CN107649758A - A kind of method that soldering is carried out to porous silicon nitride ceramic and invar alloy using composite soldering - Google Patents
A kind of method that soldering is carried out to porous silicon nitride ceramic and invar alloy using composite soldering Download PDFInfo
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- CN107649758A CN107649758A CN201710910239.6A CN201710910239A CN107649758A CN 107649758 A CN107649758 A CN 107649758A CN 201710910239 A CN201710910239 A CN 201710910239A CN 107649758 A CN107649758 A CN 107649758A
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- soldering
- welded
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- invar
- silicon nitride
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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
- B23K1/20—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
- 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
- B23K1/203—Fluxing, i.e. applying flux onto surfaces
-
- 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
- B23K1/206—Cleaning
-
- 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
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/18—Dissimilar materials
Abstract
A kind of method for carrying out soldering to porous silicon nitride ceramic and invar alloy using composite soldering, it is related to a kind of method for welding of porous silicon nitride ceramic and invar alloy.The invention aims to solve existing Si3N4Ceramics easily produce stress concentration, the problem of causing bonding strength difference in soldering cooling procedure with Invar in interface.Method for welding：First, polish；2nd, clean；3rd, from top to bottom according to porous Si3N4The order of ceramics, Ag Cu Ti+Mo paste solders, clean Cu paillon foils, Ag Cu paste solders and Invar is overlapped；4th, vacuum brazing, that is, the soldering of porous silicon nitride ceramic and invar alloy is completed.Advantage：Joint bonding strength reaches more than 65MPa, and highest bonding strength reaches 81MPa.Present invention is mainly used for porous silicon nitride ceramic and invar alloy to carry out soldering.
Description
Technical field
The present invention relates to a kind of porous silicon nitride ceramic and the method for welding of invar alloy.
Background technology
Porous Si3N4Ceramics have equally distributed micropore, and volume density is small, porosity is high, high-specific surface area and special
Physical surface properties.With good dielectric properties, absorb damping etc. characteristic thus can apply to aerospace field, and
It is the ideal material for preparing missile-borne radome.Porous ceramics has certain fragility in itself, and is difficult to deform, therefore can not pass through
The mode of mechanical connection is assembled antenna house and body.And then employ the less Invar of thermal coefficient of expansion at room temperature and close
Gold is used as antenna house connection ring, again by connection ring and body after first antenna house is connected by way of soldering with metal connection ring
Connection is assembled so as to realize.The difficult point of ceramics and solder bonding metal essentially consists in the difference of physics and chemical property.Porous Si3N4
Larger thermal coefficient of expansion gap be present between ceramics and Invar alloys.Although have under Invar Alloy At Room Temperatures relatively low hot swollen
Swollen coefficient, but its thermal coefficient of expansion is rapid as temperature raises to be risen, therefore easily in interface in soldering cooling procedure
Stress concentration is produced, causes bonding strength poor (general bonding strength is less than 52MPa), therefore the residual stress in brazing process
Alleviation is to improve the key of joint performance.
The content of the invention
The invention aims to solve existing Si3N4Ceramics easily produce with Invar in soldering cooling procedure in interface
Raw stress concentration, the problem of causing bonding strength difference, and provide it is a kind of using composite soldering to porous silicon nitride ceramic and invar
The method that alloy carries out soldering.
A kind of method that soldering is carried out to porous silicon nitride ceramic and invar alloy using composite soldering, specifically by following
What step was completed：
First, polish：By porous Si3N4The surface to be welded of ceramics is successively with 200# abrasive paper for metallograph, 400# abrasive paper for metallograph, 600# gold
Phase sand paper and 800# abrasive paper for metallograph are polished, and obtain porous Si after surface to be welded polishing3N4Ceramics；By Invar surface to be welded successively
Polished with 400# abrasive paper for metallograph, 600# abrasive paper for metallograph and 1000# abrasive paper for metallograph, obtain Invar after surface to be welded polishing；By Cu
Paillon foil is polished with 400# abrasive paper for metallograph, 600# abrasive paper for metallograph and 1000# abrasive paper for metallograph successively, is polishing to thickness as 140 μm
~150 μm, Cu paillon foils after being polished；
2nd, clean：Porous Si after surface to be welded is polished3N4Ceramics are put into alcohol and cleaned, and are obtained after drying to be welded porous
Si3N4Ceramics；Invar immerses in acetone and is cleaned by ultrasonic after surface to be welded is polished, and is rinsed after taking-up with absolute ethyl alcohol, and blow
It is dry, obtain Invar to be welded；Cu paillon foils after polishing are immersed in acetone and are cleaned by ultrasonic, are rinsed after taking-up with absolute ethyl alcohol, and
Drying, obtains clean Cu paillon foils；
3rd, Ag-Cu-Ti+Mo paste solders are coated in porous Si to be welded3N4On the surface to be welded of ceramics, by Ag-Cu pastes
On surface to be welded of the solder coated in Invar to be welded, then from top to bottom according to porous Si3N4Ceramics, Ag-Cu-Ti+Mo paste prickers
The order of material, clean Cu paillon foils, Ag-Cu paste solders and Invar is overlapped, and obtains sample to be welded；
4th, vacuum brazing：By sample to be welded with porous Si3N4Ceramics are placed in graphite jig in upper form, and to be welded
The porous Si of sample3N4Ceramic upper surface carries out physics pressure, and pressure is 1 × 104Pa~1.5 × 104Pa, it is then transferred to true
In empty soldering oven, vacuum in vacuum brazing furnace is first adjusted to 1 × 10-3Pa~6 × 10-3Pa, then heats to 300 DEG C, and
Temperature is 300 DEG C, physical pressure is 1 × 104Pa~1.5 × 104Pa and vacuum are 1 × 10-3Pa~6 × 10-3It is incubated under Pa
20min, then brazing temperature is warming up to, and be 1 × 10 in physical pressure4Pa~1.5 × 104Pa, vacuum are 1 × 10-3Pa~6
×10-3Pa and brazing temperature complete soldering, and 300 DEG C are cooled to after the completion of soldering, then cools to room temperature with the furnace, that is, is completed porous
The soldering of silicon nitride ceramics and invar alloy.
Advantage of the present invention：First, Invar alloys side is diffused to by Ti in brazing process and interacted with it, most
Throughout one's life into harmful phase.Therefore the present invention introduces Cu intermediate layers to obstruct diffusion of the Ti elements to Invar sides in solder, so as to
Realize the purpose for suppressing intermetallic compound.2nd, the residual thermal stress inside weld seam is by thermal expansion system between ceramics and solder
Caused by number mismatches.The further residual thermal stress reduced inside weld seam is, it is necessary to consider to reduce the thermal expansion of solder part
Coefficient.Mo has relatively low thermal coefficient of expansion in itself, and chemical property itself is stable, will not occur with Ag-Cu-Ti solders anti-
It should be impacted so as to butt joint tissue.Therefore the present invention adds Mo as reinforcement material in the solder close to ceramic side
To reduce the thermal coefficient of expansion of the side, the composite soldering finally obtained is Ag-Cu-Ti+Mo/Cu/Ag-Cu.3rd, the present invention is utilized
Method reaches more than 65MPa to carrying out soldering, joint bonding strength to porous silicon nitride ceramic and invar alloy, and highest connection is strong
Degree reaches 81MPa.
Brief description of the drawings
Fig. 1 is the porous silicon nitride ceramic and invar alloy compression shear performance test part joint microscopic structure that embodiment 1 obtains
Photo；
Fig. 2 is porous silicon nitride ceramic of the present invention and invar alloy weldment schematic diagram；1 represents nitride porous in figure
Silicon is ceramic, 2 expression invar alloy in figure, 3 expression Ag-Cu-Ti+Mo solder layers in figure, 4 expression Cu layers in figure, and 5 represent in figure
Ag-Cu solder layers；
Fig. 3 is the porous silicon nitride ceramic and invar alloy compression shear performance test part schematic diagram that embodiment 1 obtains；1 in figure
Porous silicon nitride ceramic is represented, 2 represent invar alloy in figure, and 3 represent Ag-Cu-Ti+Mo solder layers in figure, and 4 represent Cu in figure
Layer, 5 represent Ag-Cu solder layers in figure；
Fig. 4 is the porous silicon nitride ceramic and invar alloy compression shear performance test part shear strength test that embodiment 1 obtains
Schematic diagram；1 represents porous silicon nitride ceramic in figure, and 2 represent invar alloy in figure, and 3 represent Ag-Cu-Ti+Mo solder layers in figure,
4 represent Cu layers in figure, and 5 represent Ag-Cu solder layers in figure, and 6 represent shear strength test cushion blocks in figure, in figure ↓ represent active force
Direction.
Embodiment
Embodiment one：Present embodiment is that one kind utilizes composite soldering to porous silicon nitride ceramic and invar alloy
The method for carrying out soldering, it is characterised in that it is completed according to the following steps：
First, polish：By porous Si3N4The surface to be welded of ceramics is successively with 200# abrasive paper for metallograph, 400# abrasive paper for metallograph, 600# gold
Phase sand paper and 800# abrasive paper for metallograph are polished, and obtain porous Si after surface to be welded polishing3N4Ceramics；By Invar surface to be welded successively
Polished with 400# abrasive paper for metallograph, 600# abrasive paper for metallograph and 1000# abrasive paper for metallograph, obtain Invar after surface to be welded polishing；By Cu
Paillon foil is polished with 400# abrasive paper for metallograph, 600# abrasive paper for metallograph and 1000# abrasive paper for metallograph successively, is polishing to thickness as 140 μm
~150 μm, Cu paillon foils after being polished；
2nd, clean：Porous Si after surface to be welded is polished3N4Ceramics are put into alcohol and cleaned, and are obtained after drying to be welded porous
Si3N4Ceramics；Invar immerses in acetone and is cleaned by ultrasonic after surface to be welded is polished, and is rinsed after taking-up with absolute ethyl alcohol, and blow
It is dry, obtain Invar to be welded；Cu paillon foils after polishing are immersed in acetone and are cleaned by ultrasonic, are rinsed after taking-up with absolute ethyl alcohol, and
Drying, obtains clean Cu paillon foils；
3rd, Ag-Cu-Ti+Mo paste solders are coated in porous Si to be welded3N4On the surface to be welded of ceramics, by Ag-Cu pastes
On surface to be welded of the solder coated in Invar to be welded, then from top to bottom according to porous Si3N4Ceramics, Ag-Cu-Ti+Mo paste prickers
The order of material, clean Cu paillon foils, Ag-Cu paste solders and Invar is overlapped, and obtains sample to be welded；
4th, vacuum brazing：By sample to be welded with porous Si3N4Ceramics are placed in graphite jig in upper form, and to be welded
The porous Si of sample3N4Ceramic upper surface carries out physics pressure, and pressure is 1 × 104Pa~1.5 × 104Pa, it is then transferred to true
In empty soldering oven, vacuum in vacuum brazing furnace is first adjusted to 1 × 10-3Pa~6 × 10-3Pa, then heats to 300 DEG C, and
Temperature is 300 DEG C, physical pressure is 1 × 104Pa~1.5 × 104Pa and vacuum are 1 × 10-3Pa~6 × 10-3It is incubated under Pa
20min, then brazing temperature is warming up to, and be 1 × 10 in physical pressure4Pa~1.5 × 104Pa, vacuum are 1 × 10-3Pa~6
×10-3Pa and brazing temperature complete soldering, and 300 DEG C are cooled to after the completion of soldering, then cools to room temperature with the furnace, that is, is completed porous
The soldering of silicon nitride ceramics and invar alloy.
Invar alloys side is diffused to by Ti in brazing process and is interacted with it, ultimately generates harmful phase.Cause
This present embodiment introduces Cu intermediate layers to obstruct diffusion of the Ti elements to Invar sides in solder, suppresses gold so as to realize
The purpose of compound between category.
Residual thermal stress inside weld seam is as caused by mismatching thermal coefficient of expansion between ceramics and solder.Further
The residual thermal stress inside weld seam is reduced, it is necessary to consider to reduce the thermal coefficient of expansion of solder part.Mo has relatively low heat in itself
The coefficient of expansion, and chemical property itself is stable, will not be reacted with Ag-Cu-Ti solders so as to which butt joint tissue causes shadow
Ring.Therefore present embodiment adds Mo as reinforcement material to reduce the thermal expansion of the side in the solder close to ceramic side
Coefficient, the composite soldering finally obtained are Ag-Cu-Ti+Mo/Cu/Ag-Cu.
Using present embodiment method to carrying out soldering to porous silicon nitride ceramic and invar alloy, joint bonding strength reaches
To more than 65MPa, highest bonding strength reaches 81MPa.
Embodiment two：The difference of present embodiment and embodiment one is：It is porous described in step 1
Si3N4The porosity of ceramics is 45%~55%.Other are identical with embodiment one.
It is porous ceramics that present embodiment, which essentially consists in experiment mother metal,.Traditional ceramic of compact is higher strong mainly by it
Degree etc. is applied on structural member；And porous Si3N4Ceramics mainly take a fancy to the dielectric properties of itself and are applied to missile-borne radome, belong to
In functional material.For fine and close Si3N4Ceramic brazing research at present a lot, but porous Si3N4The soldering of ceramics is gone back at present
The porous Si used in blank stage, this experiment3N4The porosity of ceramics is 45%~55%, and brazing process center tap relates to
And to solder to porous ceramics inside penetrate into phenomena such as, therefore microstructure, the shadow of mechanical property and solder composition butt joint
Ring with ceramic of compact difference.And compared to ceramic of compact, the influence of residual stress butt joint is more obvious, this
It is the reason for present embodiment adds Mo reinforcements.
Embodiment three：Present embodiment is with one of embodiment one or two difference：Institute in step 3
The Ag-Cu-Ti+Mo paste solders stated are to prepare according to the following steps：
1., prepare raw material：According to chemical formula (Ag72Cu28)0.85Ti0.1Mo0.05Or (Ag72Cu28)0.8Ti0.1Mo0.1Prepare
Ag-Cu eutectic powders, Ti powder and granularity are 20 μm of Mo powder, and the chemical formula of the Ag-Cu eutectic powders is Ag72Cu28：2., ball
Mill mixing：The Mo powder that the Ag-Cu eutectic powders, Ti powder and granularity of step steady are 20 μm is subjected to ball milling mixing, ball milling turns
Speed is 200r/min, ratio of grinding media to material 5:1, Ball-milling Time 2h, obtain composite soldering powder；3., cream processed：Add into composite soldering powder
Enter binding agent, Ag-Cu-Ti+Mo paste solders are obtained after mixing；The binding agent is hydroxyethyl cellulose；The composite soldering
The quality of powder and the volume ratio of binding agent are 20mg:0.05mL.
Other are identical with embodiment one or two.
Embodiment four：Present embodiment is with one of embodiment one to three difference：Will in step 3
Ag-Cu-Ti+Mo paste solders are coated in porous Si to be welded3N4On the surface to be welded of ceramics, coating thickness is 100 μm~150 μm.Its
He is identical with embodiment one to three.
Embodiment five：Present embodiment is with one of embodiment one to four difference：Institute in step 3
The Ag-Cu paste solders stated are to prepare according to the following steps：Binding agent is added into Ag-Cu eutectic powders, Ag-Cu is obtained after mixing
Paste solder；The chemical formula of the Ag-Cu eutectic powders is Ag72Cu28；The binding agent is hydroxyethyl cellulose；The Ag-
The quality of Cu eutectic powders and the volume ratio of binding agent are 20mg:0.05mL.Other are identical with embodiment one to four.
Embodiment six：Present embodiment is with one of embodiment one to five difference：Will in step 3
On surface to be welded of the Ag-Cu paste solders coated in Invar to be welded, coating thickness is 100 μm~150 μm.Other and specific implementation
Mode one to five is identical.
Embodiment seven：Present embodiment is with one of embodiment one to six difference：Will in step 2
Invar, which is immersed in acetone, after surface to be welded polishing is cleaned by ultrasonic, and is cleaned by ultrasonic 15min.Other with embodiment one to
Six is identical.
Embodiment eight：Present embodiment is with one of embodiment one to seven difference：Will in step 2
Cu paillon foils immerse in acetone and are cleaned by ultrasonic after polishing, are cleaned by ultrasonic 10min.Other and the phase of embodiment one to seven
Together.
Embodiment nine：Present embodiment is with one of embodiment one to eight difference：In step 4 first
Vacuum in vacuum brazing furnace is adjusted to 6 × 10-3Pa, it is 6 × 10 in vacuum-3Using the rate of heat addition as 10 DEG C/min liters under Pa
Temperature to 300 DEG C, and temperature be 300 DEG C, physical pressure be 1 × 104Pa and vacuum are 6 × 10-320min is incubated under Pa, then
900 DEG C are warming up to 10 DEG C/min programming rate, and is 1 × 10 in physical pressure4Pa, vacuum are 6 × 10-3Pa and temperature
To carry out soldering at 900 DEG C, holding time 20min, 300 DEG C are cooled to 5 DEG C/min cooling velocity after the completion of soldering, so
After cool to room temperature with the furnace, that is, complete the soldering of porous silicon nitride ceramic and invar alloy.Other with embodiment one to
Eight is identical.
Embodiment ten：Present embodiment is with one of embodiment one to nine difference：In step 4
The porous Si of sample to be welded3N4It is as follows that ceramic upper surface carries out physics pressure detailed process：In the porous Si of sample to be welded3N4Pottery
Place one block of Mo alloy, the porous Si using Mo alloys to sample to be welded in porcelain upper surface3N4Ceramic upper surface carries out physics pressure,
Pressure is 1 × 104Pa.Other are identical with embodiment one to nine.
Present invention is not limited only to the content of the respective embodiments described above, the group of one of them or several embodiments
Contract sample can also realize the purpose of invention.
Using following verification experimental verifications effect of the present invention
Embodiment 1：A kind of method that soldering is carried out to porous silicon nitride ceramic and invar alloy using composite soldering, specifically
Complete according to the following steps：
First, polish：By porous Si3N4The surface to be welded of ceramics is successively with 200# abrasive paper for metallograph, 400# abrasive paper for metallograph, 600# gold
Phase sand paper and 800# abrasive paper for metallograph are polished, and obtain porous Si after surface to be welded polishing3N4Ceramics；By Invar surface to be welded successively
Polished with 400# abrasive paper for metallograph, 600# abrasive paper for metallograph and 1000# abrasive paper for metallograph, obtain Invar after surface to be welded polishing；By Cu
Paillon foil is polished with 400# abrasive paper for metallograph, 600# abrasive paper for metallograph and 1000# abrasive paper for metallograph successively, is polishing to thickness as 145 μm,
Cu paillon foils after being polished；Porous Si described in step 13N4The porosity of ceramics is 50%；
2nd, clean：Porous Si after surface to be welded is polished3N4Ceramics are put into alcohol and cleaned, and are obtained after drying to be welded porous
Si3N4Ceramics；Invar immerses in acetone and is cleaned by ultrasonic after surface to be welded is polished, and is cleaned by ultrasonic 15min, with anhydrous after taking-up
Alcohol flushing, and dry up, obtain Invar to be welded；Cu paillon foils after polishing are immersed in acetone and are cleaned by ultrasonic, are cleaned by ultrasonic
10min, rinsed, and dried up with absolute ethyl alcohol after taking-up, obtain clean Cu paillon foils；
3rd, Ag-Cu-Ti+Mo paste solders are coated in porous Si to be welded using coating thickness as 100 μm3N4Ceramic is to be welded
On face, coating thickness be 100 μm by Ag-Cu paste solders coated in Invar to be welded surface to be welded on, then from top to bottom according to
Porous Si3N4Ceramics, Ag-Cu-Ti+Mo paste solders, clean Cu paillon foils, Ag-Cu paste solders and Invar order are folded
Add, obtain sample to be welded；
4th, vacuum brazing：By sample to be welded with porous Si3N4Ceramics are placed in graphite jig in upper form, and to be welded
The porous Si of sample3N4Place one block of Mo alloy, the porous Si using Mo alloys to sample to be welded in ceramic upper surface3N4On ceramics
Surface carries out physics pressure, and pressure is 1 × 104Pa, it is then transferred in vacuum brazing furnace, first by vacuum in vacuum brazing furnace
It is adjusted to 6 × 10-3Pa, it is 6 × 10 in vacuum-3300 DEG C are warming up to by 10 DEG C/min of the rate of heat addition under Pa, and is in temperature
300 DEG C, physical pressure be 1 × 104Pa and vacuum are 6 × 10-320min, then the programming rate with 10 DEG C/min are incubated under Pa
900 DEG C are warming up to, and is 1 × 10 in physical pressure4Pa, vacuum are 6 × 10-3Pa and temperature are to carry out soldering, pricker at 900 DEG C
The weldering time is 20min, and 300 DEG C are cooled to 5 DEG C/min cooling velocity after the completion of soldering, then cools to room temperature with the furnace, i.e.,
The soldering of porous silicon nitride ceramic and invar alloy is completed, obtains porous silicon nitride ceramic and invar alloy compression shear performance test
Part.
Ag-Cu-Ti+Mo paste solders described in the present embodiment step 3 are to prepare according to the following steps：
1., prepare raw material：According to chemical formula (Ag72Cu28)0.85Ti0.1Mo0.05Prepare Ag-Cu eutectic powders, Ti powder and grain
The Mo powder for 20 μm is spent, the chemical formula of the Ag-Cu eutectic powders is Ag72Cu28：2., ball milling mixing：By step steady
The Mo powder that Ag-Cu eutectic powders, Ti powder and granularity are 20 μm carries out ball milling mixing, rotational speed of ball-mill 200r/min, and ratio of grinding media to material is
5:1, Ball-milling Time 2h, obtain composite soldering powder；3., cream processed：Binding agent is added into composite soldering powder, is obtained after mixing
Ag-Cu-Ti+Mo paste solders；The binding agent is hydroxyethyl cellulose；The quality of the composite soldering powder and the body of binding agent
Product ratio is 20mg:0.05mL.
Ag-Cu paste solders described in the present embodiment step 3 are to prepare according to the following steps：Into Ag-Cu eutectic powders
Binding agent is added, Ag-Cu paste solders are obtained after mixing；The chemical formula of the Ag-Cu eutectic powders is Ag72Cu28；It is described viscous
Knot agent is hydroxyethyl cellulose；The quality of the Ag-Cu eutectic powders and the volume ratio of binding agent are 20mg:0.05mL.
Present invention is mainly used for the connection between missile-borne radome and connection ring, force way is mainly shear stress.Institute
The test equipment used is Instron-5569 type universal testing machine.Pressure head loading speed is used during experiment as 0.5mm/
min.Testing result as shown in figure 1, Fig. 1 is observed that Mo reinforcements are evenly distributed in solder and are well combined with solder,
Having no the defects of obvious in weld seam is present, and Cu intermediate layers keep not finding black bulk in complete continuous state and weld seam
Poisonous metal between compound such as Fe-Ti and Ni-Ti etc. presence.Prove that it is feasible to add Mo reinforcements, while in Cu
Interbed effectively inhibits harmful phase to generate.
Embodiment 2：The present embodiment is with the difference of embodiment 1：Ag-Cu-Ti+Mo paste solders described in step 3 are
Prepare according to the following steps：
1., prepare raw material：According to chemical formula (Ag72Cu28)0.8Ti0.1Mo0.1Prepare Ag-Cu eutectic powders, Ti powder and granularity
For 20 μm of Mo powder, the chemical formula of the Ag-Cu eutectic powders is Ag72Cu28：2., ball milling mixing：By the Ag- of step steady
The Mo powder that Cu eutectic powders, Ti powder and granularity are 20 μm carries out ball milling mixing, rotational speed of ball-mill 200r/min, ratio of grinding media to material 5:1,
Ball-milling Time is 2h, obtains composite soldering powder；3., cream processed：Binding agent is added into composite soldering powder, Ag-Cu- is obtained after mixing
Ti+Mo paste solders；The binding agent is hydroxyethyl cellulose；The quality of the composite soldering powder and the volume ratio of binding agent are
20mg:0.05mL。
Other are same as Example 1.
Embodiment 3：The present embodiment is with the difference of embodiment 1：In step 3 Ag- is replaced using Ag-Cu-Ti paste solders
Cu-Ti+Mo paste solders use, and described Ag-Cu-Ti paste solders are to prepare according to the following steps：
1., prepare raw material：According to chemical formula (Ag72Cu28)0.9Ti0.1Prepare Ag-Cu eutectic powders and Ti powder, the Ag-
The chemical formula of Cu eutectic powders is Ag72Cu28：2., ball milling mixing：The Ag-Cu eutectic powders of step steady and Ti powder are carried out
Ball milling mixing, rotational speed of ball-mill 200r/min, ratio of grinding media to material 5:1, Ball-milling Time 2h, obtain composite soldering powder；3., cream processed：
Binding agent is added into composite soldering powder, Ag-Cu-Ti paste solders are obtained after mixing；The binding agent is hydroxyethyl cellulose；
The quality of the composite soldering powder and the volume ratio of binding agent are 20mg:0.05mL.
Other are same as Example 1.
Embodiment 4：The present embodiment is with the difference of embodiment 1：In step 3 Ag- is replaced using Ag-Cu-Ti paste solders
Cu-Ti+Mo paste solders use, and described Ag-Cu-Ti paste solders are to prepare according to the following steps：
1., prepare raw material：According to chemical formula (Ag72Cu28)0.95Ti0.05Prepare Ag-Cu eutectic powders and Ti powder, the Ag-
The chemical formula of Cu eutectic powders is Ag72Cu28：2., ball milling mixing：The Ag-Cu eutectic powders of step steady and Ti powder are carried out
Ball milling mixing, rotational speed of ball-mill 200r/min, ratio of grinding media to material 5:1, Ball-milling Time 2h, obtain composite soldering powder；3., cream processed：
Binding agent is added into composite soldering powder, Ag-Cu-Ti paste solders are obtained after mixing；The binding agent is hydroxyethyl cellulose；
The quality of the composite soldering powder and the volume ratio of binding agent are 20mg:0.05mL.
Other are same as Example 1.
Embodiment 5：The present embodiment is with the difference of embodiment 1：Ag-Cu-Ti+Mo paste solders described in step 3 are
Prepare according to the following steps：
1., prepare raw material：According to chemical formula (Ag72Cu28)0.9Ti0.05Mo0.05Prepare Ag-Cu eutectic powders, Ti powder and grain
The Mo powder for 20 μm is spent, the chemical formula of the Ag-Cu eutectic powders is Ag72Cu28：2., ball milling mixing：By step steady
The Mo powder that Ag-Cu eutectic powders, Ti powder and granularity are 20 μm carries out ball milling mixing, rotational speed of ball-mill 200r/min, and ratio of grinding media to material is
5:1, Ball-milling Time 2h, obtain composite soldering powder；3., cream processed：Binding agent is added into composite soldering powder, is obtained after mixing
Ag-Cu-Ti+Mo paste solders；The binding agent is hydroxyethyl cellulose；The quality of the composite soldering powder and the body of binding agent
Product ratio is 20mg:0.05mL.
Other are same as Example 1.
Embodiment 6：The present embodiment is with the difference of embodiment 1：Ag-Cu-Ti+Mo paste solders described in step 3 are
Prepare according to the following steps：
1., prepare raw material：According to chemical formula (Ag72Cu28)0.85Ti0.05Mo0.1Prepare Ag-Cu eutectic powders, Ti powder and grain
The Mo powder for 20 μm is spent, the chemical formula of the Ag-Cu eutectic powders is Ag72Cu28：2., ball milling mixing：By step steady
The Mo powder that Ag-Cu eutectic powders, Ti powder and granularity are 20 μm carries out ball milling mixing, rotational speed of ball-mill 200r/min, and ratio of grinding media to material is
5:1, Ball-milling Time 2h, obtain composite soldering powder；3., cream processed：Binding agent is added into composite soldering powder, is obtained after mixing
Ag-Cu-Ti+Mo paste solders；The binding agent is hydroxyethyl cellulose；The quality of the composite soldering powder and the body of binding agent
Product ratio is 20mg:0.05mL.
Other are same as Example 1.
Embodiment 7：The present embodiment is with the difference of embodiment 1：In step 3 Ag- is replaced using Ag-Cu-Ti paste solders
Cu-Ti+Mo paste solders use, and described Ag-Cu-Ti paste solders are to prepare according to the following steps：
1., prepare raw material：According to chemical formula (Ag72Cu28)0.85Ti0.15Prepare Ag-Cu eutectic powders and Ti powder, the Ag-
The chemical formula of Cu eutectic powders is Ag72Cu28：2., ball milling mixing：The Ag-Cu eutectic powders of step steady and Ti powder are carried out
Ball milling mixing, rotational speed of ball-mill 200r/min, ratio of grinding media to material 5:1, Ball-milling Time 2h, obtain composite soldering powder；3., cream processed：
Binding agent is added into composite soldering powder, Ag-Cu-Ti paste solders are obtained after mixing；The binding agent is hydroxyethyl cellulose；
The quality of the composite soldering powder and the volume ratio of binding agent are 20mg:0.05mL.
Other are same as Example 1.
Embodiment 8：The present embodiment is with the difference of embodiment 1：Ag-Cu-Ti+Mo paste solders described in step 3 are
Prepare according to the following steps：
1., prepare raw material：According to chemical formula (Ag72Cu28)0.8Ti0.15Mo0.05Prepare Ag-Cu eutectic powders, Ti powder and grain
The Mo powder for 20 μm is spent, the chemical formula of the Ag-Cu eutectic powders is Ag72Cu28：2., ball milling mixing：By step steady
The Mo powder that Ag-Cu eutectic powders, Ti powder and granularity are 20 μm carries out ball milling mixing, rotational speed of ball-mill 200r/min, and ratio of grinding media to material is
5:1, Ball-milling Time 2h, obtain composite soldering powder；3., cream processed：Binding agent is added into composite soldering powder, is obtained after mixing
Ag-Cu-Ti+Mo paste solders；The binding agent is hydroxyethyl cellulose；The quality of the composite soldering powder and the body of binding agent
Product ratio is 20mg:0.05mL.
Other are same as Example 1.
Embodiment 9：The present embodiment is with the difference of embodiment 1：Ag-Cu-Ti+Mo paste solders described in step 3 are
Prepare according to the following steps：
1., prepare raw material：According to chemical formula (Ag72Cu28)0.75Ti0.15Mo0.1Prepare Ag-Cu eutectic powders, Ti powder and grain
The Mo powder for 20 μm is spent, the chemical formula of the Ag-Cu eutectic powders is Ag72Cu28：2., ball milling mixing：By step steady
The Mo powder that Ag-Cu eutectic powders, Ti powder and granularity are 20 μm carries out ball milling mixing, rotational speed of ball-mill 200r/min, and ratio of grinding media to material is
5:1, Ball-milling Time 2h, obtain composite soldering powder；3., cream processed：Binding agent is added into composite soldering powder, is obtained after mixing
Ag-Cu-Ti+Mo paste solders；The binding agent is hydroxyethyl cellulose；The quality of the composite soldering powder and the body of binding agent
Product ratio is 20mg:0.05mL.
Other are same as Example 1.
The porous silicon nitride ceramic obtained to embodiment 1-9 carries out shear strength survey with invar alloy compression shear performance test part
Examination, shown in test result table 1.
Table 1
| Room temperature shear strength (MPa) | |
| Embodiment 1 | 81 |
| Embodiment 2 | 67 |
| Embodiment 3 | 52 |
| Embodiment 4 | 47 |
| Embodiment 5 | 35 |
| Embodiment 6 | 38 |
| Embodiment 7 | 44 |
| Embodiment 8 | 42 |
| Embodiment 9 | 39 |
Understand, when the atomic percentage conc of Ti in Ag-Cu-Ti solders is 0.05% and 0.15%, to add Mo by table 1
Element can reduce the shear strength of weldment.When the atomic percentage conc of Ti in Ag-Cu-Ti solders is 0.1%, addition Mo members
Element, when the atomic percentage conc of Mo in Ag-Cu-Ti+Mo solders is 0.05%, the shear strength of weldment reaches 81MPa, when
When Mo atomic percentage conc increases to 0.1% in Ag-Cu-Ti+Mo solders, the shear strength of weldment does not reach 67MPa, and not
Addition Mo elements compared to improving 15MPa, but when Mo atomic percentage conc is 0.05% compared with have dropped 14MPa, this
It is primarily due to that Ti contents are very few to cause solder and ceramics reaction insufficient, thus reaction layer thickness can be reduced, so that pottery
Combination between porcelain mother metal and solder is deteriorated.Otherwise improve when Ti contents rise the combination between ceramics and solder, as Ti contains
Amount is lasting to be risen, it will the dissolving in aggravation Cu intermediate layers, so that occurring harmful phase in weld seam, is unfavorable for joint performance, to sum up
10% Ti contents are optimum values.Adding a small amount of Mo (5%) on this basis can effectively reduce close to ceramic side pricker
The thermal coefficient of expansion of material improves joint performance so as to reduce the residual thermal stress in joint.But Mo contents continue to increase
Also the destruction in Cu intermediate layers can be aggravated so as to introduce harmful phase, therefore 5% Mo contents are optimal.
Claims (10)
- A kind of 1. method that soldering is carried out to porous silicon nitride ceramic and invar alloy using composite soldering, it is characterised in that it is Complete according to the following steps：First, polish：By porous Si3N4The surface to be welded of ceramics is successively with 200# abrasive paper for metallograph, 400# abrasive paper for metallograph, 600# metallographic sand Paper and 800# abrasive paper for metallograph are polished, and obtain porous Si after surface to be welded polishing3N4Ceramics；Invar surface to be welded is used successively 400# abrasive paper for metallograph, 600# abrasive paper for metallograph and 1000# abrasive paper for metallograph are polished, and obtain Invar after surface to be welded polishing；By Cu paper tinsels Piece is polished with 400# abrasive paper for metallograph, 600# abrasive paper for metallograph and 1000# abrasive paper for metallograph successively, be polishing to thickness for 140 μm~ 150 μm, Cu paillon foils after being polished；2nd, clean：Porous Si after surface to be welded is polished3N4Ceramics are put into alcohol and cleaned, and porous Si to be welded is obtained after drying3N4Pottery Porcelain；Invar immerses in acetone and is cleaned by ultrasonic after surface to be welded is polished, and is rinsed after taking-up with absolute ethyl alcohol, and dries up, and obtains Invar to be welded；Cu paillon foils after polishing are immersed in acetone and are cleaned by ultrasonic, are rinsed after taking-up with absolute ethyl alcohol, and are dried up, are obtained To clean Cu paillon foils；3rd, Ag-Cu-Ti+Mo paste solders are coated in porous Si to be welded3N4On the surface to be welded of ceramics, by Ag-Cu paste solders On surface to be welded coated in Invar to be welded, then from top to bottom according to porous Si3N4Ceramics, Ag-Cu-Ti+Mo paste solders, do The order of net Cu paillon foils, Ag-Cu paste solders and Invar is overlapped, and obtains sample to be welded；4th, vacuum brazing：By sample to be welded with porous Si3N4Ceramics are placed in graphite jig in upper form, and in sample to be welded Porous Si3N4Ceramic upper surface carries out physics pressure, and pressure is 1 × 104Pa~1.5 × 104Pa, it is then transferred to vacuum pricker In brazier, vacuum in vacuum brazing furnace is first adjusted to 1 × 10-3Pa~6 × 10-3Pa, 300 DEG C are then heated to, and in temperature It is 1 × 10 for 300 DEG C, physical pressure4Pa~1.5 × 104Pa and vacuum are 1 × 10-3Pa~6 × 10-3It is incubated under Pa 20min, then brazing temperature is warming up to, and be 1 × 10 in physical pressure4Pa~1.5 × 104Pa, vacuum are 1 × 10-3Pa~6 ×10-3Pa and brazing temperature complete soldering, and 300 DEG C are cooled to after the completion of soldering, then cools to room temperature with the furnace, that is, is completed porous The soldering of silicon nitride ceramics and invar alloy.
- A kind of soldering is carried out to porous silicon nitride ceramic and invar alloy using composite soldering 2. according to claim 1 Method, it is characterised in that porous Si described in step 13N4The porosity of ceramics is 45%~55%.
- A kind of soldering is carried out to porous silicon nitride ceramic and invar alloy using composite soldering 3. according to claim 1 Method, it is characterised in that the Ag-Cu-Ti+Mo paste solders described in step 3 are to prepare according to the following steps：1., prepare raw material：According to chemical formula (Ag72Cu28)0.85Ti0.1Mo0.05Or (Ag72Cu28)0.8Ti0.1Mo0.1Prepare Ag-Cu to be total to Crystalline flour end, Ti powder and granularity are 20 μm of Mo powder, and the chemical formula of the Ag-Cu eutectic powders is Ag72Cu28：2., ball milling mixing： The Mo powder that the Ag-Cu eutectic powders, Ti powder and granularity of step steady are 20 μm is subjected to ball milling mixing, rotational speed of ball-mill is 200r/min, ratio of grinding media to material 5:1, Ball-milling Time 2h, obtain composite soldering powder；3., cream processed：Added into composite soldering powder viscous Agent is tied, Ag-Cu-Ti+Mo paste solders are obtained after mixing；The binding agent is hydroxyethyl cellulose；The composite soldering powder Quality and the volume ratio of binding agent are 20mg:0.05mL.
- 4. one kind according to claim 1 or 3 carries out pricker using composite soldering to porous silicon nitride ceramic and invar alloy The method of weldering, it is characterised in that Ag-Cu-Ti+Mo paste solders are coated in porous Si to be welded in step 33N4Ceramic is to be welded On face, coating thickness is 100 μm~150 μm.
- A kind of soldering is carried out to porous silicon nitride ceramic and invar alloy using composite soldering 5. according to claim 1 Method, it is characterised in that the Ag-Cu paste solders described in step 3 are to prepare according to the following steps：Into Ag-Cu eutectic powders Binding agent is added, Ag-Cu paste solders are obtained after mixing；The chemical formula of the Ag-Cu eutectic powders is Ag72Cu28；It is described viscous Knot agent is hydroxyethyl cellulose；The quality of the Ag-Cu eutectic powders and the volume ratio of binding agent are 20mg:0.05mL.
- 6. a kind of according to claim 1 or 5 carry out pricker using composite soldering to porous silicon nitride ceramic and invar alloy The method of weldering, it is characterised in that Ag-Cu paste solders are coated on Invar to be welded surface to be welded in step 3, coating thickness For 100 μm~150 μm.
- A kind of soldering is carried out to porous silicon nitride ceramic and invar alloy using composite soldering 7. according to claim 1 Method, it is characterised in that Invar immerses in acetone and is cleaned by ultrasonic after surface to be welded is polished in step 2, is cleaned by ultrasonic 15min。
- A kind of soldering is carried out to porous silicon nitride ceramic and invar alloy using composite soldering 8. according to claim 1 Method, it is characterised in that Cu paillon foils after polishing are immersed in acetone in step 2 and are cleaned by ultrasonic, are cleaned by ultrasonic 10min.
- A kind of soldering is carried out to porous silicon nitride ceramic and invar alloy using composite soldering 9. according to claim 1 Method, it is characterised in that vacuum in vacuum brazing furnace is first adjusted to 6 × 10 in step 4-3Pa, it is 6 × 10 in vacuum-3Pa Under using the rate of heat addition as 10 DEG C/min be warming up to 300 DEG C, and temperature be 300 DEG C, physical pressure be 1 × 104Pa and vacuum For 6 × 10-3Be incubated 20min under Pa, then 900 DEG C be warming up to 10 DEG C/min programming rate, and physical pressure be 1 × 104Pa, vacuum are 6 × 10-3Pa and temperature are to carry out soldering, holding time 20min, with 5 after the completion of soldering at 900 DEG C DEG C/min cooling velocity is cooled to 300 DEG C, then cool to room temperature with the furnace, that is, complete porous silicon nitride ceramic and invar alloy Soldering.
- 10. kind according to claim 1 carries out soldering using composite soldering to porous silicon nitride ceramic and invar alloy Method, it is characterised in that in the porous Si of sample to be welded in step 43N4Ceramic upper surface carries out physics pressure detailed process such as Under：In the porous Si of sample to be welded3N4One block of Mo alloy is placed in ceramic upper surface, using Mo alloys to the porous of sample to be welded Si3N4Ceramic upper surface carries out physics pressure, and pressure is 1 × 104Pa。
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