CN105195846A - 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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- CN105195846A CN105195846A CN201510702499.5A CN201510702499A CN105195846A CN 105195846 A CN105195846 A CN 105195846A CN 201510702499 A CN201510702499 A CN 201510702499A CN 105195846 A CN105195846 A CN 105195846A
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- China
- Prior art keywords
- conductivity ceramics
- mother metal
- corresponding connector
- base mother
- ceramics base
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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
- 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
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 multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength.
Background technology
Ceramic material is all with a wide range of applications at many extreme harsh environment such as Aeronautics and Astronautics with the high-temperature comprehensive property of its excellence, is the preferred material of current hot-end component.But ceramic material fragility is larger, be difficult to the structural member obtaining large scale and complicated shape, greatly limit the engineer applied of ceramic material, therefore, realize ceramic material self or be connected with metal material reliable becoming one of key technology that ceramic material applies.General employing active soldering method realizes the connection of ceramic to ceramic and ceramic-metal, and the method technique is simple, reproducible, to connector size and dimension strong adaptability.Traditional activated method for welding, by adding active metallic element (as Ti, Zr, Hf etc.) in solder, utilizes it form chemical bond with ceramic surface generation chemical reaction and form reliable connection.But because pottery and the hot expansibility of metal (base material metal or solder) exist greatest differences, the thermal mismatching in joint cooling procedure produces residual thermal stress at linkage interface, reduces strength of joint and reliability.
Summary of the invention
The present invention will solve the problem that residual stress is large, reliability is low that low, the ceramic based material of strength of joint that existing conductivity ceramics sill method for welding connects causes with the thermal expansion coefficient difference of metal, provides a kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength.
A kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength of the present invention is carried out according to the following steps:
One, conductivity ceramics base mother metal joint face surface treatment:
A, the precision WEDM machine technology junction that conductivity ceramics base mother metal and corresponding connector is connected is utilized to be processed into arc surface, if wherein the thermal coefficient of expansion of conductivity ceramics base mother metal is less than the thermal coefficient of expansion of corresponding connector, then conductivity ceramics base mother metal surface is convex surface, the surface of corresponding connector is concave surface, and radian is equal; If the thermal coefficient of expansion of conductivity ceramics base mother metal is greater than the thermal coefficient of expansion of corresponding connector, then conductivity ceramics base mother metal surface is concave surface, and corresponding connector is convex surface, and radian is equal;
B, by Linear cut, the conductivity ceramics base mother metal joint face after step a process is processed into profile of tooth channel-shaped structure, wherein groove depth is 0.3 ~ 3mm, groove width is 0.3 ~ 3mm, and the spacing of two grooves is 0.3 ~ 2mm, and the angle of groove depth direction and to be connected tangential direction is 90 ~ 150 °;
C, by the corresponding connector polishing cleaning after the conductivity ceramics base mother metal after step b surface treatment and step a surface treatment, then clean with acetone and dry, obtaining the conductivity ceramics base mother metal after cleaning and corresponding connector;
Two, solder is prepared: composite soldering comprises B source and containing Ti eutectic alloy system, wherein the mol ratio of Ti element and B element is (10 ~ 1): 1; B source is B, TiB
2, ZrB
2, HfB
2, HfB, BN and B
4any one or a few in C, by arbitrarily than the mixture of composition, is Ti-Ni, Ti-Cu, Ag-Cu-Ti or Ti-Si containing Ti eutectic alloy; If contain B source in conductivity ceramics base mother metal or corresponding connector, then do not add B source or reduce B source addition; In the soldered fitting of end-product, the volume content of TiB whisker is not less than 5%;
Three, solder is placed
Composite soldering step 2 prepared, terpinol become lotion with ethyl cellulose uniform stirring, obtain composite soldering cream, wherein the mass ratio of composite soldering, terpinol and ethyl cellulose is 10:(0.2 ~ 2): (0.4 ~ 3), composite soldering cream is coated on step one clean after conductivity ceramics base mother metal and the joint face of corresponding connector between, obtain assembly to be welded; Maybe the composite soldering cream of preparation is placed between corresponding connector by getting rid of band or being squeezed into paper tinsel, obtains assembly to be welded;
Four, vacuum brazing connects
Assembly to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to 5 × 10
-4~ 1 × 10
-3pa, is then warming up to temperature T by vacuum brazing furnace with the speed of 15 DEG C/min
1, and be incubated 5min ~ 10min, then be warming up to brazing temperature T with the speed of 10 DEG C/min
2, and be incubated 10min ~ 20min, be then cooled to 400 DEG C with the speed of 5 ~ 10 DEG C/min, finally with stove cooling, namely complete the brazing of conductivity ceramics sill; Wherein T
1=T
2-(100 DEG C ~ 200 DEG C), T
2higher than solder liquidus temperature 10% ~ 30%.
A kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength of the present invention is carried out according to the following steps:
One, conductivity ceramics base mother metal joint face surface treatment:
By Linear cut, conductivity ceramics base mother metal joint face is processed into profile of tooth channel-shaped structure, obtain surface-treated conductivity ceramics base mother metal, wherein groove depth is 0.3 ~ 3mm, groove width is 0.3 ~ 3mm, the spacing of two grooves is 0.3 ~ 2mm, and the angle of groove depth direction and to be connected tangential direction is 90 ~ 150 °; By corresponding connector and surface-treated conductivity ceramics base mother metal polishing cleaning, then clean with acetone and dry, obtaining the conductivity ceramics base mother metal after cleaning and corresponding connector;
Two, solder is prepared: composite soldering comprises B source and containing Ti eutectic alloy system, wherein the mol ratio of Ti element and B element is (10 ~ 1): 1; B source is B, TiB
2, ZrB
2, HfB
2, HfB, BN and B
4any one or a few in C, by arbitrarily than the mixture of composition, is Ti-Ni, Ti-Cu, Ag-Cu-Ti or Ti-Si containing Ti eutectic alloy; If contain B source in conductivity ceramics base mother metal or corresponding connector, then do not add B source or reduce B source addition; In the soldered fitting of end-product, the volume content of TiB whisker is not less than 5%;
Three, solder is placed
Composite soldering step 2 prepared, terpinol become lotion with ethyl cellulose uniform stirring, obtain composite soldering cream, wherein the mass ratio of composite soldering, terpinol and ethyl cellulose is 10:(0.2 ~ 2): (0.4 ~ 3), composite soldering cream is coated on step one clean after conductivity ceramics base mother metal and the joint face of corresponding connector between, obtain assembly to be welded; Maybe the composite soldering cream of preparation is placed between corresponding connector by getting rid of band or being squeezed into paper tinsel, obtains assembly to be welded;
Four, vacuum brazing connects
Assembly to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to 5 × 10
-4~ 1 × 10
-3pa, is then warming up to temperature T by vacuum brazing furnace with the speed of 15 DEG C/min
1, and be incubated 5min ~ 10min, then be warming up to brazing temperature T with the speed of 10 DEG C/min
2, and be incubated 10min ~ 20min, be then cooled to 400 DEG C with the speed of 5 ~ 10 DEG C/min, finally with stove cooling, namely complete the brazing of conductivity ceramics sill; Wherein T
1=T
2-(100 DEG C ~ 200 DEG C), T
2higher than solder liquidus temperature 10% ~ 30%; Wherein said conductivity ceramics base mother metal is equal with the thermal coefficient of expansion of corresponding connector.
Preparation method's tool of the present invention has the following advantages:
(1) conductive characteristic making full use of conductivity ceramics sill in macro-scale introduces precision WEDM machine technology carries out the surface texture of various ways Secondary Design processing to its joint face, the stress that effectively can slow down the nearly ceramic side of ceramic/metal linkage interface is concentrated, and this technique is simple to operation, cost is low;
(2) micro-scale can simultaneously in-situ preparation TiB whisker near soldering interface and in solder layer, has following effect simultaneously:
A. the secondary operations of carrying out interface at microcosmic level is carried out to linkage interface, be distributed near interface TiB whisker can micro-scale add interface connection area and effectively slow down the nearly ceramic side of ceramic/metal linkage interface stress concentrate, can also reverse residual stress travel direction;
B. carry out modification to solder layer material, solder layer becomes Metal Substrate TiB whisker reinforced composite material from original simple metal material, effectively reduces solder layer thermal coefficient of expansion, reduces residual stress;
C. generated in-situ TiB whisker can the direction of effective twisting joint residual stress, reduces the probability that crackle occurs.
(3) by the synergy of macro-scale and micro-scale, alleviate joint stress to the full extent, improve the strength reliability of joint.The anti-compression shear strength of the conductivity ceramics sill soldered fitting that this method obtains is 155 ~ 265MPa, than adopting conventional straight interface and improve 165% ~ 345% without the soldering joint strength of wild phase.
Accompanying drawing explanation
Fig. 1 is the front view of ZrC conductivity ceramics base mother metal surface-treated in embodiment one;
Fig. 2 be Fig. 1 profile;
Fig. 3 is ZrC conductivity ceramics base mother metal after the brazing of embodiment one conductivity ceramics sill/Nb base material metal joint assembling schematic diagram; Wherein a is corresponding connector Nb mother metal, and b is composite soldering, and c is profile of tooth channel-shaped structure, and d is ZrC conductivity ceramics base mother metal;
Fig. 4 is the conventional straight interface of embodiment one contrast and the soldered fitting assembling schematic diagram without wild phase, and wherein a is corresponding connector Nb mother metal, and b is composite soldering, and d is ZrC conductivity ceramics base mother metal.
Detailed description of the invention
Detailed description of the invention one: a kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength of present embodiment is carried out according to the following steps:
One, conductivity ceramics base mother metal joint face surface treatment:
A, the precision WEDM machine technology junction that conductivity ceramics base mother metal and corresponding connector is connected is utilized to be processed into arc surface, if wherein the thermal coefficient of expansion of conductivity ceramics base mother metal is less than the thermal coefficient of expansion of corresponding connector, then conductivity ceramics base mother metal surface is convex surface, the surface of corresponding connector is concave surface, and radian is equal; If the thermal coefficient of expansion of conductivity ceramics base mother metal is greater than the thermal coefficient of expansion of corresponding connector, then conductivity ceramics base mother metal surface is concave surface, and corresponding connector is convex surface, and radian is equal;
B, by Linear cut, the conductivity ceramics base mother metal joint face after step a process is processed into profile of tooth channel-shaped structure, wherein groove depth is 0.3 ~ 3mm, groove width is 0.3 ~ 3mm, and the spacing of two grooves is 0.3 ~ 2mm, and the angle of groove depth direction and to be connected tangential direction is 90 ~ 150 °;
C, by the corresponding connector polishing cleaning after the conductivity ceramics base mother metal after step b surface treatment and step a surface treatment, then clean with acetone and dry, obtaining the conductivity ceramics base mother metal after cleaning and corresponding connector;
Two, solder is prepared: composite soldering comprises B source and containing Ti eutectic alloy system, wherein the mol ratio of Ti element and B element is (10 ~ 1): 1; B source is B, TiB
2, ZrB
2, HfB
2, HfB, BN and B
4any one or a few in C, by arbitrarily than the mixture of composition, is Ti-Ni, Ti-Cu, Ag-Cu-Ti or Ti-Si containing Ti eutectic alloy; If contain B source in conductivity ceramics base mother metal or corresponding connector, then do not add B source or reduce B source addition; In the soldered fitting of end-product, the volume content of TiB whisker is not less than 5%;
Three, solder is placed
Composite soldering step 2 prepared, terpinol become lotion with ethyl cellulose uniform stirring, obtain composite soldering cream, wherein the mass ratio of composite soldering, terpinol and ethyl cellulose is 10:(0.2 ~ 2): (0.4 ~ 3), composite soldering cream is coated on step one clean after conductivity ceramics base mother metal and the joint face of corresponding connector between, obtain assembly to be welded; Maybe the composite soldering cream of preparation is placed between corresponding connector by getting rid of band or being squeezed into paper tinsel, obtains assembly to be welded;
Four, vacuum brazing connects
Assembly to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to 5 × 10
-4~ 1 × 10
-3pa, is then warming up to temperature T by vacuum brazing furnace with the speed of 15 DEG C/min
1, and be incubated 5min ~ 10min, then be warming up to brazing temperature T with the speed of 10 DEG C/min
2, and be incubated 10min ~ 20min, be then cooled to 400 DEG C with the speed of 5 ~ 10 DEG C/min, finally with stove cooling, namely complete the brazing of conductivity ceramics sill; Wherein T
1=T
2-(100 DEG C ~ 200 DEG C), T
2higher than solder liquidus temperature 10% ~ 30%.
Preparation method's tool described in present embodiment has the following advantages:
(1) conductive characteristic making full use of conductivity ceramics sill in macro-scale introduces precision WEDM machine technology carries out the surface texture of various ways Secondary Design processing to its joint face, the stress that effectively can slow down the nearly ceramic side of ceramic/metal linkage interface is concentrated, and this technique is simple to operation, cost is low;
(2) micro-scale can simultaneously in-situ preparation TiB whisker near soldering interface and in solder layer, has following effect simultaneously:
A. the secondary operations of carrying out interface at microcosmic level is carried out to linkage interface, be distributed near interface TiB whisker can micro-scale add interface connection area and effectively slow down the nearly ceramic side of ceramic/metal linkage interface stress concentrate, can also reverse residual stress travel direction;
B. carry out modification to solder layer material, solder layer becomes Metal Substrate TiB whisker reinforced composite material from original simple metal material, effectively reduces solder layer thermal coefficient of expansion, reduces residual stress;
C. generated in-situ TiB whisker can the direction of effective twisting joint residual stress, reduces the probability that crackle occurs.
(3) by the synergy of macro-scale and micro-scale, alleviate joint stress to the full extent, improve the strength reliability of joint.The anti-compression shear strength of the conductivity ceramics sill soldered fitting that this method obtains is 155 ~ 265MPa, than adopting conventional straight interface and improve 165% ~ 345% without the soldering joint strength of wild phase.
Detailed description of the invention two: present embodiment and detailed description of the invention one unlike: described corresponding connector is metal or conductivity ceramics base mother metal.Other is identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment and detailed description of the invention one or two unlike: described conductivity ceramics base mother metal refers to the ceramic based material with conductive characteristic that will be connected with self or metal_based material.Other is identical with detailed description of the invention one or two.In present embodiment, conductivity ceramics base mother metal is boride-based ceramics, carbide base pottery, the oxide-based ceramic of conduction or the nitride based pottery of conduction.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three unlike: described metal is titanium alloy, niobium alloy or molybdenum alloy.Other is identical with one of detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four unlike: in the profile of tooth channel-shaped structure described in step one, any two grooves are parallel to each other or interlaced.Other is identical with one of detailed description of the invention one to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to five unlike: the form of described composite soldering is powdery, foil-like or sheet.Other is identical with one of detailed description of the invention one to five.
Detailed description of the invention seven: present embodiment and one of detailed description of the invention one to six unlike: the B source in the composite soldering described in step 2 is incorporated in active eutectic solder in the mode that powder ball milling mixes, or be incorporated in active eutectic solder by the mode of repeatedly melting, or be incorporated on the outer surface of active eutectic solder by plating, magnetron sputtering or electronics evaporation.Other is identical with one of detailed description of the invention one to six.
Detailed description of the invention eight: a kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength of present embodiment is carried out according to the following steps:
One, conductivity ceramics base mother metal joint face surface treatment:
By Linear cut, conductivity ceramics base mother metal joint face is processed into profile of tooth channel-shaped structure, obtain surface-treated conductivity ceramics base mother metal, wherein groove depth is 0.3 ~ 3mm, groove width is 0.3 ~ 3mm, the spacing of two grooves is 0.3 ~ 2mm, and the angle of groove depth direction and to be connected tangential direction is 90 ~ 150 °; By corresponding connector and surface-treated conductivity ceramics base mother metal polishing cleaning, then clean with acetone and dry, obtaining the conductivity ceramics base mother metal after cleaning and corresponding connector;
Two, solder is prepared: composite soldering comprises B source and containing Ti eutectic alloy system, wherein the mol ratio of Ti element and B element is (10 ~ 1): 1; B source is B, TiB
2, ZrB
2, HfB
2, HfB, BN and B
4any one or a few in C, by arbitrarily than the mixture of composition, is Ti-Ni, Ti-Cu, Ag-Cu-Ti or Ti-Si containing Ti eutectic alloy; If contain B source in conductivity ceramics base mother metal or corresponding connector, then do not add B source or reduce B source addition; In the soldered fitting of end-product, the volume content of TiB whisker is not less than 5%;
Three, solder is placed
Composite soldering step 2 prepared, terpinol become lotion with ethyl cellulose uniform stirring, obtain composite soldering cream, wherein the mass ratio of composite soldering, terpinol and ethyl cellulose is 10:(0.2 ~ 2): (0.4 ~ 3), composite soldering cream is coated on step one clean after conductivity ceramics base mother metal and the joint face of corresponding connector between, obtain assembly to be welded; Maybe the composite soldering cream of preparation is placed between corresponding connector by getting rid of band or being squeezed into paper tinsel, obtains assembly to be welded;
Four, vacuum brazing connects
Assembly to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to 5 × 10
-4~ 1 × 10
-3pa, is then warming up to temperature T by vacuum brazing furnace with the speed of 15 DEG C/min
1, and be incubated 5min ~ 10min, then be warming up to brazing temperature T with the speed of 10 DEG C/min
2, and be incubated 10min ~ 20min, be then cooled to 400 DEG C with the speed of 5 ~ 10 DEG C/min, finally with stove cooling, namely complete the brazing of conductivity ceramics sill; Wherein T
1=T
2-(100 DEG C ~ 200 DEG C), T
2higher than solder liquidus temperature 10% ~ 30%; Wherein said conductivity ceramics base mother metal is equal with the thermal coefficient of expansion of corresponding connector.
Detailed description of the invention nine: present embodiment and detailed description of the invention eight unlike: described corresponding connector is metal or conductivity ceramics base mother metal.Other is identical with detailed description of the invention eight.
Detailed description of the invention ten: present embodiment and detailed description of the invention eight or nine unlike: described conductivity ceramics base mother metal refers to the ceramic based material with conductive characteristic that will be connected with self or metal_based material.Other is identical with detailed description of the invention eight or nine.In present embodiment, conductivity ceramics base mother metal is boride-based ceramics, carbide base pottery, the oxide-based ceramic of conduction or the nitride based pottery of conduction.
Detailed description of the invention 11: one of present embodiment and detailed description of the invention eight to ten unlike: described metal is titanium alloy, niobium alloy or molybdenum alloy.Other is identical with one of detailed description of the invention eight to ten.
Detailed description of the invention 12: one of present embodiment and detailed description of the invention eight to ten one unlike: in the profile of tooth channel-shaped structure described in step one, any two grooves are parallel to each other or interlaced.Other is identical with one of detailed description of the invention eight to ten one.
Detailed description of the invention 13: present embodiment and detailed description of the invention eight to ten two unlike: the form of described composite soldering is powdery, foil-like or sheet.Other is identical with detailed description of the invention eight to ten two.
Detailed description of the invention 14: present embodiment and detailed description of the invention eight to ten three unlike: the B source in the composite soldering described in step 2 is incorporated in active eutectic solder in the mode that powder ball milling mixes, or be incorporated in active eutectic solder by the mode of repeatedly melting, or be incorporated on the outer surface of active eutectic solder by plating, magnetron sputtering or electronics evaporation.Other is identical with detailed description of the invention eight to ten three.
The following examples will be further described the present invention, but not thereby limiting the invention.
Embodiment 1: a kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength of the present embodiment is carried out according to the following steps:
One, conductivity ceramics base mother metal joint face surface treatment:
A, the precision WEDM machine technology junction that ZrC conductivity ceramics base mother metal and corresponding connector Nb mother metal is connected is utilized to be processed into arc surface, wherein ZrC mother metal surface is convex surface, the surface of corresponding connector Nb mother metal is concave surface, and the equal arc radius of radian is 20mm;
B, by Linear cut, the ZrC conductivity ceramics base mother metal joint face after step a process is processed into profile of tooth channel-shaped structure, wherein groove depth is 1.5mm, groove width is 0.4mm, and the spacing of two grooves is 0.8mm, and the angle of groove depth direction and to be connected tangential direction is 90 °;
C, by the corresponding connector Nb mother metal polishing cleaning after the ZrC conductivity ceramics base mother metal after step b surface treatment and step a surface treatment, then clean with acetone and dry, obtaining the conductivity ceramics base mother metal after cleaning and corresponding connector;
Two, solder is prepared: composite soldering comprises TiB
2with Ag-Cu-Ti eutectic alloy system, concrete compound method is: take Ag, Cu, TiB respectively
2, TiH
2powder, its mass percent is respectively: 67%, 24%, 1.5%, 7.5%, uses ball mill fully to mix in various solder powder, obtains composite soldering;
Three, solder is placed
Composite soldering step 2 prepared, terpinol become lotion with ethyl cellulose uniform stirring, obtain composite soldering cream, wherein the mass ratio of composite soldering, terpinol and ethyl cellulose is 10:0.35:1, composite soldering cream is coated on step one clean after conductivity ceramics base mother metal and the joint face of corresponding connector between, coating thickness is 200 μm, obtains assembly to be welded;
Four, vacuum brazing connects
Assembly to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to 5 × 10
-4pa, then vacuum brazing furnace is warming up to temperature 750 DEG C with the speed of 15 DEG C/min, and be incubated 10min, brazing temperature 900 DEG C is warming up to again with the speed of 10 DEG C/min, and be incubated 20min, then be cooled to 400 DEG C with the speed of 5 DEG C/min, finally with stove cooling, namely complete the brazing of conductivity ceramics sill.
Wherein as shown in Figure 1, profile as shown in Figure 2 for the front view of the ceramic base ZrC mother metal that step one is surface-treated.
ZrC conductivity ceramics base mother metal after the brazing of the present embodiment conductivity ceramics sill/Nb base material metal joint assembling schematic diagram as shown in Figure 3.
Conventional straight interface as a comparison and the soldering processes without wild phase as follows:
One, by after ZrC conductivity ceramics base mother metal and Nb mother metal straight joint face polishing cleaning, thoroughly clean with acetone and dry, obtaining the ceramic base mother metal after cleaning and corresponding connector;
Two, Ag, Cu, TiH is taken respectively
2powder, its mass percent is respectively: 69.3%, 26.4%, 4.3%, uses ball mill fully to mix in various solder powder, obtains composite soldering; Composite soldering cream is coated on step one clean after conductivity ceramics base mother metal and the joint face of corresponding connector between, coating thickness is 200 μm, obtains assembly to be welded;
Three, treat that weldment is placed in vacuum drying oven by step 3 gained, then vacuum brazing furnace is warming up to 750 DEG C with the speed of 15 DEG C/min, and be incubated 10min, brazing temperature 900 DEG C is warming up to again with the speed of 10 DEG C/min, and be incubated 20min, then be cooled to 400 DEG C with the speed of 5 DEG C/min, finally with stove cooling, namely complete the brazing of conductivity ceramics sill; Soldered fitting assembling schematic diagram as shown in Figure 4.
Adopt multiple dimensioned joint of combining the method acquisition improving conductivity ceramics sill soldering joint strength, experiment (loading speed is 0.5mm/s) is cut by normal temperature static load pressure, recording shear strength is 221MPa, and conventional straight interface as a comparison and the soldered fitting without wild phase, shear strength under same test condition is only 58MPa, and the soldered fitting shear strength namely adopting the inventive method to obtain improves 283%.
A kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength of embodiment 2, the present embodiment is carried out according to the following steps:
One, conductivity ceramics base mother metal joint face surface treatment:
A, the precision WEDM machine technology junction that conductivity ceramics base ZrC mother metal and corresponding connector Nb mother metal is connected is utilized to be processed into arc surface, wherein ZrC mother metal surface is convex surface, the surface of corresponding connector Nb mother metal is concave surface, and radian is equal, and arc radius is 15mm;
B, by Linear cut, the conductivity ceramics base ZrC mother metal joint face after step a process is processed into profile of tooth channel-shaped structure, wherein groove depth is 1.5mm, groove width is 0.4mm, and the spacing of two grooves is 0.8mm, and the angle of groove depth direction and to be connected tangential direction is 90 °;
C, by the corresponding connector Nb mother metal polishing cleaning after the ZrC conductivity ceramics base mother metal after step b surface treatment and step a surface treatment, then clean with acetone and dry, obtaining the conductivity ceramics base mother metal after cleaning and corresponding connector;
Two, solder is prepared: composite soldering comprises TiB
2with Ag-Cu-Ti eutectic alloy system, concrete compound method is: take Ag, Cu, TiB respectively
2, TiH
2powder, its mass percent is respectively: 64.5%, 20%, 7.2%, 8.3%, uses ball mill fully to mix in various solder powder, obtains composite soldering;
Three, solder is placed
Composite soldering step 2 prepared, terpinol become lotion with ethyl cellulose uniform stirring, obtain composite soldering cream, wherein the mass ratio of composite soldering, terpinol and ethyl cellulose is 10:0.35:1, composite soldering cream is coated on step one clean after conductivity ceramics base mother metal and the joint face of corresponding connector between, coating thickness is 200 μm, obtains assembly to be welded;
Four, vacuum brazing connects
Assembly to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to 5 × 10
-4pa, then vacuum brazing furnace is warming up to temperature 750 DEG C with the speed of 15 DEG C/min, and be incubated 10min, brazing temperature 900 DEG C is warming up to again with the speed of 10 DEG C/min, and be incubated 20min, then be cooled to 400 DEG C with the speed of 5 DEG C/min, finally with stove cooling, namely complete the brazing of conductivity ceramics sill.
Conventional straight interface as a comparison and the soldering processes without wild phase as follows:
One, by after ZrC conductivity ceramics base mother metal and Nb mother metal straight joint face polishing cleaning, thoroughly clean with acetone and dry, obtaining the conductivity ceramics base mother metal after cleaning and corresponding connector;
Two, Ag, Cu, TiH is taken respectively
2powder, its mass percent is respectively: 69.3%, 26.4%, 4.3%, uses ball mill fully to mix in various solder powder, obtains composite soldering; Composite soldering cream is coated on step one clean after conductivity ceramics base mother metal and the joint face of corresponding connector between, coating thickness is 200 μm, obtains assembly to be welded;
Three, treat that weldment is placed in vacuum drying oven by step 3 gained, then vacuum brazing furnace is warming up to 750 DEG C with the speed of 15 DEG C/min, and be incubated 10min, brazing temperature 900 DEG C is warming up to again with the speed of 10 DEG C/min, and be incubated 20min, then be cooled to 400 DEG C with the speed of 5 DEG C/min, finally with stove cooling, namely complete the brazing of conductivity ceramics sill;
Adopt multiple dimensioned joint of combining the method acquisition improving conductivity ceramics sill soldering joint strength, experiment (loading speed is 0.5mm/s) is cut by normal temperature static load pressure, recording shear strength is 258MPa, and conventional straight interface as a comparison and the soldered fitting without wild phase, shear strength under same test condition is only 58MPa, and the soldered fitting shear strength namely adopting the inventive method to obtain improves 345%.
Embodiment 3: a kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength of the present embodiment is carried out according to the following steps:
One, conductivity ceramics base mother metal joint face surface treatment:
By Linear cut, conductivity ceramics base ZrC mother metal joint face is processed into profile of tooth channel-shaped structure, obtain surface-treated conductivity ceramics base mother metal, wherein groove depth is 1.5mm, and groove width is 0.4mm, the spacing of two grooves is 0.8mm, and the angle of groove depth direction and to be connected tangential direction is 90 °; By corresponding connector and surface-treated conductivity ceramics base mother metal polishing cleaning, then clean with acetone and dry, obtaining the conductivity ceramics base mother metal after cleaning and corresponding connector;
Two, solder is prepared: composite soldering comprises TiB
2with Ag-Cu-Ti eutectic alloy system, concrete compound method is: take Ag, Cu, TiB respectively
2, TiH
2powder, its mass percent is respectively: 67%, 24%, 1.5%, 7.5%, uses ball mill fully to mix in various solder powder, obtains composite soldering;
Three, solder is placed
Composite soldering step 2 prepared, terpinol become lotion with ethyl cellulose uniform stirring, obtain composite soldering cream, wherein the mass ratio of composite soldering, terpinol and ethyl cellulose is 10:0.35:1, composite soldering cream is coated on step one clean after conductivity ceramics base mother metal and the joint face of corresponding connector between, coating thickness is 200 μm, obtains assembly to be welded;
Four, vacuum brazing connects
Assembly to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to 5 × 10
-4pa, then vacuum brazing furnace is warming up to temperature 750 DEG C with the speed of 15 DEG C/min, and be incubated 10min, brazing temperature 900 DEG C is warming up to again with the speed of 10 DEG C/min, and be incubated 20min, then be cooled to 400 DEG C with the speed of 5 DEG C/min, finally with stove cooling, namely complete the brazing of conductivity ceramics sill.
Conventional straight interface as a comparison and the soldering processes without wild phase as follows:
One, by after two pieces of ZrC conductivity ceramics base mother metal straight joint face polishing cleanings, thoroughly clean with acetone and dry, obtaining the conductivity ceramics base mother metal after cleaning;
Two, Ag, Cu, TiH is taken respectively
2powder, its mass percent is respectively: 69.3%, 26.4%, 4.3%, uses ball mill fully to mix in various solder powder, obtains composite soldering; Composite soldering cream is coated on step one clean after two pieces of conductivity ceramics base mother metal joint faces between, coating thickness is 200 μm, obtains assembly to be welded;
Three, treat that weldment is placed in vacuum drying oven by step 3 gained, then vacuum brazing furnace is warming up to 750 DEG C with the speed of 15 DEG C/min, and be incubated 10min, brazing temperature 900 DEG C is warming up to again with the speed of 10 DEG C/min, and be incubated 20min, then be cooled to 400 DEG C with the speed of 5 DEG C/min, finally with stove cooling, namely complete the brazing of conductivity ceramics sill;
Adopt multiple dimensioned joint of combining the method acquisition improving conductivity ceramics sill soldering joint strength, experiment (loading speed is 0.5mm/s) is cut by normal temperature static load pressure, recording shear strength is 205MPa, and conventional straight interface as a comparison and the soldered fitting without wild phase, shear strength under same test condition is only 76MPa, and the soldered fitting shear strength namely adopting the inventive method to obtain improves 171%
Known by above embodiment, the present invention, by the synergy of macro-scale and micro-scale, alleviates joint stress to the full extent, improves the strength reliability of joint.The anti-compression shear strength of the conductivity ceramics sill soldered fitting that this method obtains is 165 ~ 265MPa, than adopting conventional straight interface and improve 165% ~ 345% without the soldering joint strength of wild phase.
Claims (10)
1. a multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength, is characterized in that the method is carried out according to the following steps:
One, conductivity ceramics base mother metal joint face surface treatment:
A, the precision WEDM machine technology junction that conductivity ceramics base mother metal and corresponding connector is connected is utilized to be processed into arc surface, if wherein the thermal coefficient of expansion of conductivity ceramics base mother metal is less than the thermal coefficient of expansion of corresponding connector, then conductivity ceramics base mother metal surface is convex surface, the surface of corresponding connector is concave surface, and radian is equal; If the thermal coefficient of expansion of conductivity ceramics base mother metal is greater than the thermal coefficient of expansion of corresponding connector, then conductivity ceramics base mother metal surface is concave surface, and corresponding connector is convex surface, and radian is equal;
B, by Linear cut, the conductivity ceramics base mother metal joint face after step a process is processed into profile of tooth channel-shaped structure, wherein groove depth is 0.3 ~ 3mm, groove width is 0.3 ~ 3mm, and the spacing of two grooves is 0.3 ~ 2mm, and the angle of groove depth direction and to be connected tangential direction is 90 ~ 150 °;
C, by the corresponding connector polishing cleaning after the conductivity ceramics base mother metal after step b surface treatment and step a surface treatment, then clean with acetone and dry, obtaining the conductivity ceramics base mother metal after cleaning and corresponding connector;
Two, solder is prepared: composite soldering comprises B source and containing Ti eutectic alloy system, wherein the mol ratio of Ti element and B element is (10 ~ 1): 1; B source is B, TiB
2, ZrB
2, HfB
2, HfB, BN and B
4any one or a few in C, by arbitrarily than the mixture of composition, is Ti-Ni, Ti-Cu, Ag-Cu-Ti or Ti-Si containing Ti eutectic alloy; If contain B source in conductivity ceramics base mother metal or corresponding connector, then do not add B source or reduce B source addition; In the soldered fitting of end-product, the volume content of TiB whisker is not less than 5%;
Three, solder is placed
Composite soldering step 2 prepared, terpinol become lotion with ethyl cellulose uniform stirring, obtain composite soldering cream, wherein the mass ratio of composite soldering, terpinol and ethyl cellulose is 10:(0.2 ~ 2): (0.4 ~ 3), composite soldering cream is coated on step one clean after conductivity ceramics base mother metal and the joint face of corresponding connector between, obtain assembly to be welded; Maybe the composite soldering cream of preparation is placed between corresponding connector by getting rid of band or being squeezed into paper tinsel, obtains assembly to be welded;
Four, vacuum brazing connects
Assembly to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to 5 × 10
-4~ 1 × 10
-3pa, is then warming up to temperature T by vacuum brazing furnace with the speed of 15 DEG C/min
1, and be incubated 5min ~ 10min, then be warming up to brazing temperature T with the speed of 10 DEG C/min
2, and be incubated 10min ~ 20min, be then cooled to 400 DEG C with the speed of 5 ~ 10 DEG C/min, finally with stove cooling, namely complete the brazing of conductivity ceramics sill; Wherein T
1=T
2-(100 DEG C ~ 200 DEG C), T
2higher than solder liquidus temperature 10% ~ 30%.
2. a kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength according to claim 1, is characterized in that described corresponding connector is metal or conductivity ceramics base mother metal.
3. a kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength according to claim 1 and 2, is characterized in that described conductivity ceramics base mother metal refers to the ceramic based material with conductive characteristic be connected with self or metal_based material.
4. a kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength according to claim 2, is characterized in that described metal is titanium alloy, niobium alloy or molybdenum alloy.
5. a kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength according to claim 1, is characterized in that in the profile of tooth channel-shaped structure described in step one, any two grooves are parallel to each other or interlaced.
6. a kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength according to claim 1, is characterized in that the form of described composite soldering is powdery, foil-like or sheet.
7. a kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength according to claim 1, it is characterized in that the B source in the composite soldering described in step 2 is incorporated in active eutectic solder in the mode that powder ball milling mixes, or be incorporated in active eutectic solder by the mode of repeatedly melting, or be incorporated on the outer surface of active eutectic solder by plating, magnetron sputtering or electronics evaporation.
8. a multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength, is characterized in that the method is carried out according to the following steps:
One, conductivity ceramics base mother metal joint face surface treatment:
Profile of tooth channel-shaped structure is processed at conductivity ceramics base mother metal joint face by Linear cut, obtain surface-treated conductivity ceramics base mother metal, wherein groove depth is 0.3 ~ 3mm, groove width is 0.3 ~ 3mm, the spacing of two grooves is 0.3 ~ 2mm, and the angle of groove depth direction and to be connected tangential direction is 90 ~ 150 °; By corresponding connector and surface-treated conductivity ceramics base mother metal polishing cleaning, then clean with acetone and dry, obtaining the conductivity ceramics base mother metal after cleaning and corresponding connector;
Two, solder is prepared: composite soldering comprises B source and containing Ti eutectic alloy system, wherein the mol ratio of Ti element and B element is (10 ~ 1): 1; B source is B, TiB
2, ZrB
2, HfB
2, HfB, BN and B
4any one or a few in C, by arbitrarily than the mixture of composition, is Ti-Ni, Ti-Cu, Ag-Cu-Ti or Ti-Si containing Ti eutectic alloy; If contain B source in conductivity ceramics base mother metal or corresponding connector, then do not add B source or reduce B source addition; In the soldered fitting of end-product, the volume content of TiB whisker is not less than 5%;
Three, solder is placed
Composite soldering step 2 prepared, terpinol become lotion with ethyl cellulose uniform stirring, obtain composite soldering cream, wherein the mass ratio of composite soldering, terpinol and ethyl cellulose is 10:(0.2 ~ 2): (0.4 ~ 3), composite soldering cream is coated on step one clean after conductivity ceramics base mother metal and the joint face of corresponding connector between, obtain assembly to be welded; Maybe the composite soldering cream of preparation is placed between corresponding connector by getting rid of band or being squeezed into paper tinsel, obtains assembly to be welded;
Four, vacuum brazing connects
Assembly to be welded is placed in vacuum drying oven, vacuum brazing furnace is evacuated to 5 × 10
-4~ 1 × 10
-3pa, is then warming up to temperature T by vacuum brazing furnace with the speed of 15 DEG C/min
1, and be incubated 5min ~ 10min, then be warming up to brazing temperature T with the speed of 10 DEG C/min
2, and be incubated 10min ~ 20min, be then cooled to 400 DEG C with the speed of 5 ~ 10 DEG C/min, finally with stove cooling, namely complete the brazing of conductivity ceramics sill; Wherein T
1=T
2-(100 DEG C ~ 200 DEG C), T
2higher than solder liquidus temperature 10% ~ 30%; Wherein said conductivity ceramics base mother metal is equal with the thermal coefficient of expansion of corresponding connector.
9. a kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength according to claim 8, is characterized in that described corresponding connector is metal or conductivity ceramics base mother metal; Wherein conductivity ceramics base mother metal refers to the ceramic based material with conductive characteristic be connected with self or metal_based material.
10. a kind of multiple dimensioned method of combining raising conductivity ceramics sill soldering joint strength according to claim 9, is characterized in that described metal is titanium alloy, niobium alloy or molybdenum alloy.
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