CN115894058A - Method for flash-burning rapid densification of SiC/SiC composite material - Google Patents
Method for flash-burning rapid densification of SiC/SiC composite material Download PDFInfo
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- CN115894058A CN115894058A CN202211496130.XA CN202211496130A CN115894058A CN 115894058 A CN115894058 A CN 115894058A CN 202211496130 A CN202211496130 A CN 202211496130A CN 115894058 A CN115894058 A CN 115894058A
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Abstract
The invention provides a method for quickly densifying a SiC/SiC composite material by flash firing, which comprises the steps of firstly, mixing submicron silicon carbide powder and chopped silicon carbide fibers coated with pyrolytic carbon coatings according to a certain proportion, and performing ball milling, drying, granulation, grinding and sieving to obtain a flash firing formula which is uniformly mixed, thereby preparing SiC/SiC composite powder; and finally, wrapping the green body with a graphite felt, connecting the wrapped green body with a circuit in series, and placing the wrapped green body in flash burning equipment to prepare the compact SiC/SiC composite material. The composite powder prepared by the invention is characterized in that the flash firing formula can uniformly form sialon crystal boundaries on the surface of SiC powder, the densification can be rapidly realized under the condition of not applying any external force by the graphite felt coated green body flash firing technology, and the composite powder has wide application prospects in the fields of rapid repair of ceramic parts, mass production, environmental protection, energy conservation and the like.
Description
Technical Field
The invention belongs to the field of composite material densification, and particularly relates to a method for quickly densifying a SiC/SiC composite material.
Technical Field
The rapid densification technology has great development prospect in the field of ceramics, and compared with the traditional sintering mode, the rapid sintering can obviously shorten the longer densification period at high temperature, thereby saving important production cost for the engineering ceramic industry. The spark plasma sintering has a faster sintering rate, and the sintered material has better mechanical property and electrical property, higher density and smaller average grain diameter. However, this is an external pressure assist technique, which is prone to damage to materials that cannot be stressed, and its use is generally limited to the manufacture of geometrically simple parts. Flash firing has been applied as a non-pressure rapid densification technique to many oxide ceramic materials with ionic or electronic conductivity, such as alumina, zirconia, strontium titanate, etc. However, there has been little research on flash-fired semiconductor non-oxide ceramics such as silicon carbide (SiC) and chopped silicon carbide fiber reinforced silicon carbide composites (SiC/SiC). Sintering of additive-free SiC is very difficult, free silicon in SiC can hinder sintering and is difficult to fully densify without applying any pressure. The design and development of a novel non-pressure rapid densification SiC/SiC composite material key technology becomes an important direction for researching rapid densification of the ceramic matrix composite material at present.
Chinese patent with application number CN201710308597.X discloses a preparation method for sintering zirconium-aluminum complex-phase eutectic ceramic by using flash firing technology. Aims to provide a preparation method for sintering zirconium-aluminum complex phase eutectic ceramics by applying flash firing technology. The invention applies the flash sintering technology to Al 2 O 3 Preparation of YSE eutectic ceramics, preparation of the resultant Al 2 O 3 The YSE eutectic ceramic has a rod-like eutectic morphology, and has high-temperature stability, high fracture toughness and high bending strength; compared with other eutectic ceramic preparation methods, the preparation method provided by the invention has the advantages of simple equipment, high controllability of the preparation process, short preparation time, energy conservation and the like.
Chinese patent application No. CN202011422329.9 discloses a method for preparing a continuous fiber reinforced ceramic matrix composite material by flash firing technology. The invention aims to provide a method for preparing a continuous fiber reinforced ceramic matrix composite by using a flash firing technology, which is used for solving the technical problems of high preparation temperature, long preparation time and complicated preparation process of the conventional continuous fiber reinforced ceramic matrix composite. The flash firing technology is applied to the preparation of the continuous fiber reinforced ceramic matrix composite material, and the ceramic matrix composite material can be obtained only by hours. Compared with the traditional preparation method, the equipment for preparing the ceramic matrix composite material by using the flash firing technology is very simple, the sintering temperature is lower, the preparation period is greatly shortened, the obtained composite material is more compact, the ceramic crystal grains are finer, and the mechanical property of the material is more excellent.
Chinese patent CN202011422329.9 discloses an ultrafast sintering method and a sintering apparatus for ceramic materials. The flexible electrodes are arranged at the two ends of the ceramic blank body for firing, the ceramic blank body is quickly shrunk when flash firing occurs in the firing process, the flexible electrodes are always attached to and cover the ceramic blank body, the electrical contact is good, the arc discharge phenomenon is not found, and the ceramic is not bent or broken; compared with the prior art, the method solves the problem that the sample is fractured due to the mechanical stress generated inside the ceramic green body when flash firing occurs, and effectively improves the yield of flash firing experiments. Meanwhile, the invention does not need to coat a conductive layer on the ceramic green body to form an electrode, thereby not only reducing the working procedures, but also avoiding the problem that the ceramic material under the electrode can not be fully sintered to meet the densification requirement, and providing a new technical scheme for the ceramic flash firing technology. The invention still keeps the characteristics of short sintering time, low energy consumption, simple device and the like of the flash combustion technology.
The three inventions solve the problems of long sintering period and high cost of the ceramic matrix composite to a certain extent. Chinese patent with application number CN201811259309.7 discloses SiC f PIP rapid densification method of/SiC composite material preform. The density of the PIP post-preform reaches 2.3g/cm 3 Compared with the traditional PIP process, the preparation period is shortened by more than 25%.
The flash sintering technology is utilized to improve the densification efficiency of the ceramic material to a certain extent and reduce the temperature of a sintering furnace. The SiC ceramic has excellent performance and can be widely applied to the engineering fields of machinery, aerospace, machinery and the like, particularly in the environments of high temperature, high pressure, high corrosion and the like, so that the SiC ceramic becomes one of the most attractive materials in high temperature application. SiC ceramics are more difficult to sinter densify, requiring high temperatures and the application of pressure to densify. The pressureless rapid densification technology of SiC/SiC composite materials is also gradually becoming a hot point for the research in the field of ceramics. The development of a technology from high-temperature pressurized densification to pressureless rapid densification effectively improves the densification efficiency of the ceramic matrix composite material, reduces the sintering cost and realizes pressureless rapid sintering at low furnace temperature. However, there are few reports in China at present.
Disclosure of Invention
The invention aims to provide a method for quickly densifying a SiC/SiC composite material by flash firing, which solves the technical problems of low preparation efficiency, high preparation cost and complex preparation process of the existing SiC composite material by adopting a flash firing technology.
In order to achieve the above object, the present invention provides a flash-firing rapid densification method for a SiC/SiC composite material, which is characterized by comprising the following steps:
(1) Mixing submicron silicon carbide composite powder and chopped silicon carbide fibers with pyrolytic carbon interfaces according to a certain proportion, and performing ball milling, drying, granulation, grinding and sieving to obtain a flash firing formula which is uniformly mixed, wherein the ball milling time is 20-30 hours;
(2) Placing the mixture obtained in the step (1) in a mould for compression molding to obtain a silicon carbide green body, wherein the pressure is 100-200 MPa, and the pressure maintaining time is 60s;
(3) And (3) wrapping the silicon carbide green body obtained in the step (2) by using a graphite felt, connecting the green body and a circuit in series, placing the green body in flash firing equipment, sintering the green body by adopting a flash firing process, and cooling to obtain the compact SiC/SiC composite material.
Further, the chopped silicon carbide fiber in the step (1) comprises one of SiC nanowire and SiC chopped fiber, and the mass fraction of the silicon carbide reinforced phase is 1-3%; the submicron silicon carbide composite powder is prepared by mechanically mixing SiC powder and Al powder 2 O 3 The powder and the SiN powder are uniformly mixed to form a sialon crystal boundary on the surface of the SiC powder uniformly, the size of the powder is 50-800nm 2 O 3 Mass fraction of powder5 to 25 percent of the total amount of the powder and 2 to 8 percent of SiN powder; the adhesive used for granulating is acidic aluminum phosphate (AlPO) 4 ) And the binder comprises 3 to 5 mass percent of P to Al (atomic ratio) =23 to 1.
Further, the flash firing process in the step (3) includes: placing the green body and the circuit in series in flash burning equipment, vacuumizing to-0.1 MPa, heating the furnace to 150-200 ℃, and introducing argon; heating the green body to a preset constant temperature, and then applying a constant electric field until a flash burning phenomenon occurs; then, the furnace temperature is kept at the flash sintering temperature, a specific voltage is applied to the sample until the current is limited, and the control mode of the power supply is quickly changed from voltage control to current control; and (5) closing the flash burning equipment, and cooling along with the furnace.
Further, the length of the green body in the direction of the electric field is 5-20 cm, and the flow of argon is stabilized at 40-60 mL/min; the preset constant temperature is 300-900 ℃, and the heating rate is 5-20 ℃/min; the preset constant electric field intensity is 20-600V/cm; the current density of the current control state is 15-500 mA/mm, and the limiting current is 10-15A; the cooling rate is 5-20 ℃/min.
Advantageous effects
(1) SiC powder and Al of the invention 2 O 3 The flash sintering formula prepared by uniformly mixing the powder and the SiN powder uniformly forms a sialon crystal boundary on the surface of the SiC powder uniformly, so that the flash sintering densification degree of the SiC/SiC green body is improved;
(2) The graphite felt wraps the SiC/SiC green body, so that heat loss caused by the difference between the surface temperature of the green body and the ambient temperature in the flash firing process is reduced;
(3) The formula for the rapid densification of the SiC/SiC composite material by flash firing only needs a dozen of seconds to obtain the ceramic matrix composite material. Is beneficial to improving the densification efficiency of the ceramic matrix composite material, reducing the preparation cost and simplifying the process flow.
Drawings
FIG. 1 is a process flow diagram of a method for flash-firing rapid densification of a SiC/SiC composite material according to the present invention.
Detailed Description
The invention will now be further described with reference to the examples:
example 1
A method for flash-firing rapid densification of SiC/SiC composite material is characterized by comprising the following steps:
(1) Mixing submicron silicon carbide composite powder with chopped silicon carbide fibers with pyrolytic carbon interfaces, wherein the mass fraction of the chopped silicon carbide fibers is 1%, and performing ball milling, drying, granulation, grinding and sieving to obtain a flash firing formula which is uniformly mixed, wherein the ball milling time is 24 hours;
(2) Placing the mixture obtained in the step (1) in a mould for compression molding to obtain a silicon carbide green body, wherein the pressure is 150MPa, and the pressure maintaining time is 60s;
(3) And (3) wrapping the silicon carbide green body obtained in the step (2) by using a graphite felt, connecting the green body and a circuit in series, placing the green body in flash firing equipment, sintering the green body by adopting a flash firing process, and cooling to obtain the compact SiC/SiC composite material.
Further, the submicron silicon carbide composite powder in the step (1) is prepared by mixing SiC powder and Al powder by a mechanical mixing method 2 O 3 Mixing the powder and SiN powder uniformly to form sialon crystal boundary on the surface of SiC powder with powder size of 50nm, and adding Al 2 O 3 The powder size of the powder is 100nm and the mass fraction is 20%, and the powder size of the SiN powder is 200nm and the mass fraction is 4%; the adhesive used for granulating is acidic aluminum phosphate (AlPO) 4 ) And the binder comprises 3% of P and Al (atomic ratio) = 23: 1 by mass.
Further, the flash firing process in the step (3) includes: placing the green body and a circuit in series in flash firing equipment, wherein the length of the green body in the direction of an electric field is 10cm, vacuumizing to-0.1 MPa, heating the furnace to 150 ℃, introducing argon, and stabilizing the flow of the introduced argon at 45mL/min; heating the green body to a preset constant temperature, and then applying a constant electric field until a flash burning phenomenon occurs, wherein the preset constant temperature is 500 ℃, and the heating rate is 5 ℃/min; the preset constant electric field intensity is 200V/cm; then, keeping the furnace temperature at the flash sintering temperature, applying a specific voltage to the sample until the current is limited, quickly switching the control mode of the power supply from voltage control to current control, wherein the current density in the current control state is 200mA/mm, and the limited current is 10A; and (4) closing the flash burning equipment, wherein the temperature is reduced along with the furnace in a cooling mode, and the cooling rate is 10 ℃/min.
Example 2
A method for flash-burning rapid densification of SiC/SiC composite material is characterized by comprising the following steps:
(1) Mixing submicron silicon carbide composite powder with silicon carbide nanowires with pyrolytic carbon interfaces, wherein the mass fraction of the chopped silicon carbide fibers is 3%, and performing ball milling, drying, granulation, grinding and sieving to obtain a uniformly mixed flash-firing formula, wherein the ball milling time is 27 hours;
(2) Placing the mixture obtained in the step (1) in a mould for compression molding to obtain a silicon carbide green body, wherein the pressure is 200MPa, and the pressure maintaining time is 60s;
(3) And (3) wrapping the silicon carbide green body obtained in the step (2) by using a graphite felt, connecting the green body and a circuit in series, placing the green body in flash firing equipment, sintering the green body by adopting a flash firing process, and cooling to obtain the compact SiC/SiC composite material.
Further, the submicron silicon carbide composite powder in the step (1) is prepared by mixing SiC powder and Al powder by a mechanical mixing method 2 O 3 The powder and the SiN powder are uniformly mixed to form a sialon crystal boundary on the surface of the SiC powder uniformly, the powder size of the SiC powder is 60nm 2 O 3 The powder size of the powder is 150nm, the mass fraction is 10%, the powder size of the SiN powder is 300nm, and the mass fraction is 7%; the adhesive used for granulating is acidic aluminum phosphate (AlPO) 4 ) And the binder comprises 5% of P and Al (atomic ratio) = 23: 1 by mass percent.
Further, the flash firing process in the step (3) includes: placing the green body and a circuit in series in flash firing equipment, wherein the length of the green body in the direction of an electric field is 10cm, vacuumizing to-0.1 MPa, heating the furnace to 200 ℃, introducing argon, and stabilizing the flow of the introduced argon at 55mL/min; heating the green body to a preset constant temperature, and then applying a constant electric field until a flash burning phenomenon occurs, wherein the preset constant temperature is 700 ℃, and the heating rate is 10 ℃/min; the preset constant electric field intensity is 500V/cm; then, the furnace temperature is kept at the flash sintering temperature, specific voltage is applied to the sample until the current is limited, the control mode of the power supply is rapidly changed from voltage control to current control, the current density in the current control state is 400mA/mm, and the limiting current is 15A; and (4) closing the flash burning equipment, wherein the temperature is reduced along with the furnace in a temperature reduction mode, and the temperature reduction rate is 15 ℃/min.
The above description is only an embodiment of the present invention, but the design concept of the present invention is not limited thereto, and any insubstantial modifications made by using the design concept should fall within the scope of infringing the protection scope of the present invention. However, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (4)
1. A method for flash-burning rapid densification of SiC/SiC composite material is characterized by comprising the following steps:
(1) Mixing submicron silicon carbide composite powder and chopped silicon carbide fibers with pyrolytic carbon interfaces according to a certain proportion, and performing ball milling, drying, granulation, grinding and sieving to obtain a flash firing formula which is uniformly mixed, wherein the ball milling time is 20-30 hours;
(2) Placing the mixture obtained in the step (1) in a mould for compression molding to obtain a silicon carbide green body, wherein the pressure is 100-200 MPa, and the pressure maintaining time is 60s;
(3) And (3) wrapping the silicon carbide green body obtained in the step (2) by using a graphite felt, connecting the green body and a circuit in series, placing the green body in flash firing equipment, sintering the green body by adopting a flash firing process, and cooling to obtain the compact SiC/SiC composite material.
2. The method for flash-firing rapid densification of a SiC/SiC composite material according to claim 1, wherein the flash-fired formulation of step (1) includes chopped SiC fibers,One of SiC chopped fibers, wherein the mass fraction of the silicon carbide reinforced phase is 1-3%; the submicron silicon carbide composite powder in the flash-firing formula is prepared by mechanically mixing SiC powder and Al powder 2 O 3 The powder and the SiN powder are uniformly mixed to form a sialon crystal boundary on the surface of the SiC powder uniformly, the size of the powder is 50-800nm 2 O 3 5-25% of powder and 2-8% of SiN powder; the binder used for granulating in the flash-firing formula is acidic aluminum phosphate (AlPO) 4 ) And the binder comprises 3 to 5 mass percent of P to Al (atomic ratio) =23 to 1.
3. The method for flash-sintering rapid densification of SiC/SiC composite material according to claim 1, wherein the flash-sintering process in step (3) comprises: placing the green body and the circuit in series in flash burning equipment, vacuumizing to-0.1 MPa, heating the furnace to 150-200 ℃, and introducing argon; heating the green body to a preset constant temperature, and then applying a constant electric field until a flash burning phenomenon occurs; then, the furnace temperature is kept at the flash sintering temperature, a specific voltage is applied to the sample until the current is limited, and the control mode of the power supply is quickly changed from voltage control to current control; and (5) closing the flash burning equipment, and cooling along with the furnace.
4. The length of the green body in the direction of an electric field is 5-20 cm according to claim 3, and the flow of argon is stabilized at 40-60 mL/min; the preset constant temperature is 300-900 ℃, and the heating rate is 5-20 ℃/min; the preset constant electric field intensity is 20-600V/cm; the current density of the current control state is 15-500 mA/mm, and the limiting current is 10-15A; the cooling rate is 5-20 ℃/min.
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