CN110330356B - Silicon carbide ceramic brazing connection method - Google Patents
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- CN110330356B CN110330356B CN201910641620.6A CN201910641620A CN110330356B CN 110330356 B CN110330356 B CN 110330356B CN 201910641620 A CN201910641620 A CN 201910641620A CN 110330356 B CN110330356 B CN 110330356B
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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
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/3601—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with inorganic compounds as principal constituents
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
- C04B2237/10—Glass interlayers, e.g. frit or flux
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
- C04B2237/32—Ceramic
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- C04B2237/365—Silicon carbide
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Abstract
A silicon carbide ceramic brazing connection method relates to a silicon carbide ceramic brazing connection method. The invention aims to solve the problems of poor wettability, large residual stress, smaller weldable workpiece and the like of the metal brazing filler metal in the traditional brazing method. The method comprises the following steps: mixing Al2O3、SiO2And CaO or CaCO3Mixing, grinding, drying, melting, water quenching, grinding, sieving and drying to obtain the microcrystalline glass solder; pretreating the silicon carbide ceramic to be brazed to obtain pretreated silicon carbide ceramic; uniformly mixing the microcrystalline glass brazing filler metal and the binder, and coating the mixture between the pretreated silicon carbide ceramics to obtain a to-be-welded connecting piece of the silicon carbide ceramics; and brazing the to-be-brazed connecting piece of the silicon carbide ceramic, and then cooling along with the furnace to obtain the brazed and connected silicon carbide ceramic. The invention can obtain a silicon carbide ceramic brazing connection method.
Description
Technical Field
The invention relates to a method for brazing connection of silicon carbide ceramics.
Background
The silicon carbide ceramic is a high-temperature structural material with great development prospect, and has the characteristics of high bending strength, oxidation resistance, corrosion resistance, wear resistance, low friction coefficient and the like in addition to excellent high-temperature mechanical properties (strength, creep resistance and the like). In the field of aviation and aerospace engines, silicon carbide ceramics are widely applied in order to meet the requirements of weight reduction and high-temperature stable operation of high-performance engines. Currently, silicon carbide ceramics can be joined by mechanical joining, bonding, fusion welding, brazing, diffusion welding, and the like.
The high-reliability connection of the silicon carbide ceramics has more difficulties, and the problems of physical property mismatch and metallurgical incompatibility with welding materials are often caused by the hardness, brittleness, high melting point, small linear expansion coefficient and covalent bond type of the silicon carbide ceramics. The traditional brazing method has the problems of poor wettability of metal brazing filler metal, large residual stress, small weldable workpiece and the like.
Disclosure of Invention
The invention aims to solve the problems of poor wettability, large residual stress, smaller weldable workpiece and the like of a metal solder in the traditional brazing method, and provides a silicon carbide ceramic brazing connection method.
A silicon carbide ceramic brazing connection method comprises the following steps:
firstly, according to mass fraction Al2O3 12%~15%、SiO252 to 63 percent and the balance of CaO or CaCO3Respectively weighing Al2O3、SiO2And CaO or CaCO3；
Secondly, Al weighed in the step one2O3、SiO2And CaO or CaCO3Mixing, grinding by a wet grinding method, and drying; melting after drying, then performing water quenching, grinding by adopting a wet grinding method after water quenching, sieving after grinding, and then drying to obtain the microcrystalline glass solder;
thirdly, preprocessing the silicon carbide ceramic to be brazed to obtain preprocessed silicon carbide ceramic;
fourthly, uniformly mixing the microcrystalline glass brazing filler metal obtained in the second step with a binder, and uniformly coating the mixture among the pretreated silicon carbide ceramics obtained in the third step to obtain a to-be-welded silicon carbide ceramic connecting piece;
fifthly, carrying out brazing treatment on the to-be-welded connecting piece of the silicon carbide ceramic obtained in the fourth step, and then cooling along with the furnace to obtain the silicon carbide ceramic after brazing connection.
The invention has the beneficial effects that:
1. the invention relates to a silicon carbide ceramic brazing connection method, which aims to realize reliable connection of silicon carbide components in the nuclear industry, designs and prepares a glass brazing filler metal for brazing in an air environment, and solves the problem of poor wettability of a metal brazing filler metal in the traditional brazing method; the silicon carbide ceramics are connected in the air environment, so that the problem that a weldable workpiece is small due to the limitation of vacuum brazing equipment is solved; coefficient of thermal expansion (α =4.31 × 10) of the glass filler metal used-6K-1) Matching with silicon carbide ceramic, canResidual internal stress of the soldered joint can be effectively reduced;
2. according to the silicon carbide ceramic brazing connection method, the components of the glass brazing filler metal are reasonably selected, the corresponding designed welding process is designed, a welding joint which is free of air holes, compact in structure and high in strength can be formed, the process method is simple, vacuum equipment and surface treatment are not needed, effective connection of the silicon carbide ceramic can be achieved in the atmospheric environment, and therefore cost is reduced, the silicon carbide ceramic brazing connection method is suitable for industrial production, and has a good industrial application prospect.
The invention can obtain a silicon carbide ceramic brazing connection method.
Drawings
Fig. 1 is an SEM topography of a brazed joint of silicon carbide ceramic obtained in accordance with an eleventh embodiment after brazing.
Detailed Description
The first embodiment is as follows: the silicon carbide ceramic brazing connection method in the embodiment is completed according to the following steps:
firstly, according to mass fraction Al2O3 12%~15%、SiO252 to 63 percent and the balance of CaO or CaCO3Respectively weighing Al2O3、SiO2And CaO or CaCO3；
Secondly, Al weighed in the step one2O3、SiO2And CaO or CaCO3Mixing, grinding by a wet grinding method, and drying; melting after drying, then performing water quenching, grinding by adopting a wet grinding method after water quenching, sieving after grinding, and then drying to obtain the microcrystalline glass solder;
thirdly, preprocessing the silicon carbide ceramic to be brazed to obtain preprocessed silicon carbide ceramic;
fourthly, uniformly mixing the microcrystalline glass brazing filler metal obtained in the second step with a binder, and uniformly coating the mixture among the pretreated silicon carbide ceramics obtained in the third step to obtain a to-be-welded silicon carbide ceramic connecting piece;
fifthly, carrying out brazing treatment on the to-be-welded connecting piece of the silicon carbide ceramic obtained in the fourth step, and then cooling along with the furnace to obtain the silicon carbide ceramic after brazing connection.
The beneficial effects of the embodiment are as follows:
1. the embodiment provides a silicon carbide ceramic brazing connection method, aims to realize reliable connection of silicon carbide components in the nuclear industry, designs and prepares a glass brazing filler metal for brazing in an air environment, and solves the problem of poor wettability of a metal brazing filler metal in the traditional brazing method; the silicon carbide ceramics are connected in the air environment, so that the problem that a weldable workpiece is small due to the limitation of vacuum brazing equipment is solved; coefficient of thermal expansion (α =4.31 × 10) of the glass filler metal used-6K-1) The residual internal stress of the soldered joint can be effectively reduced by matching with the silicon carbide ceramic;
2. according to the silicon carbide ceramic brazing connection method, through reasonable selection of glass brazing filler metal components and design of a corresponding designed welding process, a welding joint which is free of air holes, compact in structure and high in strength can be formed, the process method is simple, vacuum equipment and surface treatment are not needed, effective connection of silicon carbide ceramic can be achieved in the atmospheric environment, and therefore cost is reduced, the silicon carbide ceramic brazing connection method is suitable for industrial production and has a good industrial application prospect.
The second embodiment is as follows: the present embodiment differs from the present embodiment in that: in the step one, Al is mixed according to mass fraction2O3 14.7%、SiO262% and CaO23.3%, or Al2O3 12.4%、SiO252.4% and CaCO3 35.2% of Al was weighed separately2O3、SiO2And CaO or CaCO3 。
Other steps are the same as those in the first embodiment.
The third concrete implementation mode: the first or second differences from the present embodiment are as follows: the two-position wet grinding method in the second step comprises the following steps: using absolute ethyl alcohol as medium to mix Al2O3、SiO2And CaO or CaCO3Mechanically ball-milling at the rotating speed of 550rpm for 8-10 h, wherein the mass ratio of ball materials is 2: 1.
the other steps are the same as those in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: and the drying treatment in the step two is heat preservation for 1 to 1.5 hours at the temperature of between 100 and 120 ℃, the melting is heat preservation for 1.5 to 2 hours at the temperature of 1600 ℃, and the sieving is performed by a 325-mesh sieve.
The other steps are the same as those in the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the pretreatment in the third step comprises the following steps: cutting and molding the silicon carbide ceramic to be brazed, firstly ultrasonically cleaning the silicon carbide ceramic for 5-10 min by absolute ethyl alcohol, drying the silicon carbide ceramic after ultrasonic cleaning, then polishing the silicon carbide ceramic to be smooth in surface by a sand disc, ultrasonically cleaning the silicon carbide ceramic for 5-10 min by acetone, and finally drying the silicon carbide ceramic to obtain the pretreated silicon carbide ceramic.
The other steps are the same as those in the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is as follows: the drying is carried out at the temperature of 100-120 ℃ for 1-1.5 h.
The other steps are the same as those in the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the mass ratio of the microcrystalline glass solder to the binder in the fourth step is 1: 4 to 6.
The other steps are the same as those in the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: the thickness of the coating in the fourth step is 20 μm to 200 μm.
The other steps are the same as those in the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: the adhesive in the fourth step is terpineol.
The other steps are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is as follows: the brazing treatment in the fifth step comprises the following steps: and heating the to-be-welded connecting piece of the silicon carbide ceramic obtained in the fourth step to 250-350 ℃ at a heating rate of 1-10 ℃/min, preserving heat at 250-350 ℃ for 0.5-2 h, heating to 1000 ℃ at a heating rate of 1-10 ℃/min, heating to 1300-1600 ℃ at a heating rate of 1-5 ℃/min, and preserving heat at 1300-1600 ℃ for 5-80 min.
The other steps are the same as those in the first to ninth embodiments.
The following embodiments were used to demonstrate the beneficial effects of the present invention:
the concrete implementation mode eleven: a silicon carbide ceramic brazing connection method comprises the following steps:
firstly, according to mass fraction Al2O3 14.7%、SiO2Al is weighed according to the proportion of 62 percent and 23.3 percent of CaO respectively2O3、SiO2And CaO;
secondly, Al weighed in the step one2O3、SiO2Mixing with CaO, grinding by a wet grinding method, and then placing in a muffle furnace for heat preservation for 1h at 120 ℃ for drying treatment; and (3) after drying, placing the mixture in an alumina crucible, preserving heat for 2h at 1600 ℃, melting, clamping the crucible by using crucible tongs, and then pouring molten glass into water for water quenching to obtain broken glass particles. Grinding the glass broken particles by a wet grinding method, sieving the ground glass broken particles by a 325-mesh sieve to obtain glass powder with the particle size of less than 47 mu m, and then preserving heat at 120 ℃ for 1h for drying treatment to obtain the microcrystalline glass solder;
the two-position wet grinding method in the second step comprises the following steps: grinding balls with different sizes and absolute ethyl alcohol are used as a medium to mix the mixed Al2O3、SiO2And CaO or CaCO3Mechanically ball-milling for 10 hours at the rotating speed of 550rpm, wherein the mass ratio of ball materials is 2: 1;
thirdly, cutting and forming the silicon carbide ceramic to be brazed by using a diamond inner circle cutting machine, ultrasonically cleaning the silicon carbide ceramic for 10min by absolute ethyl alcohol, placing the silicon carbide ceramic in a muffle furnace for drying after ultrasonic cleaning, preserving heat for 1h at 120 ℃, polishing by a No. 400 sand table to remove surface stains and ensure the consistency of the surface state, ultrasonically cleaning the silicon carbide ceramic for 10min by acetone, and finally preserving heat for 1h at 120 ℃ for drying to obtain the pretreated silicon carbide ceramic;
fourthly, uniformly mixing the microcrystalline glass brazing filler metal obtained in the second step with terpineol to prepare soldering paste, and uniformly coating the soldering paste between the upper test piece and the lower test piece of the pretreated silicon carbide ceramic obtained in the third step to obtain a to-be-welded connecting piece of the silicon carbide ceramic;
the mass ratio of the microcrystalline glass solder to the terpineol in the fourth step is 1: 5, the coating thickness is 100 μm;
fifthly, placing the to-be-welded connecting piece of the silicon carbide ceramic obtained in the fourth step in a muffle furnace, heating to 300 ℃ at a heating rate of 10 ℃/min, preserving heat for 1h at 300 ℃, then heating to 1000 ℃ at a heating rate of 10 ℃/min, heating to 1400 ℃ at a heating rate of 5 ℃/min, preserving heat for 10min at 1400 ℃, and finally cooling along with the furnace to obtain the silicon carbide ceramic after brazing connection.
As shown in fig. 1, the silicon carbide ceramic after brazing connection obtained in the present embodiment has a welded joint that is free of air holes and has a dense structure, and the joint shear strength at room temperature of the silicon carbide ceramic after brazing connection is 56MPa as measured.
The specific implementation mode twelve: a silicon carbide ceramic brazing connection method comprises the following steps:
firstly, according to mass fraction Al2O3 12.4%、SiO252.4% and CaCO3 35.2% of Al was weighed separately2O3、SiO2And CaCO3；
Secondly, Al weighed in the step one2O3、SiO2And CaCO3Mixing, grinding by a wet grinding method, and then placing in a muffle furnace for heat preservation for 1h at 120 ℃ for drying treatment; and (3) after drying, placing the mixture in an alumina crucible, preserving heat for 2h at 1600 ℃, melting, clamping the crucible by using crucible tongs, and then pouring molten glass into water for water quenching to obtain broken glass particles. Grinding the glass broken particles by a wet grinding method, sieving the ground glass broken particles with a 325-mesh sieve to obtain glass powder with the particle size of less than 47 mu m, and preserving heat at 120 ℃ for 1h, drying to obtain the microcrystalline glass brazing filler metal;
the two-position wet grinding method in the second step comprises the following steps: grinding balls with different sizes are adopted, and the mass ratio of the ball materials is 2: 1, absolute ethyl alcohol is used as a medium for mixing Al2O3、SiO2And CaO or CaCO3Mechanically ball-milling at the rotating speed of 550rpm for 10 hours;
thirdly, cutting and forming the silicon carbide ceramic to be brazed by using a diamond inner circle cutting machine, ultrasonically cleaning the silicon carbide ceramic for 10min by absolute ethyl alcohol, placing the silicon carbide ceramic in a muffle furnace for drying after ultrasonic cleaning, preserving heat for 1h at 120 ℃, polishing by a No. 400 sand table to remove surface stains and ensure the consistency of the surface state, ultrasonically cleaning the silicon carbide ceramic for 10min by acetone, and finally preserving heat for 1h at 120 ℃ for drying to obtain the pretreated silicon carbide ceramic;
fourthly, uniformly mixing the microcrystalline glass brazing filler metal obtained in the second step with terpineol to prepare soldering paste, and uniformly coating the soldering paste between the upper test piece and the lower test piece of the pretreated silicon carbide ceramic obtained in the third step to obtain a to-be-welded connecting piece of the silicon carbide ceramic;
the mass ratio of the microcrystalline glass solder to the terpineol in the fourth step is 1: 4-6, the coating thickness is 20-200 μm;
fifthly, placing the to-be-welded connecting piece of the silicon carbide ceramic obtained in the fourth step in a muffle furnace, heating to 300 ℃ at a heating rate of 10 ℃/min, preserving heat at 300 ℃ for 1h, then heating to 1000 ℃ at a heating rate of 10 ℃/min, heating to 1500 ℃ at a heating rate of 5 ℃/min, preserving heat at 1500 ℃ for 10min, and finally cooling along with the furnace to obtain the silicon carbide ceramic after brazing connection.
Through testing, the room-temperature shear strength of the joint of the silicon carbide ceramic after brazing connection reaches 50 MPa.
Claims (6)
1. The silicon carbide ceramic brazing connection method is characterized by comprising the following steps:
firstly, according to mass fraction Al2O3 14.7％、SiO262% and CaO23.3%, or Al2O3 12.4％、SiO252.4% and CaCO335.2% of Al was weighed separately2O3、SiO2And CaO or CaCO3；
Secondly, Al weighed in the step one2O3、SiO2And CaO or CaCO3Mixing, grinding by a wet grinding method, and drying; after drying treatment, preserving heat for 1.5-2 h at 1600 ℃, then performing water quenching, grinding by a wet grinding method after water quenching, sieving after grinding, and then performing drying treatment to obtain the microcrystalline glass solder;
thirdly, preprocessing the silicon carbide ceramic to be brazed to obtain preprocessed silicon carbide ceramic;
fourthly, uniformly mixing the microcrystalline glass solder obtained in the second step with a binder, and uniformly coating the mixture between the pretreated silicon carbide ceramics obtained in the third step to obtain a to-be-welded silicon carbide ceramic connecting piece, wherein the mass ratio of the microcrystalline glass solder to the binder is 1: 4-6, the coating thickness is 20-200 μm;
fifthly, heating the to-be-welded connecting piece of the silicon carbide ceramic obtained in the fourth step to 250-350 ℃ at a heating rate of 1-10 ℃/min, preserving heat at 250-350 ℃ for 0.5-2 h, heating to 1000 ℃ at a heating rate of 1-10 ℃/min, heating to 1300-1600 ℃ at a heating rate of 1-5 ℃/min, preserving heat at 1300-1600 ℃ for 5-80 min, and cooling along with the furnace to obtain the silicon carbide ceramic after braze welding.
2. The method of claim 1, wherein the wet grinding in step two comprises the steps of: using absolute ethyl alcohol as medium to mix Al2O3、SiO2And CaO or CaCO3Mechanically ball-milling at the rotating speed of 550rpm for 8-10 h, wherein the mass ratio of ball materials is 2: 1.
3. the method of claim 1, wherein the step two of drying comprises holding the substrate at 100-120 ℃ for 1-1.5 hours, and the step of screening comprises screening with a 325-mesh screen.
4. The method of claim 1, wherein the step of pretreating in step three comprises: cutting and molding the silicon carbide ceramic to be brazed, firstly ultrasonically cleaning the silicon carbide ceramic for 5-10 min by absolute ethyl alcohol, drying the silicon carbide ceramic after ultrasonic cleaning, then polishing the silicon carbide ceramic to be smooth in surface by a sand disc, ultrasonically cleaning the silicon carbide ceramic for 5-10 min by acetone, and finally drying the silicon carbide ceramic to obtain the pretreated silicon carbide ceramic.
5. The silicon carbide ceramic brazing connection method according to claim 4, wherein the drying is performed for 1-1.5 hours at a temperature of 100-120 ℃.
6. The method of claim 1, wherein the binder in step four is terpineol.
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| CN112299869B (en) * | 2020-10-28 | 2021-08-31 | 中国科学院上海硅酸盐研究所 | Laser welding method for silicon carbide and composite material thereof |
| CN112851389B (en) * | 2021-04-14 | 2022-03-15 | 哈尔滨工业大学 | Method for connecting SiC ceramic material by using calcium oxide/aluminum oxide/silicon dioxide/lithium oxide glass solder |
| CN114043027B (en) * | 2021-11-12 | 2024-01-12 | 哈尔滨工业大学 | Fusion leaching sintering welding method |
| CN114195542A (en) * | 2022-01-06 | 2022-03-18 | 哈尔滨工业大学 | Method for connecting silicon carbide ceramic by using microcrystalline glass solder for in-situ generation of anorthite |
| CN114892262A (en) * | 2022-05-20 | 2022-08-12 | 贵州省紫安新材料科技有限公司 | Spliced carbon heat-preservation cylinder and manufacturing method thereof |
| CN115322006A (en) * | 2022-09-13 | 2022-11-11 | 哈尔滨工业大学 | Method for connecting silicon nitride ceramic composite structure by using glass solder |
| CN115894063B (en) * | 2022-11-30 | 2023-08-04 | 广东工业大学 | Silicon carbide ceramic connection method and silicon carbide heat exchange tube manufactured by same |
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