CN108838504A - It is a kind of for spread connection silicon carbide ceramics composite interlayer and its Joining Technology - Google Patents
It is a kind of for spread connection silicon carbide ceramics composite interlayer and its Joining Technology Download PDFInfo
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- CN108838504A CN108838504A CN201810783473.1A CN201810783473A CN108838504A CN 108838504 A CN108838504 A CN 108838504A CN 201810783473 A CN201810783473 A CN 201810783473A CN 108838504 A CN108838504 A CN 108838504A
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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
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/02—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by means of a press ; Diffusion bonding
- B23K20/023—Thermo-compression bonding
- B23K20/026—Thermo-compression bonding with diffusion of soldering material
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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
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/22—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating taking account of the properties of the materials to be welded
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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
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/24—Preliminary treatment
Abstract
The invention discloses a kind of for spreading the composite interlayer and its Joining Technology of connection silicon carbide ceramics, wherein the raw material of the composite interlayer for spreading connection silicon carbide ceramics and proportion composition are as follows：High-purity hydride powder (TiH2) 55-65wt.%；High-purity silicon powder (Si) 20-25wt.%；High purity graphite powder (C) 12-17wt.%；High purity aluminum powder (Al) 1-3wt.%.The present invention utilizes discharge plasma sintering technique (Spark Plasma Sintering, SPS), is prepared for articulamentum under vacuum conditions with a thickness of 20-100 μm silicon carbide (SiC) connector.Layer material is connected mainly by silicon titanium-carbide (Ti3SiC2), silicon carbide (SiC) and titanium carbide (TiC) composition.By the proportion of feed change and the technological parameter of sintering, highest shear strength has reached 135.8MPa at room temperature, and articulamentum composite hardness has been more than the hardness of SiC base material, practical value with higher up to 28.1GPa.
Description
Technical field
The present invention relates to a kind of for spreading the composite interlayer and its Joining Technology of connection silicon carbide ceramics, belongs to ceramics
The connection area of material.
Background technique
With advances in technology with the development of modern industry, required structural material is also required it is more and more harsh, one
Under the environment such as a little extreme high temperature, high corrosion, high abrasion, strong irradiation, traditional metal material has been unable to meet use demand.?
In this case, some advanced ceramic materials, it is excellent by its high-temperature stability, corrosion resistance, wear resistance, Flouride-resistani acid phesphatase etc.
Different performance is shown one's talent, and the demand to ceramic composite materials structural member is increasing.Due to the restriction of technology and equipment,
Ceramic material is difficult to accomplish directly to prepare large scale or complex-shaped structural member, thus develops reliable ceramic joining technology just
As critical issue urgently to be resolved in the application of ceramics.
The a member of silicon carbide ceramics as structural ceramics is a kind of structural material most widely used at present.Carbonization at present
The connection means of silicon mainly have mechanical connection, soldering, diffusion to connect, without pressing phase reaction connection, precursor connection, reaction forming
Deng.Mechanical connecting joint can bear very high temperature and stress, but connector poor air-tightness, and junction is also easy to produce stress concentration.
Method for brazing can prepare fine and close soldered fitting, but the intensity of connector is lower, and temperature capacity is poor, and in some cases solder with it is to be welded
Wetability is insufficient between base material.Ceramic precursor connection method can be prepared to be connect with what the thermophysical property of silicon carbide substrate matched
Head, connection procedure do not need to impose severe pressure, but joint remains a large amount of stomata, reduce connector intensity and can
By property.
In recent years, for discharge plasma sintering technique (SPS) by domestic and international extensive concern, it has the high-efficient, burning that heats up
The remarkable advantages such as time short, the controllable, energy conservation and environmental protection of institutional framework are tied, can be used to prepare metal material, ceramic material, composite wood
Material, it is also possible to prepare nano material, amorphous block material, functionally gradient material (FGM) etc..Discharge plasma sintering technique (SPS) is applied
In connection silicon carbide ceramics and its composite material, development and popularization and application to silicon carbide ceramics have deep meaning.But by
It is mismatched in connection layer material and carbofrax material thermal expansion coefficient, causes residual stress excessive, so that occurring fine fisssure in connector
Line seriously affects the bonding strength and connection reliability of connector.Therefore, it is necessary to design suitable connection layer material, connection is overcome
Defect promotes the development and application of thyrite.
Summary of the invention
In order to make silicon carbide ceramics obtain the good connector of bonding strength, improve above-mentioned shortcoming in the prior art,
The present invention provides a kind of for spreading the composite interlayer and its Joining Technology of connection silicon carbide ceramics.
The present invention is used to spread the composite interlayer of connection silicon carbide ceramics, and raw material and proportion constitute as follows：
High-purity hydride powder (TiH2) 55-65wt.%, high-purity silicon powder (Si) 20-25wt.%, high purity graphite powder (C) 12-
17wt.%, high purity aluminum powder (Al) 1-3wt.%.
The purity of high-purity hydride powder>99%, granularity<25μm；The purity of the high-purity silicon powder>98%, granularity<40
μm；The purity of the high purity graphite powder>99%, granularity<5μm；The purity of the high purity aluminum powder>98%, granularity<100μm.
Above-mentioned raw materials are measured according to the ratio at normal temperature and are uniformly mixed, gained mixed-powder passes through discharge plasma sintering technique
(Spark Plasma Sintering, SPS) prepare diffusion connection silicon carbide ceramics connector room temperature shear strength be
32.7-135.8MPa articulamentum composite hardness is 5.1-28.1GPa.
The Joining Technology that connection silicon carbide ceramics is spread using composite interlayer of the present invention, is included the following steps：
Step 1：The preparation of composite interlayer powder
Amount weighs high-purity hydride powder (TiH according to the ratio2), high-purity silicon powder (Si), high purity graphite powder (C) and high purity aluminum powder
(Al), it is poured into after mixing in agate grinding alms bowl, using absolute alcohol as abrasive media, grinds 1-3h to being mixed thoroughly, then
It is placed in a vacuum drying oven drying, obtains composite interlayer powder；
Step 2：Welding preparation
SiC ceramic material is cut into SiC ceramic block with inner circle cutting machine, using polishing fluid to SiC ceramic block
Surface to be welded is polished, and the SiC ceramic block after polishing is put into alcoholic solution and is cleaned by ultrasonic, air-dries, obtains at room temperature
To ceramic base material to be welded；
Step 3：Assembly
By two pieces of ceramic base materials and composite interlayer powder to be welded according to graphite formed punch-Graphite pad-ceramic base material-to be welded
The assembled in sequence of composite interlayer powder-ceramic base material-Graphite pad-graphite formed punch to be welded is into graphite jig, then will assemble
The mold of completion is put into discharge plasma sintering system (SPS)；
Step 4：Discharge plasma sintering
After mold installs, connection pressure is adjusted to 20-60MPa, the vacuum degree in furnace be evacuated to 20Pa hereinafter, discharge etc. from
Son sintering obtains diffusion connection thyrite.
In step 1, drying temperature is 60 DEG C, drying time >=6h.
In step 2, the polishing fluid is 1-3.5 μm of diamond suspension polishing liquid.Further, 3.5 μm are successively used
Diamond suspension polishing liquid with 1 μm polishes the surface to be welded of SiC ceramic block.
In step 4, sintering temperature is 1200-1600 DEG C, and preferable temperature is 1400-1450 DEG C；Soaking time is 5-
30min。
In step 4, when sintering, heating rate is set as 50-100 DEG C/min；Rate of temperature fall is set as 10-20 DEG C/min,
Program stopped when being cooled to 600 DEG C, sintering are completed, then cool to temperature≤50 DEG C with the furnace, that is, can be taken off material.
In step 4, the articulamentum of the diffusion connection thyrite obtained after sintering is with a thickness of 20-100 μm.
Advantageous effects of the invention embody in the following areas：
The present invention explores suitable hydride powder (TiH2), silicon powder (Si), graphite powder (C) and aluminium powder (Al) proportion with
And suitable technological parameter, thyrite is attached.It is generated by mixed-powder reaction in-situ by titanium carbon
Silicon (Ti3SiC2), silicon carbide (SiC) and titanium carbide (TiC) composition composite interlayer.It is matched and is sintered by feed change
Technological parameter obtains different articulamentum composite materials, so that connector obtains different mechanical properties.On the one hand, in middle layer
Have a large amount of silicon carbide (SiC) generation, reduce the thermal expansion coefficient of middle layer, thus reduce middle layer and silicon carbide base material it
Between residual stress；On the other hand, due to the biphase strengthening of silicon carbide (SiC) and titanium carbide (TiC) in intermediate layer composites
Effect, obtains higher connector bonding strength.
The present invention can prepare high-intensitive silicon carbide ceramics connector, solve the one of the engineer application of silicon carbide ceramics
A technical problem.
Detailed description of the invention
Fig. 1 is mold assembly and subsequent technique test flow chart.
Fig. 2 prepares temperature in the sintering process of silicon carbide connector, pressure, displacement of pressing head and vacuum degree parameter when being 1350 DEG C
Figure.
Fig. 3 is with 59.5wt.% hydride powder (TiH2), 24.5wt.% silicon powder (Si), 13.9wt.% graphite powder (C) and
2.1wt.% aluminium powder (Al) is raw material, and using the connection pressure of 30MPa, the silicon carbide/carbon that 5min is obtained is kept the temperature at 1200 DEG C
The global tissue shape appearance figure (embodiment 1) of SiClx connector.
Fig. 4 is with 59.5wt.% hydride powder (TiH2), 24.5wt.% silicon powder (Si), 13.9wt.% graphite powder (C) and
2.1wt.% aluminium powder (Al) is raw material, and using the connection pressure of 50MPa, the silicon carbide/carbon that 10min is obtained is kept the temperature at 1300 DEG C
The global tissue shape appearance figure (embodiment 2) of SiClx connector.
Fig. 5 is with 59.5wt.% hydride powder (TiH2), 24.5wt.% silicon powder (Si), 13.9wt.% graphite powder (C) and
2.1wt.% aluminium powder (Al) is raw material, and using the connection pressure of 50MPa, the silicon carbide/carbon that 20min is obtained is kept the temperature at 1400 DEG C
The global tissue shape appearance figure (embodiment 3) of SiClx connector.
Fig. 6 is with 59.5wt.% hydride powder (TiH2), 24.5wt.% silicon powder (Si), 13.9wt.% graphite powder (C) and
2.1wt.% aluminium powder (Al) is raw material, and using the connection pressure of 50MPa, the silicon carbide/carbon that 10min is obtained is kept the temperature at 1450 DEG C
The global tissue shape appearance figure (embodiment 4) of SiClx connector.
Fig. 7 is with 61.2wt.% hydride powder (TiH2), 23.0wt.% silicon powder (Si), 14.7wt.% graphite powder (C) and
1.1wt.% aluminium powder (Al) is raw material, and using the connection pressure of 50MPa, the silicon carbide/carbon that 10min is obtained is kept the temperature at 1500 DEG C
The global tissue shape appearance figure (embodiment 5) of SiClx connector.
Fig. 8 is with 61.2wt.% hydride powder (TiH2), 23.0wt.% silicon powder (Si), 14.7wt.% graphite powder (C) and
1.1wt.% aluminium powder (Al) is raw material, and using the connection pressure of 50MPa, the silicon carbide/carbon that 10min is obtained is kept the temperature at 1600 DEG C
The global tissue shape appearance figure (embodiment 6) of SiClx connector.
Fig. 9 is with 61.2wt.% hydride powder (TiH2), 23.0wt.% silicon powder (Si), 14.7wt.% graphite powder (C) and
1.1wt.% aluminium powder (Al) is raw material, and using the connection pressure of 30MPa, the silicon carbide/carbon that 30min is obtained is kept the temperature at 1300 DEG C
The global tissue shape appearance figure (embodiment 7) of SiClx connector.
Specific embodiment
Below with reference to specific embodiment, technical matters and process of the invention are further illustrated.
High-purity hydride powder (TiH in following embodiment2) purity>99%, granularity<25μm；High-purity silicon powder (Si) it is pure
Degree>98%, granularity<40μm；The purity of high purity graphite powder (C)>99%, granularity<5μm；The purity of high purity aluminum powder (Al)>98%,
Granularity<100μm.Diamond lap polishes the diamond lap that suspension is 1-3.5 μm and polishes suspension.
Embodiment 1：
The Joining Technology of composite interlayer diffusion connection silicon carbide ceramics is as follows in the present embodiment：
1, the preparation of composite interlayer powder
With 59.5wt.% hydride powder (TiH2), 24.5wt.% silicon powder (Si), 13.9wt.% graphite powder (C) and
2.1wt.% aluminium powder (Al) is to pour into agate after raw material mixing to grind in alms bowl, and using absolute alcohol as abrasive media, 1h is to complete for grinding
It is complete to be uniformly mixed, it is subsequently placed in vacuum oven at 60 DEG C dry 6h, obtains composite interlayer powder；
2, welding preparation
With inner circle cutting machine by cylindric SiC ceramic materialIt is cut into the SiC ceramic disk of 3mm thickness,
Successively the surface to be welded of SiC ceramic disk is polished using 3.5 μm and 1 μm of diamond suspension polishing liquid, will be polished
SiC ceramic disk afterwards, which is put into alcoholic solution, to be cleaned by ultrasonic, and is air-dried at room temperature, and ceramic base material to be welded is obtained；
3, it assembles
By two pieces of ceramic base materials and composite interlayer powder to be welded according to graphite formed punch-Graphite pad-ceramic base material-to be welded
The assembled in sequence of composite interlayer powder-ceramic base material-Graphite pad-graphite formed punch to be welded is into graphite jig, then will assemble
The mold of completion is put into discharge plasma sintering system (SPS)；
4, discharge plasma sintering
After mold installs, connection pressure is adjusted to 30MPa, and the vacuum degree in furnace is evacuated to 20Pa hereinafter, carrying out plasma discharging
Sintering obtains diffusion connection thyrite.
Sintering procedure setting is as follows：1200 DEG C are warming up to the heating rate of 50 DEG C/min, 5min is kept the temperature, then with 10
DEG C/rate of temperature fall of min when being cooled to 600 DEG C program stopped, sintering complete, then cool to furnace chamber temperature≤50 with the furnace
DEG C, that is, it can be taken off material.
Through detecting, the shearing strength of joint that the present embodiment obtains can reach 32.7MPa, middle layer with a thickness of 35 μm, in
The Vickers hardness of interbed is up to 5.1GPa.
Embodiment 2：
The Joining Technology of composite interlayer diffusion connection silicon carbide ceramics is as follows in the present embodiment：
1, the preparation of composite interlayer powder
With 59.5wt.% hydride powder (TiH2), 24.5wt.% silicon powder (Si), 13.9wt.% graphite powder (C) and
2.1wt.% aluminium powder (Al) is to pour into agate after raw material mixing to grind in alms bowl, and using absolute alcohol as abrasive media, 2h is to complete for grinding
It is complete to be uniformly mixed, it is subsequently placed in vacuum oven at 60 DEG C dry 6h, obtains composite interlayer powder；
2, welding preparation
With inner circle cutting machine by cylindric SiC ceramic materialIt is cut into the SiC ceramic disk of 3mm thickness,
Successively the surface to be welded of SiC ceramic disk is polished using 3.5 μm and 1 μm of diamond suspension polishing liquid, will be polished
SiC ceramic disk afterwards, which is put into alcoholic solution, to be cleaned by ultrasonic, and is air-dried at room temperature, and ceramic base material to be welded is obtained；
3, it assembles
By two pieces of ceramic base materials and composite interlayer powder to be welded according to graphite formed punch-Graphite pad-ceramic base material-to be welded
The assembled in sequence of composite interlayer powder-ceramic base material-Graphite pad-graphite formed punch to be welded is into graphite jig, then will assemble
The mold of completion is put into discharge plasma sintering system (SPS)；
4, discharge plasma sintering
After mold installs, connection pressure is adjusted to 50MPa, and the vacuum degree in furnace is evacuated to 20Pa hereinafter, carrying out plasma discharging
Sintering obtains diffusion connection thyrite.
Sintering procedure setting is as follows：Be warming up to 1300 DEG C with the heating rate of 50 DEG C/min, protect 10min, then with 20 DEG C/
The program stopped when rate of temperature fall of min is cooled to 600 DEG C, sintering are completed, and then cool to furnace chamber temperature≤50 DEG C with the furnace, i.e.,
It can be taken off material.
Through detecting, the shearing strength of joint that the present embodiment obtains can reach 48.7MPa, middle layer with a thickness of 30 μm, in
The Vickers hardness of interbed is up to 6.0GPa.
Embodiment 3：
The Joining Technology of composite interlayer diffusion connection silicon carbide ceramics is as follows in the present embodiment：
1, the preparation of composite interlayer powder
With 59.5wt.% hydride powder (TiH2), 24.5wt.% silicon powder (Si), 13.9wt.% graphite powder (C) and
2.1wt.% aluminium powder (Al) is to pour into agate after raw material mixing to grind in alms bowl, and using absolute alcohol as abrasive media, 3h is to complete for grinding
It is complete to be uniformly mixed, it is subsequently placed in vacuum oven at 60 DEG C dry 6h, obtains composite interlayer powder；
2, welding preparation
With inner circle cutting machine by cylindric SiC ceramic materialIt is cut into the SiC ceramic disk of 3mm thickness,
Successively the surface to be welded of SiC ceramic disk is polished using 3.5 μm and 1 μm of diamond suspension polishing liquid, will be polished
SiC ceramic disk afterwards, which is put into alcoholic solution, to be cleaned by ultrasonic, and is air-dried at room temperature, and ceramic base material to be welded is obtained；
3, it assembles
By two pieces of ceramic base materials and composite interlayer powder to be welded according to graphite formed punch-Graphite pad-ceramic base material-to be welded
The assembled in sequence of composite interlayer powder-ceramic base material-Graphite pad-graphite formed punch to be welded is into graphite jig, then will assemble
The mold of completion is put into discharge plasma sintering system (SPS)；
4, discharge plasma sintering
After mold installs, connection pressure is adjusted to 50MPa, and the vacuum degree in furnace is evacuated to 20Pa hereinafter, carrying out plasma discharging
Sintering obtains diffusion connection thyrite.
Sintering procedure setting is as follows：1400 DEG C are warming up to the heating rate of 100 DEG C/min, 20min is kept the temperature, then with 20
DEG C/rate of temperature fall of min when being cooled to 600 DEG C program stopped, sintering complete, then cool to furnace chamber temperature≤50 with the furnace
DEG C, that is, it can be taken off material.
Through detecting, the shearing strength of joint that the present embodiment obtains can reach 112.5MPa, middle layer with a thickness of 40 μm, in
The Vickers hardness of interbed is up to 6.0GPa.
Embodiment 4：
The Joining Technology of composite interlayer diffusion connection silicon carbide ceramics is as follows in the present embodiment：
1, the preparation of composite interlayer powder
With 59.5wt.% hydride powder (TiH2), 24.5wt.% silicon powder (Si), 13.9wt.% graphite powder (C) and
2.1wt.% aluminium powder (Al) is to pour into agate after raw material mixing to grind in alms bowl, and using absolute alcohol as abrasive media, 3h is to complete for grinding
It is complete to be uniformly mixed, it is subsequently placed in vacuum oven at 60 DEG C dry 6h, obtains composite interlayer powder；
2, welding preparation
With inner circle cutting machine by cylindric SiC ceramic materialIt is cut into the SiC ceramic disk of 3mm thickness,
Successively the surface to be welded of SiC ceramic disk is polished using 3.5 μm and 1 μm of diamond suspension polishing liquid, will be polished
SiC ceramic disk afterwards, which is put into alcoholic solution, to be cleaned by ultrasonic, and is air-dried at room temperature, and ceramic base material to be welded is obtained；
3, it assembles
By two pieces of ceramic base materials and composite interlayer powder to be welded according to graphite formed punch-Graphite pad-ceramic base material-to be welded
The assembled in sequence of composite interlayer powder-ceramic base material-Graphite pad-graphite formed punch to be welded is into graphite jig, then will assemble
The mold of completion is put into discharge plasma sintering system (SPS)；
4, discharge plasma sintering
After mold installs, connection pressure is adjusted to 50MPa, and the vacuum degree in furnace is evacuated to 20Pa hereinafter, carrying out plasma discharging
Sintering obtains diffusion connection thyrite.
Sintering procedure setting is as follows：1450 DEG C are warming up to the heating rate of 100 DEG C/min, 10min is kept the temperature, then with 20
DEG C/rate of temperature fall of min when being cooled to 600 DEG C program stopped, sintering complete, then cool to furnace chamber temperature≤50 with the furnace
DEG C, that is, it can be taken off material.
Through detecting, the shearing strength of joint that the present embodiment obtains can reach 135.8MPa, middle layer with a thickness of 60 μm, in
The Vickers hardness of interbed is up to 12.1GPa.
Embodiment 5：
The Joining Technology of composite interlayer diffusion connection silicon carbide ceramics is as follows in the present embodiment：
1, the preparation of composite interlayer powder
With 61.2wt.% hydride powder (TiH2), 23.0wt.% silicon powder (Si), 14.7wt.% graphite powder (C) and
1.1wt.% aluminium powder (Al) is to pour into agate after raw material mixing to grind in alms bowl, and using absolute alcohol as abrasive media, 3h is to complete for grinding
It is complete to be uniformly mixed, it is subsequently placed in vacuum oven at 60 DEG C dry 6h, obtains composite interlayer powder；
2, welding preparation
With inner circle cutting machine by cylindric SiC ceramic materialIt is cut into the SiC ceramic disk of 3mm thickness,
Successively the surface to be welded of SiC ceramic disk is polished using 3.5 μm and 1 μm of diamond suspension polishing liquid, will be polished
SiC ceramic disk afterwards, which is put into alcoholic solution, to be cleaned by ultrasonic, and is air-dried at room temperature, and ceramic base material to be welded is obtained；
3, it assembles
By two pieces of ceramic base materials and composite interlayer powder to be welded according to graphite formed punch-Graphite pad-ceramic base material-to be welded
The assembled in sequence of composite interlayer powder-ceramic base material-Graphite pad-graphite formed punch to be welded is into graphite jig, then will assemble
The mold of completion is put into discharge plasma sintering system (SPS)；
4, discharge plasma sintering
After mold installs, connection pressure is adjusted to 50MPa, and the vacuum degree in furnace is evacuated to 20Pa hereinafter, carrying out plasma discharging
Sintering obtains diffusion connection thyrite.
Sintering procedure setting is as follows：1500 DEG C are warming up to the heating rate of 100 DEG C/min, 10min is kept the temperature, then with 20
DEG C/rate of temperature fall of min when being cooled to 600 DEG C program stopped, sintering complete, then cool to furnace chamber temperature≤50 with the furnace
DEG C, that is, it can be taken off material.
Through detecting, the shearing strength of joint that the present embodiment obtains can reach 86.7MPa, middle layer with a thickness of 30 μm, in
The Vickers hardness of interbed is up to 13.8GPa.
Embodiment 6：
The Joining Technology of composite interlayer diffusion connection silicon carbide ceramics is as follows in the present embodiment：
1, the preparation of composite interlayer powder
With 61.2wt.% hydride powder (TiH2), 23.0wt.% silicon powder (Si), 14.7wt.% graphite powder (C) and
1.1wt.% aluminium powder (Al) is to pour into agate after raw material mixing to grind in alms bowl, and using absolute alcohol as abrasive media, 3h is to complete for grinding
It is complete to be uniformly mixed, it is subsequently placed in vacuum oven at 60 DEG C dry 6h, obtains composite interlayer powder；
2, welding preparation
With inner circle cutting machine by cylindric SiC ceramic materialIt is cut into the SiC ceramic disk of 3mm thickness,
Successively the surface to be welded of SiC ceramic disk is polished using 3.5 μm and 1 μm of diamond suspension polishing liquid, will be polished
SiC ceramic disk afterwards, which is put into alcoholic solution, to be cleaned by ultrasonic, and is air-dried at room temperature, and ceramic base material to be welded is obtained；
3, it assembles
By two pieces of ceramic base materials and composite interlayer powder to be welded according to graphite formed punch-Graphite pad-ceramic base material-to be welded
The assembled in sequence of composite interlayer powder-ceramic base material-Graphite pad-graphite formed punch to be welded is into graphite jig, then will assemble
The mold of completion is put into discharge plasma sintering system (SPS)；
4, discharge plasma sintering
After mold installs, connection pressure is adjusted to 50MPa, and the vacuum degree in furnace is evacuated to 20Pa hereinafter, carrying out plasma discharging
Sintering obtains diffusion connection thyrite.
Sintering procedure setting is as follows：1600 DEG C are warming up to the heating rate of 50 DEG C/min, 10min is kept the temperature, then with 20
DEG C/rate of temperature fall of min when being cooled to 600 DEG C program stopped, sintering complete, then cool to furnace chamber temperature≤50 with the furnace
DEG C, that is, it can be taken off material.
Through detecting, the shearing strength of joint that the present embodiment obtains can reach 73.1MPa, middle layer with a thickness of 25 μm, in
The Vickers hardness of interbed is up to 28.1GPa.
Embodiment 7：
The Joining Technology of composite interlayer diffusion connection silicon carbide ceramics is as follows in the present embodiment：
1, the preparation of composite interlayer powder
With 61.2wt.% hydride powder (TiH2), 23.0wt.% silicon powder (Si), 14.7wt.% graphite powder (C) and
1.1wt.% aluminium powder (Al) is to pour into agate after raw material mixing to grind in alms bowl, and using absolute alcohol as abrasive media, 3h is to complete for grinding
It is complete to be uniformly mixed, it is subsequently placed in vacuum oven at 60 DEG C dry 6h, obtains composite interlayer powder；
2, welding preparation
With inner circle cutting machine by cylindric SiC ceramic materialIt is cut into the SiC ceramic disk of 3mm thickness,
Successively the surface to be welded of SiC ceramic disk is polished using 3.5 μm and 1 μm of diamond suspension polishing liquid, will be polished
SiC ceramic disk afterwards, which is put into alcoholic solution, to be cleaned by ultrasonic, and is air-dried at room temperature, and ceramic base material to be welded is obtained；
3, it assembles
By two pieces of ceramic base materials and composite interlayer powder to be welded according to graphite formed punch-Graphite pad-ceramic base material-to be welded
The assembled in sequence of composite interlayer powder-ceramic base material-Graphite pad-graphite formed punch to be welded is into graphite jig, then will assemble
The mold of completion is put into discharge plasma sintering system (SPS)；
4, discharge plasma sintering
After mold installs, connection pressure is adjusted to 30MPa, and the vacuum degree in furnace is evacuated to 20Pa hereinafter, carrying out plasma discharging
Sintering obtains diffusion connection thyrite.
Sintering procedure setting is as follows：1300 DEG C are warming up to the heating rate of 50 DEG C/min, 30min is kept the temperature, then with 10
DEG C/rate of temperature fall of min when being cooled to 600 DEG C program stopped, sintering complete, then cool to furnace chamber temperature≤50 with the furnace
DEG C, that is, it can be taken off material.
Through detecting, the shearing strength of joint that the present embodiment obtains can reach 95.2MPa, middle layer with a thickness of 100 μm, in
The Vickers hardness of interbed is up to 5.5GPa.
Embodiment result is summarized：
The present invention is generated by mixed-powder reaction in-situ by silicon titanium-carbide (Ti3SiC2), silicon carbide (SiC) and carbonization
The composite interlayer of titanium (TiC) composition, while obtaining the silicon carbide connector haveing excellent performance.Composite interlayer possesses and silicon carbide
Physical and chemical properties similar in base material, similar thermal expansion coefficient between the two have good composite effect.It is remaining in connector
Stress is lower, and crackle is less.By adjusting hydride powder (TiH in raw material powder2), silicon powder (Si), graphite powder (C) and aluminium powder
(Al) proportion and suitable technological parameter, control the composition and distribution of conversion zone, reach the effect for improving joint performance
Fruit.In 1400-1450 DEG C of preferable temperature, connector excellent connecting effect.At this time by silicon titanium-carbide (Ti in connector3SiC2), carbon
SiClx (SiC) and titanium carbide (TiC) composition, due to the two-phase humidification of silicon carbide (SiC) and titanium carbide (TiC), connector
Bonding strength is higher.The present invention can prepare high-intensitive silicon carbide ceramics connector, and the engineering for solving silicon carbide ceramics is answered
One technical problem.
Claims (10)
1. a kind of for spreading the composite interlayer of connection silicon carbide ceramics, it is characterised in that its raw material is constituted by mass percentage
It is as follows：
High-purity hydride powder 55-65wt.%, high-purity silicon powder 20-25wt.%, high purity graphite powder 12-17wt.%, high purity aluminum powder 1-
3wt.%.
2. composite interlayer according to claim 1, it is characterised in that：
The purity of high-purity hydride powder>99%, granularity<25μm；The purity of the high-purity silicon powder>98%, granularity<40μm；
The purity of the high purity graphite powder>99%, granularity<5μm；The purity of the high purity aluminum powder>98%, granularity<100μm.
3. a kind of Joining Technology of composite interlayer diffusion connection silicon carbide ceramics of any of claims 1 or 2, it is characterised in that
Include the following steps：
Step 1：The preparation of composite interlayer powder
Amount weighs high-purity hydride powder, high-purity silicon powder, high purity graphite powder and high purity aluminum powder according to the ratio, pours into agate after mixing and grinds
It grinds in alms bowl, using absolute alcohol as abrasive media, grinds 1-3h to being mixed thoroughly, be subsequently placed at drying in vacuum oven,
Obtain composite interlayer powder；
Step 2：Welding preparation
SiC ceramic material is cut into SiC ceramic block with inner circle cutting machine, using polishing fluid to the to be welded of SiC ceramic block
Connect surface to be polished, the SiC ceramic block after polishing be put into alcoholic solution and is cleaned by ultrasonic, is air-dried at room temperature, obtain to
Weld ceramic base material；
Step 3：Assembly
Two pieces of ceramic base materials and composite interlayer powder to be welded are compound according to graphite formed punch-Graphite pad-ceramic base material-to be welded
The assembled in sequence of middle layer powder-ceramic base material-Graphite pad-graphite formed punch to be welded is completed into graphite jig, then by assembly
Mold be put into discharge plasma sintering system；
Step 4：Discharge plasma sintering
After mold installs, connection pressure is adjusted to 20-60MPa, and the vacuum degree in furnace is evacuated to 20Pa hereinafter, carrying out plasma discharging burning
Knot obtains diffusion connection thyrite.
4. Joining Technology according to claim 3, it is characterised in that：
In step 1, drying temperature is 60 DEG C, drying time >=6h.
5. Joining Technology according to claim 3, it is characterised in that：
In step 2, the polishing fluid is 1-3.5 μm of diamond suspension polishing liquid.
6. Joining Technology according to claim 5, it is characterised in that：
Successively the surface to be welded of SiC ceramic block is polished using 3.5 μm and 1 μm of diamond suspension polishing liquid.
7. Joining Technology according to claim 3, it is characterised in that：
In step 4, sintering temperature is 1200-1600 DEG C, soaking time 5-30min.
8. Joining Technology according to claim 3, it is characterised in that：
In step 4, sintering temperature is 1400-1450 DEG C.
9. Joining Technology according to claim 3, it is characterised in that：
In step 4, when sintering, heating rate is set as 50-100 DEG C/min；Rate of temperature fall is set as 10-20 DEG C/min, cooling
Program stopped when to 600 DEG C, sintering are completed, then cool to temperature≤50 DEG C with the furnace, that is, can be taken off material.
10. Joining Technology according to claim 3, it is characterised in that：
In step 4, the articulamentum of the diffusion connection thyrite obtained after sintering is with a thickness of 20-100 μm.
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