CN117567168B - Method for connecting silicon carbide ceramic part and biscuit - Google Patents
Method for connecting silicon carbide ceramic part and biscuitInfo
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- CN117567168B CN117567168B CN202311625078.8A CN202311625078A CN117567168B CN 117567168 B CN117567168 B CN 117567168B CN 202311625078 A CN202311625078 A CN 202311625078A CN 117567168 B CN117567168 B CN 117567168B
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- 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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Abstract
本发明属于反应烧结SiC陶瓷技术领域，公开了一种碳化硅陶瓷部件与素坯的连接方法。步骤为：将反应烧结碳化硅的缺陷部位机加出被补工件，利用SiC素坯补配加工出单自由度互补件，涂敷粘结剂，采用间隙配合的方式连接，然后施压干燥、打磨，将连接件中烧结体与充足的Si源接触，置于特定环境中烧结，处理后精加工得到SiC陶瓷部件。本发明通过素坯互补件间隙配合的方式控制精度和余量，利用毛细管力吸附SiC烧结体中游离Si进入、Si源不断补充烧结体的动力学原理，通过同质反应连接达到提高纯度和致密化的效果，使烧结体和素坯的连接成为现实，提高了半导体装备用高纯SiC陶瓷部件的利用率，避免了重复制备工序，操作容易，过程简单。
The present invention belongs to the technical field of reaction-sintered SiC ceramics, and discloses a method for connecting a silicon carbide ceramic component to a blank. The steps are as follows: machining a defective part of the reaction-sintered silicon carbide to produce a workpiece to be repaired, using the SiC blank to complement and process a single-degree-of-freedom complementary part, applying an adhesive, connecting by gap fitting, then applying pressure to dry and polish, contacting the sintered body in the connecting part with a sufficient Si source, sintering in a specific environment, and finishing after treatment to obtain a SiC ceramic component. The present invention controls the accuracy and margin by gap fitting the complementary part of the blank, utilizes the dynamic principle of capillary force adsorbing free Si in the SiC sintered body and the Si source continuously replenishing the sintered body, and achieves the effect of improving purity and densification through homogeneous reaction connection, making the connection of the sintered body and the blank a reality, improving the utilization rate of high-purity SiC ceramic components for semiconductor equipment, avoiding repeated preparation processes, and being easy to operate and simple in process.
Description
Technical Field
The invention relates to the technical field of reaction sintering SiC ceramics, in particular to a method for connecting a silicon carbide ceramic part with a biscuit.
Background
The reaction sintering SiC has the advantages of high densification degree and purity, excellent physical and chemical properties, high reaction speed, low cost, unchanged sizes of parts before and after sintering, capability of being prepared into products with complex shapes and the like, and is well applied to the field of semiconductor front process equipment.
The SiC precision component is used as a key component in integrated circuit manufacturing equipment, is directly or indirectly contacted with a wafer, and has high requirements on the purity, the compactness and the physical and chemical properties of materials, and particularly cannot have any defects. In the process of preparing the SiC ceramic part by utilizing the reaction sintering, defects such as looseness, air holes, cracks, surface corrosion, fatigue and the like are extremely easy to occur due to improper finish machining process, sintering temperature control or use mode, so that the product is directly abandoned. For precision parts with complex structures, repeated preparation processes are tedious, difficult to process, time-consuming and labor-consuming, and cause great waste. If the defective SiC ceramic component products can be effectively connected and repaired, the material utilization rate and the product qualification rate can be directly improved.
At present, the connecting technology of the silicon carbide ceramics mainly comprises a brazing method, a diffusion welding method, a glass solder method, a reaction connecting method, a cementing method and the like. The reactive connection forms SiC as an intermediate layer through Si-C reaction, so that the problem of unmatched thermal expansion coefficients is avoided, and the method is an ideal connection mode. However, the patent CN110790586a considers that the defects are concentrated in the core part due to the influence of the thermodynamic factor or the influence of multiple sintering, that is, the Si content in the SiC after the reaction sintering reaches a saturated state, and the secondary sintering can volatilize and lose Si in the ceramic, especially in the core part, so that the core part of the SiC ceramic after sintering has loose defects, and further the mechanical property and the surface precision of the material can be affected.
Therefore, a method for effectively connecting and repairing the SiC ceramic part products by utilizing a simpler and effective method for avoiding the volatilization loss of Si in secondary sintering so as to influence the mechanical property and the surface precision of the materials becomes important.
Disclosure of Invention
Aiming at the technical problems, the invention provides a method for connecting a silicon carbide ceramic part and a biscuit, which directly improves the material utilization rate and the product qualification rate by mechanically adding a defect part and a single-degree-of-freedom complementary part and sintering the parts after connection, avoids repeated preparation procedures, and has easy operation and simple process.
In order to achieve the above object, the technical scheme of the present invention is as follows:
A method for connecting a silicon carbide ceramic component with a biscuit comprises the following steps:
s1, machining a defect part of a silicon carbide ceramic part into a specific shape to obtain a repaired workpiece;
s2, adding a single-degree-of-freedom complementary piece by using a SiC biscuit supplementing machine;
And S3, coating a pre-prepared adhesive, connecting the repaired workpiece and the complementary workpiece to obtain a connecting piece, pressing, drying, polishing, contacting with a sufficient Si source, sintering again, cleaning and finishing to obtain a qualified SiC ceramic component product.
Furthermore, in the step S1, the machining precision is +/-0.1 mm, and the surface roughness Ra of the repaired workpiece is required to be 0.8-3.2, so that the repair is facilitated, and the specific shape is matched with the complementary piece.
Further, the single-degree-of-freedom complementary piece in the step S2 is in clearance fit with the repaired workpiece, and protrudes out of the repaired workpiece after being matched.
Further, the binder in the step S3 may be a paste, emulsion or suspension, and the binder includes 15% -35% of thermoplastic resin, 20% -40% of sic micropowder, 3% -7% of carbon black and the balance of organic solvent.
Further, the thermoplastic resin is at least one of silicon resin, phenolic resin and acrylic resin, the SiC micro powder grading is the same as that of the original ceramic component during molding, the carbon black is submicron-sized modified by polyethylene glycol dispersion, the particle size is 0.5 mu m, and the organic solvent contains polyethylene glycol and ethanol.
Further, the "pressing" in the step S3 means that a pressure of 0.1-10MPa is applied to the connecting position on the connecting piece, the "drying" means that the connecting layer is solidified by standing at room temperature for 48-60h or keeping the temperature for 4-6h in a 60-80 ℃ drying oven environment, and the polishing means that the allowance on the biscuit of the complementary piece after the connection is removed.
Further, the "contact with sufficient Si source" in the step S3 means that sufficient elemental Si powder, si particles or Si blocks are provided, and only contact with the sintered body portion in the connection member, not contact with the biscuit or the connection layer in the connection member, BN permeation-blocking protection may be applied.
Further, "re-sintering" in the step S3 refers to vacuum environment at 1470-1570 ℃ for 1-3 hours. At temperatures above the melting point of Si, the gas pressure in the furnace should be made higher than the saturation vapor pressure at the highest sintering temperature of Si to prevent vaporization loss of liquid Si in the material. Finally, the biscuit continuously adsorbs free Si in the SiC sintered body, reacts and infiltrates with the connecting layer, and the Si source continuously supplements the sintered body, so that the purposes of uniform densification and no influence on surface precision are achieved.
The principle of forming compact high purity is that molten Si enters a SiC biscuit under the combined action of temperature gradient thermodynamics and capillary force dynamics, then under the promotion of further reaction dynamics of residual C in the biscuit, reaction infiltration is carried out to generate secondary SiC, a small amount of free Si fills the residual pores, 10.9% of free Si is recrystallized and expanded when the temperature is reduced, internal stress is released to the surface, and finally compact high purity Si/SiC complex phase ceramic is formed.
The invention has the beneficial effects that:
(1) The invention provides a method for connecting a silicon carbide ceramic part and a biscuit, which is characterized in that defects of a reaction sintering SiC material are effectively repaired by mechanically adding a defect part and a single-degree-of-freedom complementary part, and sintering the silicon carbide ceramic part and the biscuit after connection. By controlling the gas pressure in the furnace in the re-sintering process, the gas pressure is higher than the saturated vapor pressure of Si at the highest sintering temperature when the gas pressure is higher than the melting point temperature of Si, so that the gasification loss of liquid Si in the material is prevented. Finally, the biscuit continuously adsorbs free Si in the SiC sintered body, reacts with the connecting layer for infiltration, and the Si source continuously supplements the sintered body, so that the purposes of uniform densification and no influence on surface precision are achieved, and the mechanical property and the surface precision after connection are ensured.
(2) According to the method for connecting the silicon carbide ceramic component and the biscuit, the precision and the allowance are controlled in a manner of clearance fit of the biscuit complementary piece, the kinetic principle that free Si in the SiC sintered body is adsorbed by capillary force and the Si source is continuously supplemented to the sintered body is utilized, and the effects of improving the purity and densification are achieved through homogeneous reaction connection. Under the combined action of temperature gradient thermodynamics and capillary force dynamics, molten Si enters a SiC biscuit, then under the promotion of further reaction dynamics of residual C in the biscuit, the reaction infiltration is carried out, secondary SiC is generated, a small amount of free Si fills the residual pores, 10.9% of free Si is recrystallized and expanded when the temperature is reduced, internal stress is released to the surface, and finally compact high-purity Si/SiC complex-phase ceramic is formed.
(3) The invention provides a method for connecting a silicon carbide ceramic part and a biscuit, which realizes the connection of a sintered body and the biscuit. The unqualified products in the silicon carbide ceramic component are repaired in a biscuit-sintered body connection mode, the material utilization rate and the product qualification rate are directly improved, repeated preparation procedures are avoided, the operation is easy, and the process is simple.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic illustration of the connection between complementary pieces of a silicon carbide ceramic component product where different defects are to be located and a silicon carbide ceramic component product.
FIG. 2 is a schematic illustration of a sintering process after joining a silicon carbide ceramic sintered body component to a green complement.
Fig. 3 is a photograph (b) of a certain silicon carbide ceramic part (vacuum chuck base) and its defective location (a) and the ceramic part after repair.
FIG. 4 is a macroscopic photograph of the as-fired silicon carbide sintered body-green body connector sample of example 1 after re-firing, where (a) is before polishing and (b) is after polishing.
Fig. 5 is a metallographic photograph of the area of the joining layer of the onboard sample of example 1.
Fig. 6 is a metallographic photograph of the connection layer region of the furnace-following sample of example 4.
Fig. 7 is a metallographic photograph of the connection layer region of the furnace-associated sample of example 5.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without any inventive effort, are intended to be within the scope of the invention.
The invention provides a method for connecting a silicon carbide ceramic component and a biscuit, which specifically refers to a method for mechanically adding a specific shape at a defect part of the ceramic component to obtain a repaired workpiece, adding a single-degree-of-freedom complementary piece by using a SiC biscuit repairing machine, connecting the repaired workpiece and the single-degree-of-freedom complementary piece by using an adhesive, and adopting a clearance fit connection mode. The connection structure of the degree-of-freedom complementary piece and the repaired workpiece is shown in fig. 1. Then, the SiC ceramic part is contacted with a sufficient Si source to be sintered again, cleaned and finished to obtain the SiC ceramic part product. Wherein the Si source is only in contact with the sintered body portion of the connector and not in contact with the biscuit or the connecting layer of the connector (FIG. 2), and the position of the biscuit and the connecting layer can be coated with BN anti-infiltration protection. By gradually increasing the gas pressure in the furnace above the saturation vapor pressure of Si at the sintering temperature above the Si melting point temperature, vaporization loss of liquid Si in the material is prevented. Finally, the biscuit continuously adsorbs free Si in the SiC sintered body, reacts and infiltrates with the connecting layer, and the Si source continuously supplements the sintered body, so that the purposes of uniform densification and no influence on surface precision are achieved.
Example 1
The method for connecting the silicon carbide ceramic component and the biscuit comprises the following steps:
And (3) processing an arc column with the height of 21mm R5 from the defect part, wherein the roughness Ra is 0.8, and the repaired workpiece is obtained. Meanwhile, a single-degree-of-freedom complementary piece with the same radius is processed by utilizing the SiC biscuit, and the height is 22mm. The adhesive is prepared from 25% of phenolic resin, 30% of silicon carbide micropowder, 5% of carbon black, 5% of polyethylene glycol and 35% of ethanol, and the adhesive is coated and connected with the repaired workpiece and the complementary workpiece in a clearance fit manner. And (5) drying at room temperature for 48 hours after applying the pressure of 6MPa, and polishing the complementary piece part to the size and the precision of the product. The connecting piece is placed in a vacuum environment, a sufficient amount of Si powder is placed on the sucker base, and sintering is carried out for 2 hours at 1550 ℃. And (3) filling Ar gas when the temperature is raised to 1400 ℃ to enable the air pressure in the furnace to reach 90Pa (the saturated steam pressure of Si at 1550 ℃ is 32 Pa), cooling to room temperature, and cleaning and finishing to obtain the qualified SiC ceramic component. In addition, the furnace-following sample of this example also consisted of two parts (reaction-sintered silicon carbide and SiC green compact), and the roughness of the portion of the sintered silicon carbide to be repaired was 0.8, which was then joined by the same process conditions.
The furnace-following sample and the product were tested according to the methods of GB/T6569 Fine ceramic flexural Strength test method, GB/T3045 common abrasive Carborundum analysis method and GB/T13841 electronic ceramic surface roughness.
The three-point bending test shows that the bending strength of 12 samples with the thickness of 3-4-40 mm in the sample parent metal area is 344.6MPa on average, the connecting layer is arranged at different positions, the fracture is arranged in the middle of the sample, the bending strength of 12 samples is 342MPa on average, and the mechanical properties of the connecting layer and the parent metal are basically consistent. The surface roughness is less than Ra0.8, and the surface precision after finish machining reaches the design requirement.
Fig. 3 is a photograph of the silicon carbide vacuum chuck base and its defective position (a) and the ceramic part after connection repair (b) according to the present embodiment. The vacuum chuck connected by the method can be seen, no repair trace is basically seen in a macroscopic scale, the connection is basically consistent before and after the connection, and the connection effect is good.
FIG. 4 is a macroscopic picture of the specimens (sintered body-green body joint) after re-sintering in this example, in which (a) is before polishing, the joint layer cross section is macroscopically insignificant, and (b) barely visible as a bright line, caused by Si pool, after polishing, FIG. 5 is a metallographic picture of the joint layer region of the specimens, the joint layer is microscopically 80 μm wide, the joint surface on one side of the sintered body is smoother, the joint surface on one side of the green body is rougher, the carbon black in the binder reacts thoroughly, a large amount of fine secondary SiC is generated, the joint effect is good, and the microstructure of the joint layer and the base material is substantially uniform.
Example 2
The method for connecting the silicon carbide ceramic component and the biscuit comprises the following steps:
And (3) processing a parallelogram with the side length of 3mm and the side length of 5mm on the upper bottom surface and the lower bottom surface of the defect part respectively by using a certain reaction sintering silicon carbide ceramic component with the size of phi 250mm and 30mm, and obtaining a repaired workpiece with the roughness Ra of 1.6. Meanwhile, the SiC biscuit is processed into a single-degree-of-freedom complementary piece which has a matched shape with the workpiece to be repaired, and protrudes out of the workpiece to be repaired after being matched. The adhesive is prepared from 30% of acrylic resin, 25% of silicon carbide micropowder, 3% of carbon black, 2% of polyethylene glycol and 40% of ethanol, and the adhesive is coated and connected with the repaired workpiece and the complementary workpiece in a clearance fit manner. A tooling clamp is used for applying pressure of 1MPa, and the product is placed in a 60 ℃ drying oven for 6 hours and then polished to the size and the precision of the product. The connector was placed in a vacuum environment and a sufficient amount of Si blocks were placed on the ceramic part and sintered at 1500 ℃ for 2h. The vacuum pump was turned off at the temperature rise to 1400 ℃ to slowly raise the pressure in the furnace to 50Pa (Si saturated vapor pressure at 1500 ℃ C. Is 18 Pa), and then the pressure value was maintained by turning off the vacuum pump. And after cooling to room temperature, cleaning and finishing to obtain the repaired SiC ceramic part. In addition, the furnace-following sample of this example also consisted of two parts (reaction-sintered silicon carbide and SiC green compact), and the roughness of the portion of the sintered silicon carbide to be repaired was 1.6, which was then joined by the same process conditions.
The furnace-following samples were tested according to the methods of GB/T6569 Fine ceramic flexural Strength test method, GB/T3045 common abrasive Carboriding analysis method and GB/T13841 electronic ceramic surface roughness.
The three-point bending test shows that the bending strength of 12 samples with the thickness of 3-4-40 mm in the sample parent metal area is 343MPa on average, the connecting layer is arranged at different positions, the fracture is arranged in the middle of the sample, the bending strength of 12 samples is 340MPa on average, and the mechanical properties of the connecting layer and the parent metal are basically consistent. The surface roughness is less than Ra0.8, and the surface precision after finish machining reaches the design requirement.
Example 3
The method for connecting the silicon carbide ceramic component and the biscuit comprises the following steps:
And (3) a certain reaction sintering silicon carbide ceramic component, wherein the size of the reaction sintering silicon carbide ceramic component is phi 250mm and 30mm, a bubble exists on the boss, circular truncated cone single-degree-of-freedom complementary component biscuit with the diameters of the upper bottom surface circle and the lower bottom surface circle of 3mm and 5mm respectively and the height of 8mm is processed, and the roughness Ra of the circular truncated cone single-degree-of-freedom complementary component biscuit is 3.2, so that a repaired workpiece is obtained. Meanwhile, the SiC biscuit is processed into a single-degree-of-freedom complementary piece which has a matched shape with the workpiece to be repaired, and protrudes out of the workpiece to be repaired after being matched. The adhesive is prepared from 25% of phenolic resin, 30% of silicon carbide micropowder, 5% of carbon black, 5% of polyethylene glycol and 35% of ethanol, and the adhesive is coated and connected with the repaired workpiece and the complementary workpiece in a clearance fit manner. And (3) drying at room temperature for 60 hours after the pressure of 0.1MPa is applied, and polishing the complementary piece part to the size and the precision of the product. The connector is placed in a vacuum environment, a sufficient amount of Si powder is placed on the sucker base, and sintering is carried out for 3 hours at 1470 ℃. And (3) when the temperature is raised to 1400 ℃, ar gas is filled to enable the air pressure in the furnace to reach 50Pa (the saturated steam pressure of Si at 1470 ℃ is 14 Pa), and after the temperature is reduced to room temperature, the qualified SiC ceramic component is obtained through cleaning and finish machining. In addition, the furnace-following sample of this example also consisted of two parts (reaction-sintered silicon carbide and SiC green compact), and the roughness of the portion of the sintered silicon carbide to be repaired was 3.2, which was then joined by the same process conditions.
The furnace-following samples were tested according to the methods of GB/T6569 Fine ceramic flexural Strength test method, GB/T3045 common abrasive Carboriding analysis method and GB/T13841 electronic ceramic surface roughness.
And analyzing the qualified SiC ceramic part and the sample along with the furnace, wherein the bending strength of the base metal and the connecting layer is 340MPa, and the connecting layer width is 85 mu m, which is possibly caused by smaller pressure. The surface roughness is less than Ra0.8, and the surface precision after finish machining reaches the design requirement. The results are substantially the same as in example 1, and small differences may result from systematic errors.
Example 4
The method for connecting the silicon carbide ceramic component and the biscuit comprises the following steps:
And (3) processing an arc column with the height of 21mm R5 from the defect part, wherein the roughness Ra is 0.8, and the repaired workpiece is obtained. Meanwhile, a single-degree-of-freedom complementary piece with the same radius is processed by utilizing the SiC biscuit, and the height is 22mm. The adhesive is prepared from 15% of phenolic resin, 20% of silicon carbide micropowder, 3% of carbon black, 5% of polyethylene glycol and 57% of ethanol, and the adhesive is coated and connected with the repaired workpiece and the complementary workpiece in a clearance fit manner. A pressure of 10MPa is applied, placed in an 80 ℃ drying oven for 4 hours, and then polished to the product size and precision. The connector is placed in a vacuum environment, a sufficient amount of Si powder is placed on the base of the sucker, and the connector is sintered for 1h at 1570 ℃. And (3) when the temperature is raised to 1400 ℃, ar gas is filled to enable the air pressure in the furnace to reach 90Pa (the saturated steam pressure of Si at 1570 ℃ is 32 Pa), and after the temperature is reduced to room temperature, the qualified SiC ceramic component is obtained through cleaning and finish machining. In addition, the furnace-following sample of this example also consisted of two parts (reaction-sintered silicon carbide and SiC green compact), and the roughness of the portion of the sintered silicon carbide to be repaired was 0.8, which was then joined by the same process conditions.
The furnace-following samples were tested according to the methods of GB/T6569 Fine ceramic flexural Strength test method, GB/T3045 common abrasive Carboriding analysis method and GB/T13841 electronic ceramic surface roughness.
The three-point bending test shows that the connecting layers are arranged at different positions, the fracture is arranged in the middle of the test samples, the bending strength of 12 test samples is 290Mpa on average, and the surface roughness is less than Ra0.8. Fig. 6 shows the metallographic structure of the furnace-following sample of this example, and it can be seen from the figure that, due to the low C source content and the low solid content of SiC in the binder, a large number of free Si or Si pools appear in the connection layer, and the SiC particles are less, which cannot form an effective barrier to crack propagation.
Example 5
The method for connecting the silicon carbide ceramic component and the biscuit comprises the following steps:
And (3) processing an arc column with the height of 21mm R5 from the defect part, wherein the roughness Ra is 0.8, and the repaired workpiece is obtained. Meanwhile, a single-degree-of-freedom complementary piece with the same radius is processed by utilizing the SiC biscuit, and the height is 22mm. The adhesive is prepared from 35% of phenolic resin, 40% of silicon carbide micropowder, 7% of carbon black, 1% of n-butanol and 17% of ethanol, and the adhesive is coated and connected with the repaired workpiece and the complementary workpiece in a clearance fit manner. And (5) drying at room temperature for 48 hours after applying the pressure of 6MPa, and polishing the complementary piece part to the size and the precision of the product. The connecting piece is placed in a vacuum environment, a sufficient amount of Si powder is placed on the sucker base, and sintering is carried out for 2 hours at 1550 ℃. And (3) filling Ar gas when the temperature is raised to 1400 ℃ to enable the air pressure in the furnace to reach 90Pa (the saturated steam pressure of Si at 1550 ℃ is 32 Pa), cooling to room temperature, and cleaning and finishing to obtain the qualified SiC ceramic component. In addition, the furnace-following sample of this example also consisted of two parts (reaction-sintered silicon carbide and SiC green compact), and the roughness of the portion of the sintered silicon carbide to be repaired was 0.8, which was then joined by the same process conditions.
The furnace-following samples were tested according to the methods of GB/T6569 Fine ceramic flexural Strength test method, GB/T3045 common abrasive Carboriding analysis method and GB/T13841 electronic ceramic surface roughness.
The three-point bending test shows that when the connecting layer is arranged at different positions, fracture mainly occurs in the base material region, the bending strength of 12 samples is 350Mpa on average, and the surface roughness is less than Ra0.8. Fig. 7 shows the metallographic structure of the furnace-associated sample in this example, and it can be seen from the figure that the strength of the connecting layer is even slightly stronger than that of the base material due to the fact that a large amount of small-particle secondary SiC is generated in the connecting layer due to excessive C source, which effectively blocks crack propagation.
Comparative example 1
The method for connecting the silicon carbide ceramic part and the biscuit in this comparative example, unlike example 1, is characterized by continuously evacuating the furnace by a Roots pump at a temperature higher than 1400 ℃ to a pressure of 20Pa lower than the saturated vapor pressure (32 Pa) of Si at 1550 ℃, and comprises the following steps:
A reaction sintering silicon carbide vacuum chuck base for a certain photoetching machine has the size phi 336 mm x 21mm, a larger crack (18 mm) exists on the side surface, an arc column with the height of 21mm R5 is processed at the defect part, the roughness Ra0.8 is achieved, and meanwhile, a single degree of freedom complementary piece with the same radius is processed by utilizing a SiC biscuit, and the height is 22mm. The adhesive is prepared from 25% of phenolic resin, 30% of silicon carbide micropowder, 5% of carbon black, 5% of polyethylene glycol and 35% of ethanol, and the adhesive is coated and connected with the repaired workpiece and the complementary workpiece in a clearance fit manner. And (5) drying at room temperature for 48 hours after applying the pressure of 6MPa, and polishing the complementary piece part to the size and the precision of the product. The connecting piece is placed in a vacuum environment, a sufficient amount of Si powder is placed on the sucker base, and sintering is carried out for 2 hours at 1550 ℃. And (3) filling Ar gas when the temperature is raised to 1400 ℃ to enable the air pressure in the furnace to reach 20Pa (the saturated steam pressure of Si at 1550 ℃ is 32 Pa), cooling to room temperature, and cleaning and finishing to obtain the qualified SiC ceramic component. The finally repaired sucker base has loose core parts along with the furnace sample, the product surface appearance is poor, and the processing precision does not completely reach the standard.
Comparative example 2
The method of joining the silicon carbide ceramic member and the green body of this comparative example, unlike example 1, was such that the silicon source was in direct contact with the green body and the joining layer in the joining member, not with the sintered body, and the specific steps were as follows:
A reaction sintering silicon carbide vacuum chuck base for a certain photoetching machine has the size phi 336 mm x 21mm, a larger crack (18 mm) exists on the side surface, an arc column with the height of 21mm R5 is processed at the defect part, the roughness Ra0.8 is achieved, and meanwhile, a single degree of freedom complementary piece with the same radius is processed by utilizing a SiC biscuit, and the height is 22mm. The adhesive is prepared from 25% of phenolic resin, 30% of silicon carbide micropowder, 5% of carbon black, 5% of polyethylene glycol and 35% of ethanol, and the adhesive is coated and connected with the repaired workpiece and the complementary workpiece in a clearance fit manner. And (5) drying at room temperature for 48 hours after applying the pressure of 6MPa, and polishing the complementary piece part to the size and the precision of the product. The connector is placed in a vacuum environment, si powder is in direct contact with the biscuit and the connecting layer in the connector, and sintering is carried out for 2h at 1550 ℃. And (3) filling Ar gas when the temperature is raised to 1400 ℃ to enable the air pressure in the furnace to reach 90Pa (the saturated steam pressure of Si at 1550 ℃ is 32 Pa), cooling to room temperature, and cleaning and finishing to obtain the qualified SiC ceramic component. Finally, the Si of the connecting layer is not impregnated thoroughly, and defects such as air holes and the like are generated, so that the effect of bonding or repairing is not achieved.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (8)
1. A method for connecting a silicon carbide ceramic component with a biscuit is characterized by comprising the following steps:
S1, machining a defect part of a silicon carbide ceramic part to obtain a repaired workpiece;
s2, adding a single-degree-of-freedom complementary piece by using a SiC biscuit supplementing machine;
S3, connecting the repaired workpiece with the single-degree-of-freedom complementary piece through coating an adhesive to obtain a connecting piece;
And S4, pressing, drying and polishing the connecting piece, contacting with a Si source, sintering again, cleaning and finishing to obtain a qualified SiC ceramic part product, wherein the contact with the Si source means that the Si source only contacts with a sintered body part in the connecting piece and does not contact with a biscuit or a connecting layer in the connecting piece, and the sintering again is carried out under the condition that sintering is carried out for 1-3 hours at 1470-1570 ℃ in a vacuum environment, and when the temperature reaches 1400 ℃, the air pressure in a furnace is increased to ensure that the air pressure is higher than the saturated vapor pressure of the sintering temperature of Si.
2. The method for joining a silicon carbide ceramic component to a green body according to claim 1, wherein the machining precision in the step S1 is ±0.1mm, and the surface roughness Ra of the workpiece to be repaired is 0.8 to 3.2.
3. The method according to claim 2, wherein the single degree of freedom complementary piece in step S2 is a piece that is in clearance fit with the workpiece to be repaired and protrudes from the workpiece to be repaired after the fitting.
4. A method of joining a silicon carbide ceramic component to a green body according to claim 3, wherein the binder in step S3 is a paste, emulsion or suspension.
5. The method for joining a silicon carbide ceramic component to a green body according to claim 1 or 4, wherein the binder in step S3 comprises 15 to 35% of a thermoplastic resin, 20 to 40% of sic micropowder, 3 to 7% of carbon black, and the balance of an organic solvent.
6. The method for joining a silicon carbide ceramic component to a green body according to claim 5, wherein the thermoplastic resin is at least one of a silicone resin, a phenolic resin, and an acrylic resin, the SiC fine powder gradation is the same as that of the original ceramic component when molded, the carbon black is a submicron grade modified by dispersion of polyethylene glycol, the particle diameter is 0.5 μm, and the organic solvent contains polyethylene glycol and ethanol.
7. The method according to claim 5, wherein the pressing in the step S4 is a pressing force of 0.1-10MPa at the connecting position of the connecting piece, the drying is a standing drying or a drying at room temperature to solidify the connecting layer, and the polishing is a removal of the residual amount of the complementary piece blank after the connection.
8. The method for joining a silicon carbide ceramic component to a green body according to claim 7, wherein the Si source in step S4 is elemental Si powder, si particles or Si pieces.
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| CN108794041A (en) * | 2017-05-02 | 2018-11-13 | 中国科学院上海硅酸盐研究所 | A kind of reaction-sintered CfThe method that/SiC ceramic matrix composite material is connected with synchronous reaction |
| CN115536436A (en) * | 2021-06-30 | 2022-12-30 | 航天特种材料及工艺技术研究所 | A repair method for carbon fiber toughened ceramic matrix composite components |
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| GB2137975B (en) * | 1983-04-12 | 1986-09-17 | Atomic Energy Authority Uk | Joining silicon carbide bodies |
| JP4537669B2 (en) * | 2003-06-30 | 2010-09-01 | 株式会社東芝 | Silicon carbide-based bonded component and method for manufacturing the same |
| DE102004044942A1 (en) * | 2004-09-16 | 2006-03-30 | Esk Ceramics Gmbh & Co. Kg | Method for low-deformation diffusion welding of ceramic components |
| JP2008274101A (en) * | 2007-04-27 | 2008-11-13 | Tokai Univ | Adhesive composition for silicon carbide ceramics and method for bonding silicon carbide ceramics |
| JP5773331B2 (en) * | 2010-05-27 | 2015-09-02 | Toto株式会社 | Manufacturing method of ceramic joined body |
| US11969962B2 (en) * | 2020-09-25 | 2024-04-30 | General Electric Company | Method for repairing composite components and associated infiltration systems and methods |
| CN114012877B (en) * | 2021-11-12 | 2023-04-21 | 航天特种材料及工艺技术研究所 | Reinforcing method of continuous carbon fiber toughened ceramic matrix composite |
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| CN108794041A (en) * | 2017-05-02 | 2018-11-13 | 中国科学院上海硅酸盐研究所 | A kind of reaction-sintered CfThe method that/SiC ceramic matrix composite material is connected with synchronous reaction |
| CN115536436A (en) * | 2021-06-30 | 2022-12-30 | 航天特种材料及工艺技术研究所 | A repair method for carbon fiber toughened ceramic matrix composite components |
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