CN115958264A - Method for connecting silicon carbide - Google Patents
Method for connecting silicon carbide Download PDFInfo
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- CN115958264A CN115958264A CN202310033072.5A CN202310033072A CN115958264A CN 115958264 A CN115958264 A CN 115958264A CN 202310033072 A CN202310033072 A CN 202310033072A CN 115958264 A CN115958264 A CN 115958264A
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Abstract
Embodiments of the present application provide a method of joining silicon carbide. The connection method comprises the following steps: depositing a compact aluminum-titanium nano particle layer on the surface of the silicon carbide substrate by using a pulse laser deposition method; butting the silicon carbide substrates deposited with the aluminum-titanium nano-particle layers; and brazing the butted silicon carbide substrates to connect the silicon carbide substrates into a whole. In the method for connecting silicon carbide provided by the embodiment of the application, the aluminum titanium nano particle layer can be used as a connecting layer for connecting a silicon carbide substrate; meanwhile, the particles of the connecting layer formed by deposition through a pulse laser deposition method are in a nanometer size, so that the temperature required by the brazing of the silicon carbide substrate can be reduced; in addition, by using the pulse laser deposition method, the connection layer can be deposited on the surface of the silicon carbide substrate with more shapes, so that the limitation of the shape of the silicon carbide substrate on connection is reduced.
Description
Technical Field
The embodiment of the application relates to the technical field of material connection, in particular to a connection method of silicon carbide.
Background
Silicon carbide has many excellent characteristics such as good high temperature characteristic, good radiation resistance, low neutron absorption cross section, low activation, low tritium permeability and the like, and is very suitable for being applied to nuclear reactors. Silicon carbide, however, has poor processability and difficulty in obtaining net shape, and thus, joining silicon carbide with silicon carbide or other materials is required to produce devices with larger volumes and more complex shapes.
In the related art, there is a connection method of silicon carbide, for example, by applying Al, si powder made into slurry onto a silicon carbide substrate as a connection layer and connecting the silicon carbide substrates through the connection layer; or the high-entropy metal infiltration phase infiltrates into the silicon carbide substrate in a gas phase form to be used as a connecting layer, and then the silicon carbide substrate is connected through the connecting layer, and the like. However, the above-mentioned method for connecting silicon carbide is difficult to control the thickness of the connecting layer, and the welding temperature is high, so that the effect of connecting silicon carbide is poor.
Disclosure of Invention
In view of the above problems, embodiments of the present application provide a method of connecting silicon carbide, including: depositing a compact aluminum-titanium nano particle layer on the surface of the silicon carbide substrate by using a pulse laser deposition method; butting the silicon carbide substrates deposited with the aluminum-titanium nano particle layers; and brazing the butted silicon carbide substrates to connect the silicon carbide substrates into a whole.
According to the silicon carbide connection method provided by the embodiment of the application, the aluminum titanium nano particle layer can be used as a connection layer for connecting a silicon carbide substrate, and the composition and the thickness of the connection layer can be controlled by adjusting the working parameters during pulse laser deposition, so that the thickness and the composition of the connection layer are uniform and controllable; meanwhile, the particles of the connecting layer formed by deposition through a pulse laser deposition method are in a nanometer size, so that the temperature required by the brazing of the silicon carbide substrate can be reduced, and the connection process of the silicon carbide substrate is easier; in addition, by using the pulse laser deposition method, the connection layer can be deposited on the surface of the silicon carbide substrate with more shapes, and the limitation of the shape of the silicon carbide substrate on connection is reduced.
Drawings
The above and/or additional aspects and advantages of the present application will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
fig. 1 is a schematic flow chart illustrating a method for bonding silicon carbide according to an embodiment of the present disclosure;
FIG. 2 is a schematic illustration of a pulsed laser deposition system for depositing a dense layer of aluminum titanium nanoparticles on a surface of a silicon carbide substrate according to an embodiment of the present disclosure;
FIG. 3 is a schematic illustration of the butting of silicon carbide substrates with a deposited aluminum titanium nanoparticle layer in accordance with an embodiment of the present application;
FIG. 4 is a schematic flow diagram illustrating the docking of a silicon carbide substrate having a deposited aluminum-titanium nanoparticle layer according to an embodiment of the present disclosure;
FIG. 5 is a schematic illustration of another embodiment of the present application for depositing a dense layer of aluminum titanium nanoparticles on a surface of a silicon carbide substrate using a pulsed laser deposition system;
FIG. 6 is a schematic illustration of the docking of a silicon carbide substrate with a deposited aluminum titanium nanoparticle layer according to another embodiment of the present application;
FIG. 7 is a schematic flow diagram illustrating the docking of a silicon carbide substrate having a deposited aluminum titanium nanoparticle layer according to another embodiment of the present disclosure;
FIG. 8 is a topographical view of an aluminum titanium nanoparticle layer of an embodiment of the present application;
fig. 9 is a topography of a heated aluminum titanium nanoparticle layer according to an embodiment of the present application.
It should be noted that the drawings are not necessarily drawn to scale and are merely shown in a schematic manner that does not interfere with the understanding of those skilled in the art.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments in the present application without making any creative effort belong to the protection scope of the present application. For the embodiments of the present application, it should also be noted that, in a case of no conflict, the embodiments of the present application and features of the embodiments may be combined with each other to obtain a new embodiment.
The embodiment of the application provides a silicon carbide connecting method. In the embodiment, a connecting layer is deposited on the surface of the silicon carbide substrate, and then the silicon carbide substrates are connected in a soldering mode.
Fig. 1 is a schematic flow chart illustrating a method for joining silicon carbide according to an embodiment of the present disclosure. As shown in fig. 1, the method for connecting silicon carbide may include steps S101 to S103.
Specifically, step S101, depositing a dense aluminum-titanium nanoparticle layer on the surface of the silicon carbide substrate by using a pulsed laser deposition method; step S102, butting the silicon carbide substrates deposited with the aluminum-titanium nano particle layer; and S102, soldering the butted silicon carbide substrates to connect the silicon carbide substrates into a whole.
According to the silicon carbide connection method provided by the embodiment of the application, the aluminum titanium nano particle layer can be used as a connection layer for connecting a silicon carbide substrate, and the composition and the thickness of the connection layer can be controlled by adjusting the working parameters during pulse laser deposition, so that the thickness and the composition of the connection layer are uniform and controllable.
Meanwhile, the particles of the connecting layer formed by deposition by the pulse laser deposition method are in a nanometer size, and the connecting layer formed by the aluminum titanium nanoparticles in the nanometer size is used as the solder, so that the temperature required by the brazing of the silicon carbide substrate can be reduced, and the connecting process of the silicon carbide substrate is easier.
In addition, the pulse laser deposition method forms the connecting layer by sputtering the target material to the nano particles and depositing the nano particles on the surface of the silicon carbide substrate, so that the connecting layer can be deposited on the surface of the silicon carbide substrate with more shapes by using the pulse laser deposition method, and the limitation of the shape of the silicon carbide substrate on connection is reduced.
In some embodiments, the step of depositing a layer of aluminum titanium nanoparticles on the surface of the silicon carbide substrate using a pulsed laser deposition process may comprise: heating the silicon carbide substrate; and respectively bombarding the aluminum target material and the titanium target material by the double-beam pulse laser under the vacuum condition, so that the aluminum nanoparticles and the titanium nanoparticles sputtered by the aluminum target material and the titanium target material are simultaneously deposited on the surface of the silicon carbide substrate.
In some embodiments, a pulsed deposition system may be used to deposit a surface of a silicon carbide substrate. Fig. 2 is a schematic view of depositing a dense aluminum titanium nanoparticle layer on a surface of a flat-plate silicon carbide substrate by using a pulsed laser deposition system according to an embodiment of the present disclosure, and fig. 5 is a schematic view of depositing a dense aluminum titanium nanoparticle layer on a surface of a silicon carbide substrate in an end plug shape by using a pulsed laser deposition system according to an embodiment of the present disclosure.
As shown in fig. 2 and 5, the pulsed laser deposition system may include a sample stage 10, a first target stage 21, a second target stage 22, a first pulsed laser 31, a second pulsed laser 32, and a vacuum chamber 40. The sample stage 10, the first target stage 21, the second target stage 22, the first pulse laser 31, and the second pulse laser 32 may be disposed in the vacuum chamber 40.
The sample stage 10 is for carrying a silicon carbide substrate 100. The sample stage 10 is configured to rotate to drive the silicon carbide substrate 100 disposed on the sample stage 10 to rotate together, the sample stage 10 is further configured to heat the silicon carbide substrate 100, and the heated silicon carbide substrate 100 may facilitate the deposition of nanoparticles. In some embodiments, the heating temperature of the sample stage 10 may range from 0 to 600 ℃, and preferably, the heating temperature may be 500 ℃.
The first target table 21 and the second target table 22 are used to carry the first target 200 and the second target 300, respectively. In this embodiment, the first target 200 may be an aluminum target, the second target 300 may be a titanium target, and the metal purity of the aluminum target and the titanium target may be 99.999%. The first target table 21 and the second target table 22 are configured to be rotatable to rotate the first target 200 and the second target 300 provided on the first target table 21 and the second target table 22, respectively, together.
The first pulse laser 31 and the second pulse laser 32 are used for performing irradiation bombardment on the first target material and the second target material arranged on the first target material table 21 and the second target material table 22, respectively, so that nanoparticles are sputtered from the target materials. The first pulse laser 31 and the second pulse laser 32 are configured to be power-tunable to adjust the speed at which the nanoparticles are sputtered from the first target 200 and the second target 300, respectively. The frequency range of the first pulse laser 31 and the second pulse laser 32 may be 500kHz to 2MHz, and the pulse width of the pulse laser generated by the first pulse laser 31 and the second pulse laser 32 may be 10ns to 300fs.
The vacuum chamber 40 is used to provide a vacuum environment for the pulsed laser deposition system to prevent air from interfering with nanoparticle formation and deposition. In some embodiments, the vacuum provided by the vacuum chamber 40 can range from 500Pa to 6 × 10 Pa -3 Pa, in other embodiments, the vacuum chamber 40 may provide 2 × 10 -4 Pa vacuum degree.
In this embodiment, the silicon carbide substrate 100 may be placed in the vacuum chamber 40 and fixed on the sample stage 10, and the silicon carbide substrate 100 may be heated by the sample stage 10; meanwhile, in the vacuum chamber 40, the aluminum target material and the titanium target material are bombarded by the dual-beam pulse laser generated by the first pulse laser 31 and the second pulse laser 32, respectively. After being bombarded by laser, the aluminum target and the titanium target respectively sputter aluminum nanoparticles and titanium nanoparticles, and the aluminum nanoparticles and the titanium nanoparticles move to the surface of the silicon carbide substrate 100 in the vacuum chamber 40 and are deposited on the surface of the silicon carbide substrate 100. The aluminum nanoparticles and titanium nanoparticles sputtered from the aluminum target and titanium target may be deposited on the surface of the silicon carbide substrate 100 simultaneously, so that the composition of the aluminum-titanium nanoparticle layer is more uniform.
In some embodiments, the composition of the layer of aluminum titanium nanoparticles may be controlled by adjusting the laser power bombarding the aluminum target material and/or adjusting the laser power bombarding the titanium target material.
It can be appreciated that the laser power bombarding the aluminum target and the laser power bombarding the titanium target affect the speed at which the aluminum nanoparticles and the titanium nanoparticles are sputtered, respectively. Specifically, the higher the laser power, the faster the speed at which the aluminum nanoparticles and the titanium nanoparticles are sputtered, the more nanoparticles are deposited on the surface of the silicon carbide substrate 100 per unit time. Therefore, in this embodiment, the components of the aluminum-titanium nanoparticle layer can be controlled by adjusting the laser power for bombarding the aluminum target material and/or adjusting the laser power for bombarding the titanium target material. For example, increasing the laser power to bombard the aluminum target and/or decreasing the laser power to bombard the titanium target may increase the atomic percentage of aluminum in the layer of aluminum-titanium nanoparticles (reflecting the proportion of aluminum nanoparticles).
In some embodiments, the laser power to bombard the aluminum target may be any value between 50W, 60W, 70W, 80W, 90W, 100W, or 50W to 100W, and correspondingly, the laser power to bombard the titanium target may be any value between 50W, 40W, 30W, 20W, 10W, or 10W to 50W. In the above-described aluminum-titanium nanoparticle layer formed by the power, the atomic percentage of aluminum may be any value between 50at%, 60at%, 70at%, 80at%, 90at%, 100at%, or 50at% to 100at%, respectively, and correspondingly, the atomic percentage of titanium may be any value between 50at%, 40at%, 30at%, 20at%, 0at%, or 10at% to 50at%, respectively.
In some embodiments, the deposition time of the pulsed laser deposition may be adjusted to control the thickness of the aluminum titanium nanoparticle layer on the surface of the silicon carbide substrate 100.
It is understood that the thickness of the aluminum titanium nanoparticle layer is affected by the deposition time of the pulsed laser deposition system. Specifically, the longer the deposition time of the pulsed laser deposition system, the more aluminum nanoparticles and titanium nanoparticles are deposited on the surface of the silicon carbide substrate 100, and the greater the thickness of the aluminum-titanium nanoparticle layer. Therefore, in this embodiment, the thickness of the aluminum-titanium nanoparticle layer on the surface of the silicon carbide substrate 100 can be controlled by adjusting the deposition time of the pulsed laser deposition system. In some embodiments, the thickness of the aluminum titanium nanoparticle layer on the surface of the silicon carbide substrate 100 may be adjusted in a range of 10 to 30 μm by controlling the deposition time.
In some embodiments, the silicon carbide substrate 100 may be controlled to rotate during the deposition process to uniformly deposit a layer of aluminum titanium nanoparticles on the surface of the silicon carbide substrate 100. In this embodiment, by controlling the rotation of the silicon carbide substrate 100, different portions of the surface of the silicon carbide substrate 100 can be constantly changed in position, and are prevented from being fixed at the same position in the vacuum chamber 40, so that the deposition of the aluminum-titanium nanoparticle layer is more uniform.
In some embodiments, the aluminum target and the titanium target may be controlled to rotate during deposition so that the laser bombards the aluminum target and the titanium target uniformly. It can be understood that, during the deposition process, the aluminum target and the titanium target respectively sputter the aluminum nanoparticles and the titanium nanoparticles, and the aluminum target and the titanium target are continuously consumed, so that the surfaces of the aluminum target and the titanium target may be uneven, and the sputtering speed of the nanoparticles may be changed, which may interfere with the thickness control of the aluminum-titanium nanoparticle layer. Therefore, in the embodiment, the aluminum target and the titanium target can be uniformly bombarded by the laser by controlling the rotation of the aluminum target and the titanium target, so that the sputtering speed of the nano particles is uniform and controllable, and the thickness control of the aluminum-titanium nano particle layer is facilitated.
In some embodiments, the step of brazing the butted silicon carbide substrates comprises: placing the butted silicon carbide substrate in a brazing furnace under a vacuum condition; controlling the temperature of the brazing furnace to rise to a preset temperature and preserving the temperature so as to enable the aluminum phase in the aluminum-titanium nano particle layer to react with the silicon carbide substrate 100 to form a Ti-containing material 3 Si(Al)C 2 A nanoparticle connecting layer of phases; the brazing furnace is cooled to obtain the integrally connected silicon carbide substrate 100.
In this embodiment, the brazing furnace may be formed in a vacuum condition to prevent air from interfering with the brazing process, and for example, the brazing furnace may be formed in a 2 × 10 manner -5 Pa vacuum degree.
Because the particle diameter in the aluminum titanium nano particle layer is nano, the temperature required by melting the aluminum titanium nano particle layer can be reduced. The Al-Ti nanoparticle layer may be melted and reacted with the silicon carbide substrate 100at a predetermined temperature to produce Ti 3 Si(Al)C 2 Thereby increasing the bonding strength of the silicon carbide substrate 100. In this embodiment, since the thickness of the aluminum-titanium nanoparticle layer is controllable, when the thickness of the aluminum-titanium nanoparticle layer is small, almost all aluminum phases in the aluminum-titanium nanoparticle layer can react with the silicon carbide substrate 100 to generate Ti 3 Si(Al)C 2 Phase to make the silicon carbide substrate 100 more robust.
In some embodiments, the step of controlling the brazing furnace to heat up to a predetermined temperature and holding includes: controlling the temperature of the brazing furnace to rise to a first preset temperature; and after the brazing furnace is kept at the first preset temperature for the first preset time, controlling the brazing furnace to continuously raise the temperature to the second preset temperature, and keeping the temperature for the second preset time. The first predetermined temperature may be a temperature at which the aluminium phase melts, for example 1000 ℃; the second predetermined temperature may be a temperature at which the aluminum completely reacts with the silicon carbide substrate 100, for example, 1400 ℃. The rate of temperature increase to the first predetermined temperature may be 8 ℃/min and the rate of temperature increase to the second predetermined temperature may be 6 ℃/min.
As shown in fig. 3 and 6, an upper pressure plate 51 and a lower support plate 52 may be provided in the brazing furnace, and when brazing two silicon carbide substrates, the aluminum titanium nanoparticle layers 400 deposited on the two silicon carbide substrates may be butted first by the upper pressure plate 51 and the lower support plate 52.
Specifically, as shown in fig. 3 and 4, when brazing two flat plate-type silicon carbide substrates 100, one silicon carbide substrate 100 may be fixed to the upper platen 51 with the surface on which the aluminum-titanium nanoparticle layer 400 is deposited facing downward, while the other silicon carbide substrate 100 may be fixed to the lower plate 52 with the surface on which the aluminum-titanium nanoparticle layer 400 is deposited facing upward, and then the distance between the upper platen 51 and the lower plate 52 may be reduced to bring the two aluminum-titanium nanoparticle layers 400 deposited on the two silicon carbide substrates into contact with each other, thereby completing the butt joint. Then heating to melt the Al-Ti nanoparticle layer 400, and reacting the Al phase with the silicon carbide matrix to form Ti-containing alloy 3 Si(Al)C 2 Nanoparticle connection layer of phases 500.
In this embodiment, the two flat plate-shaped silicon carbide substrates 100 can be tightly joined to each other, and a joint having good airtightness and high-temperature strength can be obtained. The shear strength of the joint was 102MPa.
In another embodiment, as shown in fig. 6 and 7, when brazing the silicon carbide end plugs 110 and the silicon carbide cladding 120, a layer of aluminum titanium nanoparticles 400 may be deposited on the surface of the silicon carbide end plugs 110, the silicon carbide cladding 120 may then be secured to the bottom plate 52, and the silicon carbide end plugs 110 may be plugged into the silicon carbide cladding 120 to complete the butt joint. Then the Al-Ti nanoparticle layer 400 is melted by heating, and the Al phase therein reacts with the silicon carbide matrix to form Ti-containing nanoparticles 3 Si(Al)C 2 Nanoparticle connection layer of phases 500.
In this embodiment, silicon carbide end plugs 110 and silicon carbide cladding 120 may form a tight joint, resulting in a joint that is both gas tight and strong at high temperatures. The shear strength of the connection joint was 94MPa.
FIG. 8 is a topographical view of an aluminum titanium nanoparticle layer of an embodiment of the present application; fig. 9 is a topography of a heated aluminum titanium nanoparticle layer according to an embodiment of the present application. FIG. 8 shows the state where the degree of vacuum is 8X 10 -3 The atomic fraction of aluminum deposited under the Pa is 20at percent of the morphology of the aluminum-titanium nanoparticle layer; FIG. 9 shows the state of vacuum at 8X 10 -3 Pa, and the atomic fraction of aluminum deposited under the condition of heating at 500 ℃ is 20at percent of the morphology of the aluminum-titanium nanoparticle layer. As shown in fig. 8 and 9, by using the method provided by the embodiment of the present application, an aluminum titanium nanoparticle layer with a uniform thickness can be formed.
The above embodiments are merely examples, and not intended to limit the scope of the present application, and all modifications, equivalents, and flow charts using the contents of the specification and drawings of the present application, or those directly or indirectly applied to other related arts, are included in the scope of the present application.
Claims (10)
1. A method of joining silicon carbide, comprising:
depositing a compact aluminum-titanium nano particle layer on the surface of the silicon carbide substrate by using a pulse laser deposition method;
butting the silicon carbide substrates deposited with the aluminum-titanium nanoparticle layers;
and brazing the butted silicon carbide substrates to connect the silicon carbide substrates into a whole.
2. The method of claim 1, wherein the step of depositing a dense layer of aluminum titanium nanoparticles on the surface of the silicon carbide substrate using pulsed laser deposition comprises:
heating the silicon carbide substrate;
and respectively bombarding the aluminum target material and the titanium target material by double beams of pulse laser under a vacuum condition, so that the aluminum nanoparticles and the titanium nanoparticles sputtered by the aluminum target material and the titanium target material are simultaneously deposited on the surface of the silicon carbide substrate.
3. The method of claim 2, further comprising:
and (3) adjusting the laser power for bombarding the aluminum target material and/or adjusting the laser power for bombarding the titanium target material to control the components of the aluminum-titanium nano particle layer.
4. The method of claim 2, further comprising:
adjusting the deposition time of the deposition to control the thickness of the aluminum-titanium nanoparticle layer on the surface of the silicon carbide substrate.
5. The method of claim 4, further comprising:
and in the deposition process, controlling the silicon carbide substrate to rotate so as to uniformly deposit the aluminum-titanium nano particle layer on the surface of the silicon carbide substrate.
6. The method of claim 5, further comprising:
and in the deposition process, controlling the aluminum target and the titanium target to rotate so that the laser can uniformly bombard the aluminum target and the titanium target.
7. The method of claim 1, wherein the step of brazing the butted silicon carbide substrate comprises:
placing the butted silicon carbide substrate in a brazing furnace under a vacuum condition;
controlling the temperature of the brazing furnace to be raised to a preset temperature and preserving the temperature so as to enable the aluminum phase in the aluminum-titanium nano particle layer to react with the silicon carbide substrate to form a titanium-containing titanium 3 Si(Al)C 2 A nanoparticle connection layer of phases;
and cooling the brazing furnace to obtain the silicon carbide substrate connected into a whole.
8. The method of claim 7, wherein the step of controlling the brazing furnace to heat to a predetermined temperature and holding comprises:
controlling the temperature of the brazing furnace to rise to a first preset temperature;
and after the brazing furnace is kept at the first preset temperature for first preset time, controlling the brazing furnace to continuously raise the temperature to a second preset temperature, and keeping the temperature for second preset time.
9. The method according to any one of claims 1 to 8, wherein the thickness of the layer of aluminum titanium nanoparticles on the surface of the silicon carbide substrate is 10 to 30 μm.
10. A method according to any one of claims 1 to 8, wherein the atomic percent of aluminium in the layer of aluminium titanium nanoparticles on the surface of the silicon carbide substrate is in the range 50 to 100at%.
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