CN115925266A - Method for connecting silicon carbide ceramics by cordierite microcrystalline glass solder - Google Patents
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- CN115925266A CN115925266A CN202211533777.5A CN202211533777A CN115925266A CN 115925266 A CN115925266 A CN 115925266A CN 202211533777 A CN202211533777 A CN 202211533777A CN 115925266 A CN115925266 A CN 115925266A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Abstract
A method for connecting silicon carbide ceramics by using cordierite microcrystalline glass solder relates to a method for connecting silicon carbide ceramics by using microcrystalline glass solder. The invention aims to solve the technical problems that the existing microcrystalline glass solder has higher thermal expansion coefficient and is not suitable for connecting ceramics with low thermal expansion coefficient such as silicon carbide and the like. The invention develops a Yb 2 O 3 ‑MgO‑Al 2 O 3 ‑SiO 2 The microcrystalline glass solder and the technology for connecting the microcrystalline glass solder and the silicon carbide ceramic form a microcrystalline glass connecting layer through crystallization reaction in the welding thermal cycle process, and on one hand, the microcrystalline glass solder can improve the quality of glassSoftening temperature, thereby improving the high-temperature stability thereof; on the other hand, the thermal expansion coefficient can be adjusted and controlled to match with the parent metal by controlling the crystallization behavior of the glass, and the average thermal expansion coefficient is 3.78 multiplied by 10 ‑6 The temperature per DEG C, improves the residual stress of the joint, has the shear strength of 70-80 MPa, and realizes the reliable connection of the joint under the non-pressure condition.
Description
Technical Field
The invention relates to a method for connecting silicon carbide ceramics by using a microcrystalline glass solder.
Background
With the progress of modern science and technology, nuclear energy is developed as a clean renewable energy source to solve the problems of resource crisis, environmental pollution and the like. In 2011, nuclear power station accidents occurred in fukushima of japan, and people turned nuclear fuel cladding tube materials from traditional zirconium alloy materials to silicon carbide (SiC) materials with higher safety, such as bulk silicon carbide ceramics or silicon carbide fiber reinforced silicon carbide ceramics (SiC) f /SiC) composite material. The silicon carbide has the advantages of high melting point (2370 ℃), good wear resistance, excellent high-temperature mechanical property, low reactivity with water vapor, low neutron absorption cross section (0.12 target-en), irradiation dimensional stability, corrosion resistance and the like, is listed as a nuclear fuel cladding candidate material with wide application prospect, and can improve the safety of a reactor. The structural materials used in nuclear reactors are generally large in size, complex in shape and harsh in service environments. Wherein the shell and end caps of the core fuel clad require suitable joining techniques to ensure their hermeticity. If the silicon carbide ceramic and the composite material thereof are applied to the engineering of the cladding structure, the connection sealing technology is inevitably involved. Due to the strong covalent bond bonding characteristic of the silicon carbide, the silicon carbide is endowed with high chemical stability and excellent performance, and simultaneously brings the characteristics of large brittleness, high melting point, slow self-diffusion and the like of the material, and the actual engineering requirements of components with complex shapes are difficult to meet by adopting the traditional fusion welding and diffusion welding technology and the machining forming method.
In the ceramic connection technology, glass and ceramic have excellent chemical compatibility, and the adjustable thermal expansion coefficient and low cost enable the glass solder to become an optional material for connecting ceramic materials, and a microcrystalline glass connection layer is formed through crystallization reaction in the connection process, so that the effects of adjusting the thermal expansion coefficient of the connection layer and improving high temperature resistance can be achieved.
Disclosure of Invention
The invention provides a method for connecting silicon carbide ceramics by using cordierite microcrystalline glass solder, aiming at solving the technical problems that the conventional microcrystalline glass solder has higher thermal expansion coefficient and is not suitable for connecting low-thermal expansion coefficient ceramics such as silicon carbide and the like.
The method for connecting the silicon carbide ceramics by the cordierite microcrystalline glass solder comprises the following steps:
1. weighing 4 raw material powders according to the following mass percentage: 5.7 to 20.7 percent of MgO and Al 2 O 3 17.8% by mass of Yb 2 O 3 0-15% of SiO 2 The mass percentage content of (A) is 61.5%; then ball-milling and mixing the weighed 4 raw material powders, putting the mixture into a crucible, and carrying out high-temperature melting at the smelting temperature of 1550-1600 ℃ for 2-2.5 h to obtain glass melt with uniform components;
2. pouring molten glass into deionized water for water quenching, taking out from the water to obtain broken glass slag, drying and performing ball milling treatment to obtain fine glass powder, and sieving the glass powder to remove uncrushed glass blocks to obtain glass solder;
3. grinding and polishing the to-be-connected surface of the ceramic base material: carrying out surface grinding and polishing treatment by adopting diamond grinding paste with the diameter of 1 mu m to obtain a surface to be connected, then placing the base material in alcohol for ultrasonic cleaning for 15-20 min, and drying for later use; the ceramic base material is bulk silicon carbide ceramic or SiC f a/SiC composite ceramic;
4. putting the glass solder prepared in the step two into a tabletting mold to be pressed into a sheet shape with the thickness of 0.1-0.5 mm, and then putting the sheet into a sandwich structure between two ceramic base materials;
5. and (3) placing the assembled sandwich structure in an atmosphere furnace, realizing non-pressure connection under the condition of inert atmosphere, heating to 1320-1380 ℃, preserving heat for 10-15 min, and cooling along with the furnace to finish the whole connection process.
The invention develops a Yb 2 O 3 -MgO-Al 2 O 3 -SiO 2 (YbMAS) glass-ceramic solder andthe technology of connecting the silicon carbide ceramic can form a microcrystalline glass connecting layer through crystallization reaction in the welding thermal cycle process, so that the softening temperature of glass can be improved, and the high-temperature stability of the glass is improved; on the other hand, the thermal expansion coefficient of the glass can be regulated and controlled to be matched with the base material by controlling the crystallization behavior of the glass, so that the residual stress of the joint is improved, and the joint can be reliably connected under the non-pressure condition.
The invention has the following beneficial effects:
the invention adopts Yb 2 O 3 -MgO-Al 2 O 3 -SiO 2 The glass solder realizes the connection of silicon carbide ceramics at 1320-1380 ℃, a microstructure which takes a microcrystalline glass phase as a main part is formed in the center of a welding seam, and the average thermal expansion coefficient is 3.78 multiplied by 10 -6 /. Degree.C., matching the base material (the coefficient of thermal expansion of the silicon carbide ceramic is 4X 10) -6 /° c). The crystals are mainly cordierite (Mg) 2 Al 4 Si 5 O 18 ) And the formed welding line is compact and has no defects such as air holes and cracks, and the influence of the defects on the strength and the air tightness of the joint is avoided. The silicon carbide ceramic connecting joint obtained by the invention is reliable in connection, the shear strength reaches 70-80 MPa, the connection of the silicon carbide ceramic cladding tube and the end plug is realized, and the technical support is further provided for the application of silicon carbide in the nuclear fuel cladding tube.
Drawings
FIG. 1 is a graph of the thermal expansion of a microcrystalline glass solder in test one;
FIG. 2 is a photograph of the microstructure of a typical joint formed by joining a glass-ceramic to a silicon carbide ceramic in test one;
FIG. 3 is an XRD pattern of the weld of trial one;
FIG. 4 test five SiC f The assembly of the/SiC ceramic pipe and the SiC end plug is shown schematically;
fig. 5 is a photograph of the assembled real object after the five tests.
Detailed Description
The first embodiment is as follows: the embodiment is a method for connecting silicon carbide ceramics by cordierite microcrystalline glass solder, which is specifically carried out according to the following steps:
1. weighing 4 raw material powders according to the following mass percentages: 5.7 to 20.7 percent of MgO and Al 2 O 3 17.8% by mass of Yb 2 O 3 0-15% of SiO 2 The mass percentage content of (A) is 61.5%; then ball-milling and mixing the weighed 4 raw material powders, putting the mixture into a crucible, and carrying out high-temperature melting at the smelting temperature of 1550-1600 ℃ for 2-2.5 h to obtain glass melt with uniform components;
2. pouring molten glass into deionized water for water quenching, taking out from the water to obtain broken glass slag, drying and performing ball milling treatment to obtain fine glass powder, and sieving the glass powder to remove uncrushed glass blocks to obtain glass solder;
3. grinding and polishing the to-be-connected surface of the ceramic base material: carrying out surface grinding and polishing treatment by adopting diamond grinding paste with the diameter of 1 mu m to obtain a surface to be connected, then placing the base material in alcohol for ultrasonic cleaning for 15-20 min, and drying for later use; the ceramic base material is bulk silicon carbide ceramic or SiC f a/SiC composite ceramic;
4. putting the glass solder prepared in the step two into a tabletting mold to be pressed into a sheet shape with the thickness of 0.1-0.5 mm, and then putting the sheet into a sandwich structure between two ceramic base materials;
5. and (3) placing the assembled sandwich structure in an atmosphere furnace, realizing non-pressure connection under the condition of inert atmosphere, heating to 1320-1380 ℃, preserving heat for 10-15 min, and cooling along with the furnace to finish the whole connection process.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: in the first step, the mass percentage of MgO is 15.7 percent, and Al is 2 O 3 17.8% by mass of Yb 2 O 3 Is 5 percent by mass, siO 2 The mass percentage of (B) is 61.5%. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: in the first step, the smelting temperature is 1550 ℃, and the temperature is kept for 2h. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode is as follows: the difference between this embodiment mode and one of the first to third embodiment modes is: and ball milling for 12h in the step one. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the fourth difference between this embodiment and the specific embodiment is that: and in the second step, the mixture is sieved by a 300-mesh sieve. The rest is the same as the fourth embodiment.
The sixth specific implementation mode: the fifth embodiment is different from the fifth embodiment in that: ultrasonic cleaning for 15min in the third step. The rest is the same as the fifth embodiment.
The seventh embodiment: the sixth embodiment is different from the sixth embodiment in that: and step four, putting the glass solder prepared in the step two into a tabletting mold to be pressed into a 0.2mm sheet. The rest is the same as the sixth embodiment.
The specific implementation mode is eight: the seventh embodiment is different from the seventh embodiment in that: and fifthly, the inert atmosphere is argon. The rest is the same as the seventh embodiment.
The specific implementation method nine: the eighth embodiment is different from the eighth embodiment in that: and step five, heating to 1340 ℃ and preserving the temperature for 10-15 min. The rest is the same as in the eighth embodiment.
The specific implementation mode is ten: the ninth embodiment differs from the ninth embodiment in that: and step five, heating to 1340 ℃ and preserving the heat for 10min. The rest is the same as in the ninth embodiment.
The invention was verified with the following tests:
test one: the test is a method for connecting silicon carbide ceramics by cordierite microcrystalline glass solder, and is specifically carried out according to the following steps:
1. weighing 4 raw material powders according to the following mass percentages: 15.7 percent of MgO and Al 2 O 3 17.8% by mass of Yb 2 O 3 Is 5 percent by mass, siO 2 The mass percentage content of (A) is 61.5%; then the 4 kinds of raw material powder are weighed and processedBall-milling and mixing for 12h, putting into a crucible, and carrying out high-temperature melting at 1550 ℃ for 2h to obtain glass melt with uniform components;
2. pouring molten glass into deionized water for water quenching, taking out from the water to obtain broken glass slag, drying and performing ball milling treatment to obtain fine glass powder, and screening the glass powder through a 300-mesh sieve to remove unbroken glass blocks to obtain glass solder;
test of coefficient of thermal expansion of glass solder: placing the glass solder in an atmosphere furnace, heating to 1340 deg.C under argon gas condition, holding for 10min, cooling with the furnace, measuring its thermal expansion coefficient curve, and the result is shown in FIG. 1, which is that the thermal expansion coefficient is 3.78 × 10 -6 /° C, and is matched with the base material (the thermal expansion coefficient of the silicon carbide ceramic is 4 x 10) -6 /℃)。
3. Grinding and polishing the to-be-connected surface of the ceramic base material: carrying out surface grinding and polishing treatment by adopting diamond grinding paste with the diameter of 1 mu m to obtain a surface to be connected, then placing the base material in alcohol for ultrasonic cleaning for 15min, and drying for later use; the ceramic base material is two block silicon carbide ceramics;
4. putting the glass solder prepared in the step two into a tabletting mold, pressing into a 0.2mm sheet shape, and then placing between two ceramic base materials to form a sandwich structure;
5. and (3) placing the assembled sandwich structure in an atmosphere furnace, realizing pressureless connection under the argon condition, heating to 1340 ℃, preserving the temperature for 10min, cooling along with the furnace, and completing the whole connection process, wherein the obtained joint microstructure is shown in figure 2, and the joint microstructure is complete and has no obvious defect.
Fig. 3 is an XRD pattern of the weld of the first test, from which it can be seen that two crystal phases can be detected in the glass-ceramic obtained after the glass solder is subjected to the joining treatment of heat preservation at 1340 ℃ for 10min. The main precipitated phase is cordierite (Mg) 2 Al 4 Si 5 O 18 PDF # 97-008-6344), having a hexagonal lattice structure with the lattice parameters:
α =90 °, β =90 °, γ =120 °; the other precipitated phase is enstatite (MgSiO) 3 PDF # 97-003-4074).
And evaluating the performance of the joint in the first test by adopting the compressive shear strength to obtain the joint with the room-temperature shear strength of 80MPa.
And (2) test II: this test differs from the test one in that: in the first step, the mass percentage of MgO is 20.7 percent, and Al is 2 O 3 Is 17.8 percent by mass, siO 2 The mass percentage of (B) is 61.5%. The rest were the same as in test one.
And evaluating the joint performance of the second test by adopting the compressive shear strength, wherein the room-temperature shear strength of the obtained joint is 72MPa.
And (3) testing three: this test differs from the test one in that: 10.7 percent of MgO and Al 2 O 3 17.8% of Yb 2 O 3 Is 10 percent by mass of SiO 2 The content of (b) is 61.5% by mass. The rest is the same as test one.
And evaluating the performance of the joint in the third test by adopting the compressive shear strength to obtain the joint with the room-temperature shear strength of 85MPa.
And (4) testing four: this test differs from the test one in that: 5.7 percent of MgO and Al 2 O 3 17.8% by mass of Yb 2 O 3 Is 15 percent by mass, siO 2 The mass percentage of (B) is 61.5%. The rest is the same as test one.
And evaluating the performance of the joint in the fourth test by adopting the compressive shear strength to obtain the joint with the room-temperature shear strength of 20MPa.
And (5) testing: for the silicon carbide fiber reinforced silicon carbide (SiC) in practical demand f the/SiC) ceramic pipe is assembled and connected with the SiC end cover, and the process is shown in figure 4; 5% Yb prepared by test one 2 O 3 -15.7％MgO-17.8％Al 2 O 3 -61.5％SiO 2 Glass ceramicsAnd solder (5 YbMAS) is put in an argon atmosphere, the connection temperature is 1340 ℃, and the heat preservation time is 10min, so that a joint with a good packaging effect of the cladding tube is obtained, and a physical photograph is shown in figure 5.
Claims (10)
1. A method for connecting silicon carbide ceramics by cordierite microcrystalline glass solder is characterized in that the method for connecting the silicon carbide ceramics by the cordierite microcrystalline glass solder is carried out according to the following steps:
1. weighing 4 raw material powders according to the following mass percentages: 5.7 to 20.7 percent of MgO and Al 2 O 3 17.8% by mass of Yb 2 O 3 0-15% of SiO 2 The mass percentage content of (A) is 61.5%; then ball-milling and mixing the weighed 4 raw material powders, putting the mixture into a crucible, and carrying out high-temperature melting at the smelting temperature of 1550-1600 ℃ for 2-2.5 h to obtain glass melt with uniform components;
2. pouring molten glass into deionized water for water quenching, taking out from the water to obtain broken glass slag, drying and performing ball milling treatment to obtain fine glass powder, and sieving the glass powder to remove uncrushed glass blocks to obtain glass solder;
3. grinding and polishing the to-be-connected surface of the ceramic base material: carrying out surface grinding and polishing treatment by adopting diamond grinding paste with the diameter of 1 mu m to obtain a surface to be connected, then placing the base material in alcohol for ultrasonic cleaning for 15-20 min, and drying for later use; the ceramic base material is bulk silicon carbide ceramic or SiC f a/SiC composite ceramic;
4. putting the glass solder prepared in the step two into a tabletting mold, pressing into a sheet shape of 0.1-0.5 mm, and then placing between two ceramic parent metals to form a sandwich structure;
5. and placing the assembled sandwich structure in an atmosphere furnace, realizing non-pressure connection under the condition of inert atmosphere, heating to 1320-1380 ℃, preserving heat for 10-15 min, and cooling along with the furnace to finish the whole connection process.
2. According to claim1, the method for connecting the silicon carbide ceramics by the cordierite microcrystalline glass solder is characterized in that in the step one, the mass percentage of MgO is 15.7 percent, and Al is contained 2 O 3 17.8% by mass of Yb 2 O 3 Is 5 percent by mass, siO 2 The content of (b) is 61.5% by mass.
3. The method of claim 1, wherein the melting temperature in step one is 1550 ℃ and the temperature is kept for 2h.
4. The method of claim 1, wherein the first step comprises ball milling for 12 hours.
5. The method of claim 1, wherein in step two, the cordierite glass-ceramic solder is passed through a 300 mesh screen.
6. The method for connecting the silicon carbide ceramics by the cordierite microcrystalline glass solder as claimed in claim 1, wherein the ultrasonic cleaning is carried out for 15min in the third step.
7. The method for bonding silicon carbide ceramics by using cordierite glass-ceramic solders according to claim 1, wherein the glass solder prepared in step two is placed in a tabletting mold and pressed into 0.2mm tablets in step four.
8. The method of joining silicon carbide ceramics by cordierite-glass-ceramic solder according to claim 1, wherein the inert atmosphere in step five is argon.
9. The method for connecting the silicon carbide ceramics by the cordierite microcrystalline glass solder according to claim 1, wherein in the fifth step, the temperature is raised to 1340 ℃ and kept for 10-15 min.
10. The method of claim 9, wherein in step five the temperature is raised to 1340 ℃ and held for 10min.
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