CN109822260A - Solder and its method for welding for air atmosphere soldering SiC ceramic - Google Patents

Solder and its method for welding for air atmosphere soldering SiC ceramic Download PDF

Info

Publication number
CN109822260A
CN109822260A CN201910281252.9A CN201910281252A CN109822260A CN 109822260 A CN109822260 A CN 109822260A CN 201910281252 A CN201910281252 A CN 201910281252A CN 109822260 A CN109822260 A CN 109822260A
Authority
CN
China
Prior art keywords
sic ceramic
powder
solder
air atmosphere
welding
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910281252.9A
Other languages
Chinese (zh)
Inventor
曹健
王志权
司晓庆
李淳
亓钧雷
冯吉才
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Harbin Institute of Technology
Original Assignee
Harbin Institute of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Harbin Institute of Technology filed Critical Harbin Institute of Technology
Priority to CN201910281252.9A priority Critical patent/CN109822260A/en
Publication of CN109822260A publication Critical patent/CN109822260A/en
Pending legal-status Critical Current

Links

Abstract

For the solder and its method for welding of air atmosphere soldering SiC ceramic, the invention belongs to SiC ceramic interconnection technique fields, it will solve the problems such as connection atmosphere requirements present in existing SiC ceramic brazing process are high, apparatus and process is complicated and Joint Reliability is poor.Solder system used is Ag-V2O5, wherein Ag powder is matrix, V2O5Powder is reaction addition phase.Method for welding: one, surface grinding process is carried out to SiC ceramic;Two, by Ag powder and V2O5Sphere of powder mill is uniformly mixed;Three, binder is prepared;Four, solder mixed-powder and binder are mixed to get solder paste;Five, solder paste is coated in ceramic surface to be welded;Six, it is placed in Muffle furnace after the assembly is completed, completes soldering connection in 950-1100 DEG C of temperature range.The present invention realizes SiC ceramic being reliably connected in air atmosphere, and apparatus and process is easy, high production efficiency.Meanwhile connector oxidation resistance is excellent, stable mechanical performance.

Description

Solder and its method for welding for air atmosphere soldering SiC ceramic
Technical field
The invention belongs to SiC ceramic interconnection technique fields, and in particular to one kind can be used for being brazed SiC ceramic in air atmosphere Novel solder system and its method for welding.
Background technique
Silicon carbide ceramics (Silica Carbide, SiC) have high mechanical strength, chemical property is stable, high-temperature behavior is excellent Therefore the features such as different and radiation resistance ability is strong has in the energy, chemical industry, aerospace and nuclear industry field and extremely widely answers Use background.As a kind of typical structure/function ceramics, SiC ceramic is processed into generally according to actual demand in industrial production The component of various complicated shapes.Due to itself extreme hardness, brittleness is larger, it is difficult to be carried out by traditional mechanical processing tools Machine-shaping significantly limits the further expansion of its application prospect.In ceramic joining field, soldering because it is efficiently convenient, The features such as repeatable good and joint performance is stablized and be used widely.
Currently, the method for welding for SiC ceramic mainly has vacuum active soldering and glass soldering.Wherein, vacuum active Soldering is chemically reacted mainly by means of the Ti/Zr/Ni/Cr/Co isoreactivity metal in solder with SiC ceramic, realizes solder In the good wet of SiC ceramic surface and being reliably connected between ceramic base material.To avoid active element oxidation deactivation, entirely connect It must assure that excellent vacuum condition or stable protective atmosphere in termination process, while more demanding to brazing equipment.? Higher economic cost is necessarily brought in actual industrial production.In addition, vacuum active soldered fitting do not have generally it is resistance to anti-oxidant Ability certainly will influence the reliability and applicability of connector, limit application of the SiC ceramic in high temperature oxidation stability environment.With glass Although the glass soldering that glass is solder can connect SiC ceramic in air atmosphere, glass itself has larger brittleness, intolerant to The defects of impact, easy crack initiation.In sintering and brazing process crystalline polamer inevitably occurs for glass solder, solder Linear expansion coefficient changes therewith, leads in soldered fitting that there are larger residual stress, reduces soldered fitting mechanical performance.
Air reaction is brazed (Reactive air brazing, RAB) method usually with noble metal-metal oxide system (such as Ag-CuO/V2O5Deng) it is solder, it has been successfully applied to the connection of the oxide ceramics such as zirconium oxide and aluminium oxide at present.Solder Itself has splendid oxidation resistance, and connection procedure can be carried out directly in high temperature air atmosphere, simple process, production efficiency It is high.Ag base solder plasticity is excellent, can be by being plastically deformed the thermal stress being effectively reduced in soldered fitting.Air reaction soldering connects Head performance is stablized, and applicability is good.But this method is only used for the connection of oxide ceramics at present.Thought by using for reference the design Think, air reaction method for welding is introduced to the connection area of SiC ceramic, solves to need height in SiC ceramic brazing process by direct The problems such as vacuum environment, connector be not anti-oxidant and performance is unstable pushes SiC ceramic answering in high temperature oxidation stability environment extensively With, while soldering production cost and device requirement can be significantly reduced, greatly improve production efficiency.So far, not yet related In any report of the air reaction soldering for the connection of the non-oxide ceramics such as SiC, noble metal-metal oxygen in air atmosphere is solved Combination problem between compound solder and SiC ceramic matrix is crucial research object.
Summary of the invention
The invention aims to solve connection atmosphere requirements height, equipment work present in existing SiC ceramic brazing process The problems such as skill complexity and poor Joint Reliability.Meanwhile the good oxidation resistance of soldered fitting and reliable mechanical performance are assigned, To meet SiC ceramic in the extensive use demand of a variety of industrial circles, so that providing one kind can be used for air atmosphere soldering SiC The novel solder system and method for welding of ceramics.
The present invention is brazed the solder of SiC ceramic by Ag powder and V for air atmosphere2O5Powder composition, wherein Ag powder is solder base Body, V2O5Powder is reaction addition phase, V2O5The additive amount of powder is 1~20mol%.
Solder of the present invention for air atmosphere soldering SiC ceramic can carry out brazing process in air atmosphere, be brazed When specimen surface need to apply certain pressure, brazing process carries out in Muffle furnace.
Method for welding of the present invention for the solder of air atmosphere soldering SiC ceramic is realized according to the following steps:
One, SiC ceramic to be welded is surface-treated, i.e., is polished with sand paper welding surface, then by burnishing part SiC ceramic after reason, which immerses in acetone soln, to be cleaned by ultrasonic, the SiC ceramic after being surface-treated;
Two, by Ag powder and V2O5Powder mull mixes, wherein V2O5The additive amount of powder is 1~20mol%, after grinding To mixed-powder, then dehydrated alcohol will be added in mixed-powder and carry out ball-milling treatment, be sieved after drying, obtain uniform solder Mixed-powder;
Three, ethyl cellulose is dissolved in terpinol, obtains ethyl cellulose-terpineol solution binder;
Four, solder mixed-powder obtained in step 2 is added in ethyl cellulose-terpineol solution binder, stirring Solder paste is obtained after mixing;
Five, solder paste is coated uniformly on to the surface to be welded of SiC ceramic by the way of silk-screen printing;
Six, it will be coated with the SiC ceramic surface to be welded fitting assembly of solder paste, be put into Muffle furnace, applied soldering pressure, add 200 DEG C of 30~60min of degasification are warming up to when hot first, are then warming up to 400~500 DEG C of 30~60min of plastic removal, then be warming up to 950~1100 DEG C of ranges keep the temperature 10~60min, then cool to room temperature with the furnace, complete the soldering of SiC ceramic.
The advantages of novel solder system and technique of the present invention for being used to be brazed SiC ceramic, is:
(a) the reliable soldering that SiC ceramic can be realized in air atmosphere, does not need high vacuum or protective atmosphere, shows Work simplifies soldering processes, and production efficiency greatly improves, while brazing equipment used is Muffle furnace, and device requirement threshold is low;
(b) solder system is Ag-V2O5, itself has splendid oxidation resistance, and gained SiC ceramic soldered fitting can answer For various oxidative environments, SiC ceramic can effectively be pushed to be applied to more extensive industrial circle;
(c) V in solder2O5The SiO of continuous uniform can be generated in ceramic surface with SiC ceramic vigorous reaction2Layer, really Combining closely between solder and ceramic matrix is protected, while brazed seam matrix is Ag, can be effectively relieved and be connect by plastic deformation Head residual stress, ensure that the reliable mechanical performance of SiC ceramic connector.
Detailed description of the invention
Fig. 1 is that embodiment one selects Ag-V2O5Joint interface tissue topography obtained by solder brazing SiC ceramic;
Fig. 2 is that embodiment one selects Ag-V2O5Connector room temperature shear strength test figure obtained by solder brazing SiC ceramic.
Specific embodiment
Specific embodiment 1: present embodiment is brazed the solder of SiC ceramic by Ag powder and V for air atmosphere2O5Powder group At wherein Ag powder is solder matrix, V2O5Powder is reaction addition phase, V2O5The additive amount of powder is 1~20mol%.
Specific embodiment 2: the present embodiment is different from the first embodiment in that the partial size of the Ag powder is 5 ~10 μm.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that the V2O5The grain of powder Diameter is 5~10 μm.
Specific embodiment 4: present embodiment for air atmosphere soldering SiC ceramic solder method for welding according to The following steps are implemented:
One, SiC ceramic to be welded is surface-treated, i.e., is polished with sand paper welding surface, then by burnishing part SiC ceramic after reason, which immerses in acetone soln, to be cleaned by ultrasonic, the SiC ceramic after being surface-treated;
Two, by Ag powder and V2O5Powder mull mixes, wherein V2O5The additive amount of powder is 1~20mol%, after grinding To mixed-powder, then dehydrated alcohol will be added in mixed-powder and carry out ball-milling treatment, be sieved after drying, obtain uniform solder Mixed-powder;
Three, ethyl cellulose is dissolved in terpinol, obtains ethyl cellulose-terpineol solution binder;
Four, solder mixed-powder obtained in step 2 is added in ethyl cellulose-terpineol solution binder, stirring Solder paste is obtained after mixing;
Five, solder paste is coated uniformly on to the surface to be welded of SiC ceramic by the way of silk-screen printing;
Six, it will be coated with the SiC ceramic surface to be welded fitting assembly of solder paste, be put into Muffle furnace, applied soldering pressure, add 200 DEG C of 30~60min of degasification are warming up to when hot first, are then warming up to 400~500 DEG C of 30~60min of plastic removal, then be warming up to 950~1100 DEG C of ranges keep the temperature 10~60min, then cool to room temperature with the furnace, complete the soldering of SiC ceramic.
Specific embodiment 5: mixed-powder is placed in by present embodiment from step 2 unlike specific embodiment four In agate jar and dehydrated alcohol progress ball-milling treatment, mixed-powder and dehydrated alcohol weight ratio in the ball grinder is added For (1~2): 1, drum's speed of rotation 300-400r/min, Ball-milling Time 3h.
Specific embodiment 6: present embodiment unlike specific embodiment four or five in step 2 dry after mistake 300~400 meshes.
Specific embodiment 7: described in step 3 unlike one of present embodiment and specific embodiment four to six The content of ethyl cellulose is 2~10wt% in ethyl cellulose-terpineol solution binder.
Specific embodiment 8: described in step 4 unlike one of present embodiment and specific embodiment four to seven Solder mixed-powder and ethyl cellulose-terpineol solution binder weight ratio are (2~4): 1.
Specific embodiment 9: described in step 5 unlike one of present embodiment and specific embodiment four to eight The mesh number of web plate used by method for printing screen is 300~400, and screen thickness is 100~200 μm.
Specific embodiment 10: applying in step 6 unlike one of present embodiment and specific embodiment four to nine Soldering pressure is 2~30kPa.
Specific embodiment 11: described in step 6 unlike one of present embodiment and specific embodiment four to ten Muffle furnace heating with rate of temperature fall control in 2~15 DEG C/min.
Specific embodiment 12: present embodiment exists from step 6 unlike specific embodiment four to one of 11 Brazing temperature is that 25~45min is kept the temperature at 950~1100 DEG C.
Specific embodiment 13: present embodiment from unlike specific embodiment four to one of 11 in step 2 By Ag powder and V2O5Powder mull mixes, wherein V2O5The additive amount of powder is 4~10mol%.
Embodiment one: the present embodiment is used for the method for welding of the solder of air atmosphere soldering SiC ceramic according to the following steps Implement:
One, SiC ceramic to be welded is surface-treated, #1000 sand paper is selected to beat the welding surface of SiC ceramic Mill obtains uniform ceramic surface to be welded, then immerses in acetone soln the SiC ceramic after grinding process and be cleaned by ultrasonic 15min, the impurity such as removal surface and oil contaminant, the SiC ceramic after being surface-treated;
Two, Ag and V is weighed according to Mol ratio2O5Powder, V2O5Content is 8mol%, by powder after the completion of weighing End is placed in ground and mixed in agate crucible, and then mixed-powder is placed in agate jar and dehydrated alcohol, mixed powder is added The weight ratio of end and dehydrated alcohol is 1:1, the ball-milling treatment 3h under 300r/min speed conditions, crosses 300 mesh after 100 DEG C of drying Sieve, obtains uniform solder mixed-powder;
Three, it takes appropriate ethyl cellulose to be dissolved in terpinol, obtains ethyl cellulose-terpineol solution binder, The additive amount of middle ethyl cellulose is 2wt%;
Four, solder mixed-powder obtained in step 2 is added in ethyl cellulose-terpineol solution binder, solder Mixed-powder and ethyl cellulose-terpineol solution binder weight ratio are 2:1, obtain solder paste after being uniformly mixed;
Five, solder paste obtained in step 4 is coated uniformly on using with a thickness of 100 μm of 300 mesh silk-screen printing web plates SiC ceramic surface to be welded;
Six, it will be coated with the SiC ceramic surface to be welded fitting assembly of solder paste obtained in step 5, be then placed in Muffle furnace In, apply 20kPa pressure in sample top, it is ensured that be in close contact between solder and ceramics, when heating is warming up to 200 DEG C first and removes Gas 30min is then warming up to 400 DEG C of plastic removal 30min, then is warming up to 1050 DEG C of heat preservation 30min, then cools to room temperature with the furnace, Complete the soldering of SiC ceramic.
For the quality of directly perceived characterization soldered fitting of the present invention, the SiC ceramic joint interface tissue after soldering is seen It examines, the typical interface tissue scanning Electronic Speculum back scattering photo that embodiment one obtains is as shown in Figure 1.The result shows that Ag-V2O5Solder It is well combined with two sides ceramics base material, the defects of pore-free crackle.Brazed seam center is with Ag+VO2For matrix, a small amount of remaining V2O5 For Dispersed precipitate in brazed seam, two sides SiC ceramic surface generates uniformly continuous SiO2Conversion zone.It meanwhile being characterization soldering The mechanical property of connector carries out room temperature shear strength test to SiC ceramic soldered fitting, as a result as shown in Figure 2.The result shows that Connector highest shear strength is close to 60MPa, it was demonstrated that the novel solder system and method for welding that the present invention is developed can be in air The reliable SiC ceramic soldered fitting of performance is obtained in atmosphere.
Embodiment two: the present embodiment is used for the method for welding of the solder of air atmosphere soldering SiC ceramic according to the following steps Implement:
One, SiC ceramic is surface-treated, #1000 sand paper is selected to polish its surface, obtained uniform to be welded Then ceramics after grinding process are immersed in acetone soln and are cleaned by ultrasonic 15min by ceramic surface, removal surface and oil contaminant etc. is miscellaneous Matter, the SiC ceramic after being surface-treated;
Two, Ag and V is weighed according to Mol ratio2O5Powder, V2O5Content is 8mol%, by powder after the completion of weighing End is placed in ground and mixed in agate crucible, and then mixed-powder is placed in agate jar and dehydrated alcohol, solder powder is added Weight ratio with dehydrated alcohol is 1:1, the ball-milling treatment 3h under 350r/min speed conditions, crosses 300 meshes after 100 DEG C of drying, Obtain uniform solder mixed-powder;
Three, it takes appropriate ethyl cellulose to be dissolved in terpinol, obtains ethyl cellulose-terpineol solution binder, The additive amount of middle ethyl cellulose is 2wt%;
Four, solder mixed-powder obtained in step 2 is added in ethyl cellulose-terpineol solution binder, solder Mixed-powder and ethyl cellulose-terpineol solution binder weight ratio are 2:1, obtain solder paste after being uniformly mixed;
Five, solder paste obtained in step 4 is coated uniformly on using with a thickness of 200 μm of 300 mesh silk-screen printing web plates SiC ceramic surface to be welded;
Six, it will be coated with the SiC ceramic surface to be welded fitting assembly of solder paste obtained in step 5, be then placed in Muffle furnace In, apply 20kPa pressure in sample top, it is ensured that be in close contact between solder and ceramics, when heating is warming up to 200 DEG C first and removes Gas 30min is then warming up to 400 DEG C of plastic removal 30min, then is warming up to 1050 DEG C of heat preservation 10min, then cools to room temperature with the furnace, Complete the soldering of SiC ceramic.
Shear strength test is carried out to SiC ceramic soldered fitting obtained by the present embodiment, connector average shear strength is 52Mpa。
Embodiment three: the present embodiment is used for the method for welding of the solder of air atmosphere soldering SiC ceramic according to the following steps Implement:
One, SiC ceramic is surface-treated, selects #1000 sand paper to polish SiC ceramic welding surface, obtains Then ceramics after grinding process are immersed in acetone soln and are cleaned by ultrasonic 15min, remove surface by uniform ceramic surface to be welded The impurity such as greasy dirt, the SiC ceramic after being surface-treated;
Two, Ag and V is weighed according to Mol ratio2O5Powder, V2O5Content is 8mol%, by powder after the completion of weighing End is placed in ground and mixed in agate crucible, and then mixed-powder is placed in agate jar and dehydrated alcohol, mixed powder is added The weight ratio of end and dehydrated alcohol is 2:1, the ball-milling treatment 3h under 350r/min speed conditions, crosses 300 mesh after 100 DEG C of drying Sieve, obtains uniform solder mixed-powder;
Three, it takes appropriate ethyl cellulose to be dissolved in terpinol, obtains ethyl cellulose-terpineol solution binder, The additive amount of middle ethyl cellulose is 4wt%;
Four, solder mixed-powder obtained in step 2 is added in ethyl cellulose-terpineol solution binder, solder Mixed-powder and ethyl cellulose-terpineol solution binder weight ratio are 2:1, obtain solder paste after being uniformly mixed;
Five, solder paste obtained in step 4 is coated uniformly on using with a thickness of 100 μm of 300 mesh silk-screen printing web plates SiC ceramic surface to be welded;
Six, it will be coated with the SiC ceramic surface to be welded fitting assembly of solder paste obtained in step 5, be then placed in Muffle furnace In, apply 20kPa pressure in sample top, it is ensured that be in close contact between solder and ceramics, when heating is warming up to 200 DEG C first and removes Gas 30min is then warming up to 400 DEG C of plastic removal 30min, then is warming up to 1100 DEG C of heat preservation 10min, then cools to room temperature with the furnace, Complete the soldering of SiC ceramic.
Shear strength test is carried out to SiC ceramic soldered fitting obtained by the present embodiment, connector average shear strength is 45MPa。
Example IV: the present embodiment is used for the method for welding of the solder of air atmosphere soldering SiC ceramic according to the following steps Implement:
One, SiC ceramic is surface-treated, selects #1000 sand paper to polish the welding surface of SiC ceramic, obtains To uniform ceramic surface to be welded, then the ceramics after grinding process are immersed in acetone soln and are cleaned by ultrasonic 15min, remove table The impurity such as face greasy dirt, the SiC ceramic after being surface-treated;
Two, Ag and V is weighed according to Mol ratio2O5Powder, V2O5Content is 4mol%, by powder after the completion of weighing End is placed in ground and mixed in agate crucible, and then mixed-powder is placed in agate jar and dehydrated alcohol, mixed powder is added The weight ratio of end and dehydrated alcohol is 2:1, the ball-milling treatment 3h under 400r/min speed conditions, crosses 300 mesh after 100 DEG C of drying Sieve, obtains uniform solder mixed-powder;
Three, it takes appropriate ethyl cellulose to be dissolved in terpinol, obtains ethyl cellulose-terpineol solution binder, The additive amount of middle ethyl cellulose is 8wt%;
Four, solder mixed-powder obtained in step 2 is added in ethyl cellulose-terpineol solution binder, solder Mixed-powder and ethyl cellulose-terpineol solution binder weight ratio are 3:1, obtain solder paste after being uniformly mixed;
Five, solder paste obtained in step 4 is coated uniformly on using with a thickness of 100 μm of 300 mesh silk-screen printing web plates SiC ceramic surface to be welded;
Six, it will be coated with the SiC ceramic surface to be welded fitting assembly of solder paste obtained in step 5, be then placed in Muffle furnace In, apply 20kPa pressure in sample top, it is ensured that be in close contact between solder and ceramics, when heating is warming up to 200 DEG C first and removes Gas 30min is then warming up to 400 DEG C of plastic removal 30min, then is warming up to 950 DEG C of heat preservation 30min, then cools to room temperature with the furnace, complete At the soldering of SiC ceramic.
Shear strength test is carried out to SiC ceramic soldered fitting obtained by the present embodiment, connector average shear strength is 40MPa。
Embodiment five: the present embodiment is used for the method for welding of the solder of air atmosphere soldering SiC ceramic according to the following steps Implement:
One, SiC ceramic is surface-treated, selects #1000 sand paper to polish the welding surface of SiC ceramic, obtains To uniform ceramic surface to be welded, then the ceramics after grinding process are immersed in acetone soln and are cleaned by ultrasonic 15min, remove table The impurity such as face greasy dirt, the SiC ceramic after being surface-treated;
Two, Ag and V is weighed according to Mol ratio2O5Powder, V2O5Content is 20mol%, by powder after the completion of weighing End is placed in ground and mixed in agate crucible, and then mixed-powder is placed in agate jar and dehydrated alcohol, solder powder is added Weight ratio with dehydrated alcohol is 2:1, the ball-milling treatment 3h under 400r/min speed conditions, crosses 300 meshes after 100 DEG C of drying, Obtain uniform solder mixed-powder;
Three, it takes appropriate ethyl cellulose to be dissolved in terpinol, obtains ethyl cellulose-terpineol solution binder, The additive amount of middle ethyl cellulose is 10wt%;
Four, solder mixed-powder obtained in step 2 is added in ethyl cellulose-terpineol solution binder, solder Mixed-powder and ethyl cellulose-terpineol solution binder weight ratio are 3.5:1, obtain solder after being uniformly mixed Cream;
Five, solder paste obtained in step 4 is coated uniformly on using with a thickness of 100 μm of 300 mesh silk-screen printing web plates SiC ceramic surface to be welded;
Six, it will be coated with the SiC ceramic surface to be welded fitting assembly of solder paste obtained in step 5, be then placed in Muffle furnace In, apply 30kPa pressure in sample top, it is ensured that be in close contact between solder and ceramics, when heating is warming up to 200 DEG C first and removes Gas 30min is then warming up to 400 DEG C of plastic removal 30min, then is warming up to 900 DEG C of heat preservation 30min, then cools to room temperature with the furnace, complete At the soldering of SiC ceramic.
Shear strength test is carried out to SiC ceramic soldered fitting obtained by the present embodiment, connector average shear strength is 34MPa。
Embodiment six: the present embodiment is used for the method for welding of the solder of air atmosphere soldering SiC ceramic according to the following steps Implement:
One, SiC ceramic is surface-treated, selects #1000 sand paper to polish the welding surface of SiC ceramic, obtains To uniform ceramic surface to be welded, then the ceramics after grinding process are immersed in acetone soln and are cleaned by ultrasonic 15min, remove table The impurity such as face greasy dirt, the SiC ceramic after being surface-treated;
Two, Ag and V is weighed according to Mol ratio2O5Powder, V2O5Content is 2mol%, by powder after the completion of weighing End is placed in ground and mixed in agate crucible, and then mixed-powder is placed in agate jar and dehydrated alcohol, solder powder is added Weight ratio with dehydrated alcohol is 2:1, the ball-milling treatment 3h under 400r/min speed conditions, crosses 300 meshes after 100 DEG C of drying, Obtain uniform solder mixed-powder;
Three, it takes appropriate ethyl cellulose to be dissolved in terpinol, obtains ethyl cellulose-terpineol solution binder, The additive amount of middle ethyl cellulose is 10wt%;
Four, solder mixed-powder obtained in step 2 is added in ethyl cellulose-terpineol solution binder, solder Mixed-powder and ethyl cellulose-terpineol solution binder weight ratio are 4:1, obtain solder paste after being uniformly mixed;
Five, solder paste obtained in step 4 is coated uniformly on using with a thickness of 100 μm of 400 mesh silk-screen printing web plates SiC ceramic surface to be welded;
Six, it will be coated with the SiC ceramic surface to be welded fitting assembly of solder paste obtained in step 5, be then placed in Muffle furnace In, apply 5kPa pressure in sample top, it is ensured that be in close contact between solder and ceramics, when heating is warming up to 200 DEG C first and removes Gas 30min is then warming up to 500 DEG C of plastic removal 30min, then is warming up to 900 DEG C of heat preservation 60min, then cools to room temperature with the furnace, complete At the soldering of SiC ceramic.
Shear strength test is carried out to SiC ceramic soldered fitting obtained by the present embodiment, connector average shear strength is 37MPa。

Claims (10)

1. the solder for air atmosphere soldering SiC ceramic, it is characterised in that this is used for the solder of air atmosphere soldering SiC ceramic By Ag powder and V2O5Powder composition, wherein Ag powder is solder matrix, V2O5Powder is reaction addition phase, V2O5The additive amount of powder be 1~ 20mol%.
2. the solder according to claim 1 for air atmosphere soldering SiC ceramic, it is characterised in that the Ag powder Partial size is 5~10 μm.
3. the solder according to claim 1 for air atmosphere soldering SiC ceramic, it is characterised in that the V2O5Powder Partial size be 5~10 μm.
4. the method for welding of the solder for air atmosphere soldering SiC ceramic, it is characterised in that the method for welding is according to following step It is rapid to realize:
One, SiC ceramic to be welded is surface-treated, i.e., is polished with sand paper welding surface, it then will be after grinding process SiC ceramic immerse acetone soln in be cleaned by ultrasonic, the SiC ceramic after being surface-treated;
Two, by Ag powder and V2O5Powder mull mixes, wherein V2O5The additive amount of powder is 1~20mol%, is mixed after grinding Then powder will be added dehydrated alcohol and carry out ball-milling treatment, is sieved after drying, obtains uniform solder mixed powder in mixed-powder End;
Three, ethyl cellulose is dissolved in terpinol, obtains ethyl cellulose-terpineol solution binder;
Four, solder mixed-powder obtained in step 2 is added in ethyl cellulose-terpineol solution binder, is stirred Solder paste is obtained after uniformly;
Five, solder paste is coated uniformly on to the surface to be welded of SiC ceramic by the way of silk-screen printing;
Six, it will be coated with the SiC ceramic surface to be welded fitting assembly of solder paste, be put into Muffle furnace, apply soldering pressure, when heating It is warming up to 200 DEG C of 30~60min of degasification first, is then warming up to 400~500 DEG C of 30~60min of plastic removal, then it is warming up to 950~ 1100 DEG C of ranges keep the temperature 10~60min, then cool to room temperature with the furnace, complete the soldering of SiC ceramic.
5. the method for welding of the solder according to claim 4 for air atmosphere soldering SiC ceramic, it is characterised in that step 300~400 meshes are crossed after drying in rapid two.
6. the method for welding of the solder according to claim 4 for air atmosphere soldering SiC ceramic, it is characterised in that step The content of ethyl cellulose is 2~10wt% in ethyl cellulose described in rapid three-terpineol solution binder.
7. the method for welding of the solder according to claim 4 for air atmosphere soldering SiC ceramic, it is characterised in that step Solder mixed-powder described in rapid four and ethyl cellulose-terpineol solution binder weight ratio are (2~4): 1.
8. the method for welding of the solder according to claim 4 for air atmosphere soldering SiC ceramic, it is characterised in that step The mesh number of web plate used by method for printing screen described in rapid five is 300~400, and screen thickness is 100~200 μm.
9. the method for welding of the solder according to claim 4 for air atmosphere soldering SiC ceramic, it is characterised in that step Applying soldering pressure in rapid six is 2~30kPa.
10. the method for welding of the solder according to claim 4 for air atmosphere soldering SiC ceramic, it is characterised in that Step 6 keeps the temperature 25~45min at being 950~1100 DEG C in brazing temperature.
CN201910281252.9A 2019-04-09 2019-04-09 Solder and its method for welding for air atmosphere soldering SiC ceramic Pending CN109822260A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910281252.9A CN109822260A (en) 2019-04-09 2019-04-09 Solder and its method for welding for air atmosphere soldering SiC ceramic

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910281252.9A CN109822260A (en) 2019-04-09 2019-04-09 Solder and its method for welding for air atmosphere soldering SiC ceramic

Publications (1)

Publication Number Publication Date
CN109822260A true CN109822260A (en) 2019-05-31

Family

ID=66874877

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910281252.9A Pending CN109822260A (en) 2019-04-09 2019-04-09 Solder and its method for welding for air atmosphere soldering SiC ceramic

Country Status (1)

Country Link
CN (1) CN109822260A (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110653442A (en) * 2019-10-12 2020-01-07 哈尔滨工业大学 Method for aluminizing auxiliary air reaction brazing on titanium alloy surface
CN111482731A (en) * 2020-05-11 2020-08-04 湖南翰坤实业有限公司 Preparation method and application of metal welding material
CN111644739A (en) * 2020-06-15 2020-09-11 哈尔滨工业大学 Brazing filler metal system for air atmosphere brazing YSZ ceramic and brazing method
CN113213472A (en) * 2021-05-20 2021-08-06 哈尔滨工业大学 Method for preparing complex-structure carbon material anti-oxidation coating with assistance of metal liquid phase
CN113245653A (en) * 2021-06-04 2021-08-13 哈尔滨工业大学 Method for connecting ceramic and metal in air by using solid silver
CN113857605A (en) * 2021-09-13 2021-12-31 哈尔滨工业大学 Method for aluminizing surface of low-carbon steel and performing air reaction brazing with alumina ceramic
CN115213583A (en) * 2022-07-15 2022-10-21 西北工业大学 Brazing filler metal for SiCf/SiC composite material connection and brazing connection method

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59232692A (en) * 1983-06-17 1984-12-27 Ngk Spark Plug Co Ltd Brazing filler metal for joining ceramics and metal or the like and composite body composed of ceramics and metal or the like using said brazing filler metal
US20030132270A1 (en) * 2002-01-11 2003-07-17 Weil K. Scott Oxidation ceramic to metal braze seals for applications in high temperature electrochemical devices and method of making
CN101960660A (en) * 2008-03-08 2011-01-26 于利奇研究中心有限公司 Sealing arrangement for high-temperature fuel cell stack
US20130193194A1 (en) * 2010-04-19 2013-08-01 Aegis Technology Inc. Innovative braze and brazing process for hermetic sealing between ceramic and metal components in a high-temperature oxidizing or reducing atmosphere
CN106112309A (en) * 2016-07-27 2016-11-16 江苏科技大学 A kind of brazing material for SiC ceramic soldering and use the technique that this material carries out soldering
CN107151147A (en) * 2017-07-03 2017-09-12 合肥工业大学 It is a kind of to be used for the solder and soldering processes of silicon carbide ceramics soldering in atmosphere
CN108465891A (en) * 2018-03-22 2018-08-31 哈尔滨工业大学 A kind of connection method of yttrium iron garnet ferrite ceramics and copper

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59232692A (en) * 1983-06-17 1984-12-27 Ngk Spark Plug Co Ltd Brazing filler metal for joining ceramics and metal or the like and composite body composed of ceramics and metal or the like using said brazing filler metal
US20030132270A1 (en) * 2002-01-11 2003-07-17 Weil K. Scott Oxidation ceramic to metal braze seals for applications in high temperature electrochemical devices and method of making
CN101960660A (en) * 2008-03-08 2011-01-26 于利奇研究中心有限公司 Sealing arrangement for high-temperature fuel cell stack
US20130193194A1 (en) * 2010-04-19 2013-08-01 Aegis Technology Inc. Innovative braze and brazing process for hermetic sealing between ceramic and metal components in a high-temperature oxidizing or reducing atmosphere
CN106112309A (en) * 2016-07-27 2016-11-16 江苏科技大学 A kind of brazing material for SiC ceramic soldering and use the technique that this material carries out soldering
CN107151147A (en) * 2017-07-03 2017-09-12 合肥工业大学 It is a kind of to be used for the solder and soldering processes of silicon carbide ceramics soldering in atmosphere
CN108465891A (en) * 2018-03-22 2018-08-31 哈尔滨工业大学 A kind of connection method of yttrium iron garnet ferrite ceramics and copper

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王志权等: "陶瓷空气反应钎焊研究综述", 《精密成形工程》 *
石宇皓等: "陶瓷连接技术及其应用", 《精密成形工程》 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110653442A (en) * 2019-10-12 2020-01-07 哈尔滨工业大学 Method for aluminizing auxiliary air reaction brazing on titanium alloy surface
CN111482731A (en) * 2020-05-11 2020-08-04 湖南翰坤实业有限公司 Preparation method and application of metal welding material
CN111644739A (en) * 2020-06-15 2020-09-11 哈尔滨工业大学 Brazing filler metal system for air atmosphere brazing YSZ ceramic and brazing method
CN113213472A (en) * 2021-05-20 2021-08-06 哈尔滨工业大学 Method for preparing complex-structure carbon material anti-oxidation coating with assistance of metal liquid phase
CN113245653A (en) * 2021-06-04 2021-08-13 哈尔滨工业大学 Method for connecting ceramic and metal in air by using solid silver
CN113245653B (en) * 2021-06-04 2022-03-25 哈尔滨工业大学 Method for connecting ceramic and metal in air by using solid silver
CN113857605A (en) * 2021-09-13 2021-12-31 哈尔滨工业大学 Method for aluminizing surface of low-carbon steel and performing air reaction brazing with alumina ceramic
CN115213583A (en) * 2022-07-15 2022-10-21 西北工业大学 Brazing filler metal for SiCf/SiC composite material connection and brazing connection method
CN115213583B (en) * 2022-07-15 2024-04-12 西北工业大学 Brazing connection method for SiCf/SiC composite material connection

Similar Documents

Publication Publication Date Title
CN109822260A (en) Solder and its method for welding for air atmosphere soldering SiC ceramic
CN107324809B (en) Porous silicon carbide ceramic and preparation method and application thereof
CN105418131B (en) A kind of aluminium oxide ceramics low temperature brazing connection method
CN100528810C (en) Non-pressure braze welding method for ZrO2 ceramic and stainless steel or Al2O3 ceramic
CN104646852B (en) Pricker applies cream and its application
CN110330356B (en) Silicon carbide ceramic brazing connection method
CN108147671A (en) It is a kind of for devitrified glass solder of connecting silicon nitride ceramics and preparation method thereof
CN108907385B (en) Method for brazing sapphire at low temperature
CN103056553A (en) Solder, preparation method thereof and method for connecting sapphire and niobium or niobium alloys by using solder
CN110253100B (en) YSZ ceramic and stainless steel air reaction brazing connection method
CN111153713A (en) Ceramic metallization slurry and preparation method and application thereof
CN104387103B (en) The method for welding of a kind of zirconia ceramics and metallic substance
CN109721379B (en) Method for connecting AlON ceramic by using AlON powder as raw material
JP4181076B2 (en) Method of joining sintered bodies and composite structure obtained thereby
CN114769940A (en) AgCuTi-based composite solder and soldering method for connecting AlN ceramic and Cu by using same
CN104319043B (en) Manufacturing method of negative-temperature-coefficient thermistor chip electrode
CN111644739A (en) Brazing filler metal system for air atmosphere brazing YSZ ceramic and brazing method
CN109369208A (en) A kind of silicon carbide connection solder and its preparation method and application
CN106116627B (en) A kind of method of phosphate glass solder law temperature joining aluminium oxide ceramics
CN107385367A (en) A kind of preparation method of fine grain hypoxemia type multiphase Mo Si B alloys
CN112122826A (en) Soldering paste for brazing titanium-based composite material and silicon nitride ceramic, and method and application thereof
CN101468799B (en) Presureless connection and brazing method for ZrO2 ceramic and Al2O3 ceramic
US20200035637A1 (en) Bonding material and bonded product using same
CN113245653B (en) Method for connecting ceramic and metal in air by using solid silver
CN105397336A (en) Composite brazing filler material for sealing flat plate type solid oxide fuel battery and brazing method of composite brazing filler material

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20190531