acetone and dried again, the conductivity ceramics base mother metal after being cleaned and correspondingly connector；
2nd, solder is prepared：Composite soldering includes B sources and the system of eutectic alloy containing Ti, and the mol ratio of wherein Ti elements and B element is
(10～1):1；B sources are B, TiB2、ZrB2、HfB2, HfB, BN and B4Any one or a few in C is by mixed arbitrarily than composition
Compound, the system of eutectic alloy containing Ti is Ti-Ni, Ti-Cu, Ag-Cu-Ti or Ti-Si；If conductivity ceramics base mother metal or correspondence connector
In contain B sources, then be not added with B sources or reduce B sources addition；The volume content of TiB whiskers is not less than in the soldered fitting of end-product
5%；
3rd, solder is placed
The composite soldering of step 2 preparation, terpineol, into mastic, are obtained into composite soldering cream with ethyl cellulose uniform stirring, its
The mass ratio of middle composite soldering, terpineol and ethyl cellulose is 10:(0.2～2):(0.4～3), by the coating of composite soldering cream
In step one cleaning after conductivity ceramics base mother metal and correspondence connector joint face between, obtain final product component to be welded；Or will prepare
Composite soldering cream by get rid of band or be squeezed into after paper tinsel be placed in correspondence connector between, obtain component to be welded；
4th, vacuum brazing connection
Component to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to into 5 × 10-4～1 × 10-3Pa, then by vacuum pricker
Brazier is warming up to temperature T with the speed of 15 DEG C/min1, and 5min～10min is incubated, then pricker is warming up to the speed of 10 DEG C/min
Weldering temperature T2, and 10min～20min is incubated, then it is cooled to 400 DEG C with the speed of 5～10 DEG C/min, last furnace cooling,
Complete the soldering connection of conductivity ceramics sill；Wherein T1=T2- (100 DEG C～200 DEG C), T2Higher than solder liquidus temperature
10%～30%.
2. the method that a kind of multiple dimensioned joint according to claim 1 improves conductivity ceramics sill soldering joint strength,
It is characterized in that described corresponding connector is metal or conductivity ceramics base mother metal.
3. a kind of multiple dimensioned joint according to claim 1 and 2 improves the side of conductivity ceramics sill soldering joint strength
Method, it is characterised in that described conductivity ceramics base mother metal refers to the pottery with conductive characteristic being connected with itself or metal_based material
Porcelain sill.
4. the method that a kind of multiple dimensioned joint according to claim 2 improves conductivity ceramics sill soldering joint strength,
It is characterized in that described metal is titanium alloy, niobium alloy or molybdenum alloy.
5. the method that a kind of multiple dimensioned joint according to claim 1 improves conductivity ceramics sill soldering joint strength,
It is characterized in that any two groove is parallel to each other or interlaced in the profile of tooth groove-like structure described in step one.
6. the method that a kind of multiple dimensioned joint according to claim 1 improves conductivity ceramics sill soldering joint strength,
It is characterized in that the form of described composite soldering is powdery.
7. the method that a kind of multiple dimensioned joint according to claim 1 improves conductivity ceramics sill soldering joint strength,
It is characterized in that the B sources in the composite soldering described in step 2 are incorporated into active eutectic solder in the way of powder body ball milling mixing
In, or be incorporated into by way of multiple melting in active eutectic solder, or drawn by plating, magnetron sputtering or electronics evaporation
Enter on the outer surface of active eutectic solder.
8. it is a kind of it is multiple dimensioned joint improve conductivity ceramics sill soldering joint strength method, it is characterised in that the method press with
Lower step is carried out：
First, conductivity ceramics base mother metal joint face surface treatment：
Profile of tooth groove-like structure is processed in conductivity ceramics base mother metal joint face by wire cutting, surface-treated conductive pottery is obtained
Porcelain base mother metal, wherein groove depth are 0.3～3mm, and groove width is 0.3～3mm, and the spacing of two grooves is 0.3～2mm, groove depth direction
It it is 90～150 ° with the angle of face tangential direction to be connected；Correspondence connector and surface-treated conductivity ceramics base mother metal are beaten
Mill cleaning, then cleaned with acetone and dried, the conductivity ceramics base mother metal after being cleaned and correspondingly connector；
2nd, solder is prepared：Composite soldering includes B sources and the system of eutectic alloy containing Ti, and the mol ratio of wherein Ti elements and B element is
(10～1):1；B sources are B, TiB2、ZrB2、HfB2, HfB, BN and B4Any one or a few in C is by mixed arbitrarily than composition
Compound, the system of eutectic alloy containing Ti is Ti-Ni, Ti-Cu, Ag-Cu-Ti or Ti-Si；If conductivity ceramics base mother metal or correspondence connector
In contain B sources, then be not added with B sources or reduce B sources addition；The volume content of TiB whiskers is not less than in the soldered fitting of end-product
5%；
3rd, solder is placed
The composite soldering of step 2 preparation, terpineol, into mastic, are obtained into composite soldering cream with ethyl cellulose uniform stirring, its
The mass ratio of middle composite soldering, terpineol and ethyl cellulose is 10:(0.2～2):(0.4～3), by the coating of composite soldering cream
In step one cleaning after conductivity ceramics base mother metal and correspondence connector joint face between, obtain final product component to be welded；Or will prepare
Composite soldering cream by get rid of band or be squeezed into after paper tinsel be placed in correspondence connector between, obtain component to be welded；
4th, vacuum brazing connection
Component to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to into 5 × 10-4～1 × 10-3Pa, then by vacuum pricker
Brazier is warming up to temperature T with the speed of 15 DEG C/min1, and 5min～10min is incubated, then pricker is warming up to the speed of 10 DEG C/min
Weldering temperature T2, and 10min～20min is incubated, then it is cooled to 400 DEG C with the speed of 5～10 DEG C/min, last furnace cooling,
Complete the soldering connection of conductivity ceramics sill；Wherein T1=T2- (100 DEG C～200 DEG C), T2Higher than solder liquidus temperature
10%～30%；Wherein described conductivity ceramics base mother metal is equal with the thermal coefficient of expansion of corresponding connector.
9. the method that a kind of multiple dimensioned joint according to claim 8 improves conductivity ceramics sill soldering joint strength,
It is characterized in that described corresponding connector is metal or conductivity ceramics base mother metal；Wherein conductivity ceramics base mother metal is referred to and itself
Or the ceramic based material with conductive characteristic of metal_based material connection.
10. the method that a kind of multiple dimensioned joint according to claim 9 improves conductivity ceramics sill soldering joint strength,
It is characterized in that described metal is titanium alloy, niobium alloy or molybdenum alloy.
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| CN106312369A (en) * | 2016-10-31 | 2017-01-11 | 天津航空机电有限公司 | Solder for connecting ceramics with kovar alloys |
| CN109465570B (en) * | 2018-12-13 | 2022-02-01 | 郑州机械研究所有限公司 | Ti-Si high-temperature brazing filler metal |
| CN111747769B (en) * | 2020-06-30 | 2022-12-09 | 哈尔滨工业大学（威海） | AlMgB 14 -TiB 2 Vacuum brazing method for composite ceramic and TiAl-based alloy |
| CN112638062A (en) * | 2021-03-10 | 2021-04-09 | 北京漠石科技有限公司 | Active brazing filler metal for ceramic circuit board |
| CN113275683B (en) * | 2021-03-29 | 2022-09-23 | 南京工程学院 | Preparation method of metal ceramic composite material with overlapped double bionic structures |
| CN114633218B (en) * | 2022-03-04 | 2023-09-19 | 贵州捷盛钻具股份有限公司 | Surface treatment method and device for drill rod and drill rod manufacturing method |
| CN115709318A (en) * | 2022-12-08 | 2023-02-24 | 哈尔滨工业大学 | Unilateral heat source resistance brazing method for conductive ceramics and metal |
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