CN115141028B - Method for preparing silicon carbide based composite material integral turbine disk based on gel casting pre-reinforcement - Google Patents
Method for preparing silicon carbide based composite material integral turbine disk based on gel casting pre-reinforcement Download PDFInfo
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Abstract
The invention relates to a method for preparing a silicon carbide based composite material integral turbine disk based on gel casting pre-strengthening, which adopts gel casting to prepare SiC by combining carbon thermal reduction pre-strengthening and PIP technology w A method of integrating a turbine disk with SiC composite material. Is required to be in SiC w The temperature gradient is set in the drying process of the biscuit, and the drying time of the corresponding temperature section needs to be strictly controlled. To SiC is required w Pre-strengthening the preform by applying to SiC w Adding proper amount of silicon dioxide particles into gel casting slurry, performing carbothermic reduction reaction on the silicon dioxide particles and carbon remained by organic matters in a vacuum gel discharging stage to form silicon carbide phase, and performing subsequent repeated impregnation of sucrose and silica sol solution and high-temperature carbothermic reduction reaction on SiC w Forming a certain amount of silicon carbide phase in the preform, opposite to SiC w The biscuit has a pre-strengthening effect. In the PIP process, the concentration of the precursor, the cracking temperature, the heating rate and the heat treatment conditions need to be strictly controlled.
Description
Technical Field
The invention belongs to a manufacturing method of an integral turbine disk of SiC ceramic matrix composite, and relates to a method for preparing an integral turbine disk of silicon carbide matrix composite based on gel casting pre-strengthening.
Background
The working environment of the rotating parts of the aero-engine, represented by the integral turbine disc, is very harsh, and needs to bear ultra-high temperature (higher than 1500 ℃), high load and complex stress. The silicon carbide (SiC) ceramic matrix composite has the advantages of light weight, high strength, high temperature resistance, oxidation resistance and the like, and has wide application prospect in the aerospace field. Wherein the SiC fiber reinforced SiC ceramic matrix composite (SiC f SiC) is considered to be a good heatStructural material suitable for medium load structural components. At present, the temperature resistance of domestic commercial grade SiC fibers is still to be improved, decomposition, crystallization and grain growth start to occur at the temperature of generally higher than 1350 ℃, and the continuous SiC fiber reinforced composite material has anisotropic characteristics, so that SiC is prepared f The application of the SiC composite material to rotating parts such as an integral turbine disk and the like in ultra-high temperature and complex stress environments is limited. Silicon carbide whisker (SiC) w ) The single crystal reinforcement is a single crystal reinforcement with stoichiometric ratio, has good temperature resistance and can be kept stable at 1800 ℃; the elastic modulus and the tensile strength are very high, and are respectively 550GPa and 20.8GPa; and SiC is provided with w Reinforced composites generally have isotropic characteristics. The above characteristics enable SiC w The SiC composite material is one of the most ideal candidate materials for rotating parts such as an integral turbine disk of an aero-engine.
SiC w The SiC composite materials are generally prepared based on sintering processes, which are very high sintering temperatures (generally above 1800 ℃) for SiC, since SiC is a covalent bond compound w Causing relatively large thermal damage; and the linear shrinkage rate of the composite material after sintering is very large (usually 20% -30%), and the near-net-size preparation of the complex structure of the whole turbine disk cannot be realized. Different from the traditional sintering process, the preparation of whisker preform and densification are carried out by taking reference to the process route of continuous fiber reinforced ceramic matrix composite (CFCs), and the isotropic, high-strength and high-temperature resistant SiC is hopeful to be realized w SiC composite and its overall turbine disk near net dimensions. Chen Naiji et al (Microstructure and properties of SiC) w SiC was molded by gel casting/SiC composites prepared by gel-casting combined with precursor infiltration and pyrolysis. Ceram Int 2018,44 (1): 969-979) w The prefabricated body is densified by CVI or PIP method, thereby realizing SiC w Preparation of SiC composite material. The developed process is suitable for preparing small-size and simple-shape structural parts, and is not suitable for large-size and complex-shape integral turbine discs. The reason is that the gel casting process fixes SiC through the organic three-dimensional network formed by the organic monomer and the cross-linking agent w Powder, thereby realizing SiC w And (5) forming a preform. Glue discharging treatmentFront SiC w Is connected by an organic framework, and no organic matters are used for SiC after the glue discharging treatment w Is (1) SiC w The strength of the prefabricated body is very low only by physical contact and lap joint, the forming stability of the large-size and complex-shape integral turbine disk biscuit is difficult to ensure, and irrecoverable catastrophic damages such as cracking and the like are more likely to occur due to the action of stress in the subsequent processing and densification processes.
Therefore, the strength of the monolithic turbine disk greenbody, i.e., whisker preform, must be increased to avoid cracking problems due to large size and complex structural effects, while further optimizing the subsequent densification process to match the preform structure. In view of the former, we propose a way of pre-strengthening the whisker preform, namely, pre-strengthening firstly gives a certain strength to the preform, so that the blank is supported with enough strength in the subsequent densification process and is not damaged. Aiming at the latter, considering the unavoidable problem of density gradient when preparing thick-wall parts by a Chemical Vapor Infiltration (CVI) method and the problem that the residual silicon content in a matrix prepared by a Reactive Melt Infiltration (RMI) method is difficult to reduce, the densification process of the whole turbine disk adopts a precursor impregnation cracking method (PIP) which has simple and controllable process, short period and low cost. Meanwhile, according to the structural characteristics of the integral turbine disk, the method and the device provide for adjusting the concentration of the impregnating precursor in the PIP process every time, and setting a certain precursor concentration gradient under the whole period to realize the uniform distribution of the ceramic matrix in the whisker preform, so that the problems of difficult densification such as crusting, density difference, closed pore and the like are avoided, and the manufacture of the large-size and complex-shape integral turbine disk is better realized. On the basis, to further match SiC w Excellent temperature resistance and satisfies whole turbine dish superhigh temperature work requirement, this patent proposes carrying out high temperature treatment to combined material behind PIP densification in-process specific heat, alleviates the inside residual stress of material on the one hand, makes the partial closed pore that produces in the schizolysis process change into open pore on the one hand, promotes the infiltration efficiency of follow-up precursor and combined material's density, improves the heat stability of base member on the one hand.
In summary, the invention provides a gel casting process combined with carbothermic recoveryPreparation of SiC by pre-strengthening of original reaction w The biscuit is densified by PIP method to obtain SiC w The SiC composite material integral turbine disk realizes the near-net-size manufacturing of high-performance aeroengine rotating parts.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a method for preparing a silicon carbide-based composite material integral turbine disc based on gel casting pre-strengthening.
Technical proposal
A method for preparing a silicon carbide-based composite material integral turbine disk based on gel casting pre-reinforcement is characterized by comprising the following steps:
step 1, siC w Pretreatment: heating the whisker in a vacuum heat treatment furnace to 1600-1700 ℃, preserving heat for 0.5-1h, cooling to room temperature, soaking the whisker in 9wt.% hydrofluoric acid aqueous solution for 5-10h, washing off the hydrofluoric acid until the pH value is=7, and finally drying the whisker in an oven at 100-150 ℃;
step 2, siC w Shaping a biscuit: 10 to 55wt.% of SiC w And SiC (silicon carbide) w SiO with mass ratio of 13:100 2 0.05 to 0.15wt.% of dispersant ammonium polyacrylate, 4 to 6wt.% of monomer acrylamide AM, 0.3 to 0.5wt.% of cross-linking agent methylene bisacrylamide, and 0.2 to 0.5wt.% of initiator ammonium persulfate APS; and putting the solvent and the pH regulator tetramethylammonium hydroxide into a ball mill for ball milling to obtain uniform slurry; pouring the slurry into a mould of an integral turbine disk by adopting a gel casting process, and placing the mould in an oven at 80-100 ℃ for curing and demoulding to obtain SiC w A biscuit;
step 3, siC w Drying the biscuit: siC is subjected to w Naturally drying the biscuit at room temperature for 48-96h, then drying in a 40 ℃ oven for 12-36h, and raising the temperature to 60-80 ℃ to enable SiC w Fully drying the biscuit;
step 4, siC w Pre-strengthening of the biscuit: siC dried in step 3 w Placing the biscuit into a high-temperature tube furnace for carbothermic reduction reaction, and respectively preserving heat between three gradients of 500 ℃, 1300 ℃ and 1500 DEG CThen cooling to 600 ℃, finally naturally cooling to room temperature, and finally, carrying out SiC reaction on the mixture w Performing preliminary reinforcement on the prefabricated body;
and then preliminary pre-strengthening SiC w The preform is impregnated with sucrose/SiO by vacuum combined with pressurized impregnation 2 Placing the sol mixed solution into a high-temperature tube furnace, respectively preserving heat between three gradients of 500 ℃, 1300 ℃ and 1500 ℃, cooling to 600 ℃, and naturally cooling to room temperature to obtain pre-reinforced SiC w A preform;
step 5, siC w PIP densification of preform: the SiC with certain strength obtained in the step 4 is processed w Precursor concentration gradient PIP densification is carried out on the prefabricated body, the PIP circulation times are immersed in solutions with different precursor concentrations for a plurality of times, meanwhile, after the PIP circulation is carried out for a plurality of times, high-temperature treatment is carried out on the material to improve the open pores and the compactness of the material, and finally, dense SiC is obtained w A SiC monolithic turbine disk; the precursor solution is a mixed solution of PCS and dimethylbenzene, and the mass ratio of the PCS to the dimethylbenzene is 1:5-1.
In the preparation of the slurry in the step 2: siC is subjected to w And SiO 2 Powder and dispersant ammonium polyacrylate PAA-NH 4 Dispersing the pH regulator tetramethylammonium hydroxide TMAH of which the weight percent is less than 3.5 in 35-88 in deionized water, and ball milling for 6-24 hours; then adding monomer acrylamide AM and cross-linking agent methylene bisacrylamide MBAM, and continuing ball milling for 0.5-2 h; adding an initiator ammonium persulfate APS into the obtained slurry, stirring in vacuum for removing bubbles for 20-60 s, vibrating for removing bubbles for 1-3 min, and pouring into a mold; demolding after complete solidification at 80 ℃ to obtain SiC w And (5) biscuit.
The step 4 is characterized in that heat is preserved between three gradients of 500 ℃, 1300 ℃ and 1500 ℃, then the temperature is reduced to 600 ℃, and finally the process of naturally cooling to room temperature is as follows: argon Ar is introduced for protection, the temperature is raised to 500 ℃ from room temperature at 1 ℃/min, then the temperature is raised to 1300 ℃ at 3-5 ℃/min, the heat is preserved for 3-10h, the temperature is raised to 1500 ℃ at 1-3 ℃/min, the heat is preserved for 2-3h, then the temperature is lowered to 600 ℃ at 5 ℃/min, and finally the temperature is naturally cooled to the room temperature.
The method adopting vacuum combined with pressurized impregnation is obtained by preliminary pre-strengtheningSiC w Preform impregnation with sucrose/SiO 2 And (3) carrying out vacuum impregnation on the sol mixed solution for 30min, then carrying out pressurized impregnation for 1-4 h under the pressure of 3MPa, taking out the preform, and drying.
The sucrose/SiO 2 SiO in the sol mixed solution 2 Sol-to-sucrose=11:6 mass ratio.
The PIP densification process in the step 5 is as follows: vacuum-pressure soaking according to the mass ratio of PCS to xylene of 1:5, 1:3 and 1:1 respectively, and heat treating the material at 1500deg.C for 1-2 hr after PIP circulation. Repeating the process to finally obtain compact SiC w SiC monolithic turbine disk.
The PIP densification process in the step 5 is as follows: 1-4 PIP cycles to select 1:5 solution ratio, 5-8 PIP cycles to select 1:3 solution ratio, and 9-12 PIP cycles to select 1:1 solution ratio; the material was subjected to a heat treatment at 1500 ℃ for 1-2h after the 3 rd, 6 th and 9 th PIP cycles.
The pressure impregnation pressure is 3MPa, and the atmosphere is nitrogen N 2 The dipping time is 1-3 h.
Advantageous effects
The invention provides a method for preparing a silicon carbide based composite material integral turbine disk based on gel casting pre-strengthening, which adopts gel casting to prepare SiC by combining carbon thermal reduction pre-strengthening and PIP technology w A method of integrating a turbine disk with SiC composite material. Is required to be in SiC w The temperature gradient is set in the drying process of the biscuit, and the drying time of the corresponding temperature section needs to be strictly controlled. To SiC is required w Pre-strengthening the preform by applying to SiC w Adding proper amount of silicon dioxide particles into gel casting slurry, performing carbothermic reduction reaction on the silicon dioxide particles and carbon remained by organic matters in a vacuum gel discharging stage to form silicon carbide phase, and performing subsequent repeated impregnation of sucrose and silica sol solution and high-temperature carbothermic reduction reaction on SiC w Forming a certain amount of silicon carbide phase in the preform, opposite to SiC w The biscuit has a pre-strengthening effect. In the PIP process, the concentration of the precursor, the cracking temperature, the heating rate and the heat treatment conditions need to be strictly controlled.
The concrete steps are as follows:
1. the invention adopts gel casting technology to prepare the SiC of the integral turbine disk w The preform can utilize organic polymer to perform gel reaction to solidify ceramic particles in situ, thereby realizing the near net size molding of large-scale whisker preforms with complex shapes. The blank formed by the process can keep isotropic characteristics, has good uniformity, and is beneficial to improving the reliability and stability of the component.
2. The invention adopts gel casting technology to prepare the SiC of the integral turbine disk w For the preform, special mention is made of SiC w The biscuit is subjected to gradient temperature drying, namely, the biscuit is firstly dried at room temperature for 48-96h, then dried at 40 ℃ for 12-36h, and finally heated to 60-80 ℃ for drying until the quality is not obviously changed, so that the moisture in the thick-wall part material is sufficiently dried, and deformation and thermal stress accumulation caused by overlarge temperature difference between the inside and the outside of the material are reduced.
3. The core step of the invention is to strengthen the preform by carbothermic reduction process. SiO addition to gel casting slurries 2 The powder is directly carbonized with the organic matters in the preform at high temperature to generate carbothermic reaction to generate silicon carbide; subsequent re-passage of SiC w Preform impregnation with sucrose and SiO 2 And (3) the sol mixed solution is subjected to carbothermic reduction reaction to continuously generate silicon carbide. The silicon carbide matrixes are uniformly dispersed and coated around the whisker, so that the whisker is protected and supported to a certain extent, and the strengthening effect is achieved. The pre-strengthening process of the carbothermic reduction process hardly generates shrinkage or expansion stress, and does not cause cracking of the whole turbine disk. SiC after pre-strengthening w The strength of the preform can be improved from 0.6MPa to 21.4MPa, so that possible deformation and cracking caused by the subsequent PIP shrinkage process are effectively avoided.
4. When PIP is adopted as densification technology, the concentration gradient infiltration method is particularly provided, namely, the concentration of infiltration precursors in different PIP circulation times is adjusted, and a certain precursor concentration gradient is set in the whole period to realize the uniform distribution of the ceramic matrix in the whisker preform. On the basis, the patent also provides that the composite material is subjected to high-temperature treatment after a specific furnace number in the PIP densification process, so that the release is realizedResidual stress in the material, and partial closed pores generated in the cracking process are converted into open pores, so that the infiltration efficiency of the precursor and the compactness of the composite material are improved, and the thermal stability of the matrix is improved. The density of the final composite material can reach 2.63g/cm 3 The open porosity can be reduced to 8 percent, and the bending strength and the fracture toughness can reach 262MPa and 4.62 MPa-m respectively 1/2 。
Drawings
Fig. 1 is a process flow diagram of the present invention.
FIG. 2 shows a pre-strengthened rectangular parallelepiped SiC prepared in example 1 of the present invention w Macroscopic photograph of the preform.
FIG. 3 shows disc-shaped SiC after pre-strengthening, prepared in example 2 of the present invention w Macroscopic photograph of the preform.
FIG. 4 shows pre-strengthened SiC prepared in example 3 of the invention w Preform Scanning Electron Microscope (SEM) photographs.
FIG. 5 is SiC prepared in example 4 of the present invention w Photographs of polished cross sections of the SiC composite integral turbine disk.
Detailed Description
The invention will now be further described with reference to examples, figures:
the method for preparing the silicon carbide-based composite material integral turbine disk based on gel casting pre-reinforcement is characterized by comprising the following steps of:
1.SiC w pretreatment: heating the whisker in a vacuum heat treatment furnace to 1600-1700 ℃, preserving heat for 0.5-1h, cooling to room temperature, soaking the whisker in 9wt.% hydrofluoric acid aqueous solution for 5-10h, washing off the hydrofluoric acid until the pH value is=7, and finally drying the whisker in an oven at 100-150 ℃.
2.SiC w Shaping a biscuit: adopting gel casting technology to obtain SiC obtained in the step 1 w With SiO 2 Placing the powder, the solvent, the pH regulator, the dispersing agent, the monomer and the crosslinking agent into a ball mill for ball milling to obtain uniform slurry, pouring, and placing into an oven at 80-100 ℃ for curing and demoulding to obtain SiC w And (5) biscuit.
3.SiC w Drying the biscuit: the steps are as follows2 SiC obtained w Naturally drying the biscuit at room temperature for 48-96h, then drying in a 40 ℃ oven for 12-36h, and finally raising the temperature to 60-80 ℃ to enable SiC w The biscuit is sufficiently dried until the quality is not obviously changed.
4.SiC w Pre-strengthening of the biscuit: siC obtained in the step 3 w The biscuit is directly put into a high-temperature tube furnace for carbothermic reduction reaction, and the SiC can be reacted by the process w Carbon obtained by carbonizing organic matters in biscuit and SiO in biscuit 2 A small amount of SiC phase is generated by the reaction, and the reaction is carried out on SiC w The preform is initially reinforced. SiC to be preliminarily pre-strengthened w The preform is impregnated with sucrose/SiO by vacuum combined with pressurized impregnation 2 The sol mixed solution is finally subjected to the same high-temperature carbothermic reaction to finally obtain the pre-reinforced SiC w And (3) prefabricating a body.
5.SiC w PIP densification of preform: the SiC with certain strength obtained in the step 4 is processed w Precursor concentration gradient PIP densification is carried out on the prefabricated body, namely solutions with different precursor concentrations are immersed in different PIP circulation times, meanwhile, after PIP circulation is carried out for a certain furnace time, high-temperature treatment is carried out on the material to improve the open pores and the compactness of the material, and finally dense SiC is obtained w SiC monolithic turbine disk.
The gel injection molding process in the step 2 comprises the following steps: 10 to 55wt.% of SiC w And with SiC w The mass ratio is 13:100 SiO 2 Powder, 0.05-0.15 wt.% of dispersant ammonium polyacrylate (PAA-NH) 4 ) 0 to 3.5wt.% of pH regulator tetramethylammonium hydroxide (TMAH) is dispersed in 35 to 88wt.% of deionized water for ball milling for 6 to 24 hours; adding 4-6 wt.% of monomer Acrylamide (AM) and 0.3-0.5 wt.% of cross-linking agent Methylene Bisacrylamide (MBAM) for continuous ball milling for 0.5-2 h; adding 0.2-0.5 wt.% of initiator Ammonium Persulfate (APS) into the obtained slurry, stirring in vacuum for removing bubbles for 20-60 s, vibrating for removing bubbles for 1-3 min, and pouring into a mold; demolding after complete solidification at 80 ℃ to obtain SiC w And (5) biscuit.
Step 3 SiC w The biscuit drying process comprises the following steps: siC obtained in step 2 w The biscuit is self-heated at room temperatureDrying for 48-96h, drying in 40 deg.C oven for 12-36h, and heating to 60-80 deg.C to obtain SiC w The biscuit is sufficiently dried until the quality is not obviously changed.
The pre-strengthening process in the step 4 is as follows: siC obtained in the step 3 w Directly placing the biscuit into a tubular furnace with the caliber larger than the diameter of the biscuit, introducing argon (Ar) for protection, heating from room temperature to 500 ℃ at 1 ℃/min, then heating to 1300 ℃ at 3-5 ℃/min, preserving heat for 3-10h, heating to 1500 ℃ at 1-3 ℃/min, preserving heat for 2-3h, cooling to 600 ℃ at 5 ℃/min, and finally naturally cooling to room temperature. The process can lead SiC to w Carbon obtained by carbonizing organic matters in biscuit and SiO in biscuit 2 A small amount of SiC phase is generated by the reaction, and the reaction is carried out on SiC w The preform is initially reinforced. Then preliminary pre-strengthening the obtained SiC w Preform impregnation of SiO 2 Sol: sucrose = 11:6 mass ratio slurry, adopting a vacuum combined pressurizing and impregnating method, pressurizing and impregnating for 1-4 hours under the pressure of 3MPa after vacuum impregnation for 30min, taking out the preform, and wiping the surface solution with paper towel; finally SiC is added w The prefabricated body is put into a tube furnace to carry out the same high-temperature carbothermic reduction reaction, and finally the pre-reinforced SiC is obtained w And (3) prefabricating a body.
The PIP densification process in step 5 is as follows: the SiC with certain strength obtained in the step 4 is processed w The prefabricated body is subjected to PIP densification, and the concrete process is as follows: preparing PCS: the mass ratio of the dimethylbenzene is 1: 5. 1: 3. 1:1, and vacuum-pressure impregnation was performed according to the formulation sequence. Wherein, the vacuum impregnation method is the same as the step 4, the pressure impregnation pressure is 3MPa, and the atmosphere is nitrogen (N) 2 ) The dipping time is 1-3 h. Proved by a large number of experiments, in order to realize the effective permeation of the precursor solution in the prefabricated body, 1-4 PIP cycles are selected to be 1:5, 5-8 PIP cycles we selected 1:3, 9-12 PIP cycles we selected 1: 1. Meanwhile, in order to improve the density of the matrix, the material is subjected to heat treatment at 1500 ℃ for 1-2h after the 3 rd, 6 th and 9 th PIP cycles. Repeating the process to finally obtain compact SiC w SiC monolithic turbine disk.
Example 1
Step 1.SiC w Pretreatment: the whisker is placed in a vacuum heat treatment furnace, the temperature is raised to 1700 ℃ for 1h, then the whisker is cooled to room temperature, then the whisker is placed in a 9wt.% hydrofluoric acid aqueous solution for soaking for 5h, the hydrofluoric acid is washed to be pH=7, and finally the whisker is placed in an oven for drying at 150 ℃.
Step 2.SiC w Shaping a biscuit: 128g of SiC w 16.64g of SiO 2 Powder, 67.59g deionized water, 0.17g PAA-NH 4 Putting 5.087g of TMAH into a ball milling tank for ball milling for 18 hours, adding 13g of AM and 0.867g of MBAM, and continuing ball milling for 1 hour to obtain slurry with good fluidity; adding 0.54g of APS into the obtained slurry, stirring in vacuum to remove bubbles for 60s, vibrating to remove bubbles for 2min, pouring into a mold, completely curing at 80 ℃, and demolding to obtain SiC w And (5) biscuit.
Step 3.SiC w Drying the biscuit: siC obtained in step 2 w Naturally drying the biscuit at room temperature for 48h, then placing the biscuit into a 40 ℃ oven for drying for 12h, and finally raising the temperature to 80 ℃ to enable the SiC to be dried w The biscuit is fully dried until the quality is not obviously changed.
Step 4.SiC w Pre-strengthening of the preform: siC obtained in the step 3 w Putting the biscuit into a tubular furnace with the caliber larger than the diameter of the biscuit, introducing argon (Ar) for protection, heating from room temperature to 500 ℃ at 1 ℃/min, heating to 1300 ℃ at 3 ℃/min, preserving heat for 3 hours, heating to 1500 ℃ at 3 ℃/min, preserving heat for 2 hours, cooling to 600 ℃ at 5 ℃/min, and naturally cooling to room temperature. The process can lead SiC to w Carbon obtained by carbonizing organic matters in biscuit and SiO in biscuit 2 A small amount of SiC phase is generated by the reaction, and the reaction is carried out on SiC w The preform is initially reinforced. Then preliminary pre-strengthening the obtained SiC w Preform impregnation of SiO 2 Sol: sucrose = 11:6 mass ratio slurry, adopting a vacuum combined pressurizing and impregnating method, pressurizing and impregnating for 1h under the pressure of 3MPa after vacuum impregnation for 30min, taking out the preform, and wiping the surface solution with paper towel; finally SiC is added w The prefabricated body is put into a tube furnace to carry out the same high-temperature carbothermic reduction reaction, and finally the pre-reinforced SiC is obtained w And (3) prefabricating a body.
Step 5.SiC w PIP densification of preform:the SiC with certain strength obtained in the step 4 is processed w The prefabricated body is subjected to PIP densification, and the concrete process is as follows: preparing PCS: the mass ratio of the dimethylbenzene is 1: 5. 1: 3. 1:1, and vacuum-pressure impregnation was performed according to the formulation sequence. Wherein, the vacuum impregnation method is the same as the step 4, the pressure impregnation pressure is 3MPa, and the atmosphere is nitrogen (N) 2 ) The impregnation time was 1h. Proved by a large number of experiments, in order to realize the effective permeation of the precursor solution in the prefabricated body, 1-4 PIP cycles are selected to be 1:5, 5-8 PIP cycles we selected 1:3, 9-12 PIP cycles we selected 1: 1. Meanwhile, in order to improve the density of the matrix, the material is subjected to heat treatment at 1500 ℃ for 1h after PIP circulation for 3 rd, 6 th and 9 th times. The process is repeated to finally obtain the porous material with the porosity of 12.1 percent and the volume density of 2.28g/cm 3 SiC of (2) w SiC monolithic turbine disk.
Example 2
Step 1.SiC w Pretreatment: the whisker is placed in a vacuum heat treatment furnace, the temperature is raised to 1700 ℃ for 1h, then the whisker is cooled to room temperature, then the whisker is placed in a 9wt.% hydrofluoric acid aqueous solution for soaking for 5h, the hydrofluoric acid is washed to be pH=7, and finally the whisker is placed in an oven for drying at 150 ℃.
Step 2.SiC w Shaping a biscuit: 153.6g of SiC are reacted w 19.97g of SiO 2 Powder, 90.27g deionized water and 0.259g PAA-NH 4 Putting 5.895g of TMAH into a ball milling tank for ball milling for 24 hours, adding 14.56g of AM and 0.97g of MBAM, and continuing ball milling for 1 hour to obtain slurry with good fluidity; adding 0.26g of APS into the obtained slurry, stirring in vacuum to remove bubbles for 30s, vibrating to remove bubbles for 3min, pouring into a mold, completely curing at 80 ℃, and demolding to obtain SiC w And (5) biscuit.
Step 3.SiC w Drying the biscuit: siC obtained in step 2 w Naturally drying the biscuit at room temperature for 48h, then placing the biscuit into a 40 ℃ oven for drying for 12h, and finally raising the temperature to 80 ℃ to enable the SiC to be dried w The biscuit is fully dried until the quality is not obviously changed.
Step 4.SiC w Pre-strengthening of the preform: siC obtained in the step 3 w The diameter of the biscuit is larger than that of the biscuitAnd (3) introducing argon (Ar) into a tubular furnace with the diameter for protection, heating from room temperature to 500 ℃ at 1 ℃/min, heating to 1300 ℃ at 5 ℃/min, preserving heat for 3 hours, heating to 1500 ℃ at 1 ℃/min, preserving heat for 2 hours, cooling to 600 ℃ at 5 ℃/min, and naturally cooling to room temperature. The process can lead SiC to w Carbon obtained by carbonizing organic matters in biscuit and SiO in biscuit 2 A small amount of SiC phase is generated by the reaction, and the reaction is carried out on SiC w The preform is initially reinforced. Then preliminary pre-strengthening the obtained SiC w Preform impregnation of SiO 2 Sol: sucrose = 11:6 mass ratio slurry, adopting a vacuum combined pressurizing and impregnating method, pressurizing and impregnating for 2 hours under the pressure of 3MPa after vacuum impregnation for 30 minutes, taking out the preform, and wiping the surface solution with paper towel; finally SiC is added w The prefabricated body is put into a tube furnace to carry out the same high-temperature carbothermic reduction reaction, and finally the pre-reinforced SiC is obtained w And (3) prefabricating a body.
Step 5.SiC w PIP densification of preform: the SiC with certain strength obtained in the step 4 is processed w The prefabricated body is subjected to PIP densification, and the concrete process is as follows: preparing PCS: the mass ratio of the dimethylbenzene is 1: 5. 1: 3. 1:1, and vacuum-pressure impregnation was performed according to the formulation sequence. Wherein, the vacuum impregnation method is the same as the step 4, the pressure impregnation pressure is 3MPa, and the atmosphere is nitrogen (N) 2 ) The impregnation time was 2h. Proved by a large number of experiments, in order to realize the effective permeation of the precursor solution in the prefabricated body, 1-4 PIP cycles are selected to be 1:5, 5-8 PIP cycles we selected 1:3, 9-12 PIP cycles we selected 1: 1. Meanwhile, in order to improve the density of the matrix, the material is subjected to heat treatment at 1500 ℃ for 1h after PIP circulation for 3 rd, 6 th and 9 th times. The process is repeated to finally obtain the porous material with the porosity of 16.2 percent and the volume density of 2.21g/cm 3 SiC of (2) w SiC monolithic turbine disk.
Example 3
Step 1.SiC w Pretreatment: heating the whisker in a vacuum heat treatment furnace to 1700 ℃, preserving heat for 1h, cooling to room temperature, soaking the whisker in 9wt.% hydrofluoric acid aqueous solution for 5h, washing off the hydrofluoric acid until the pH value is 7, and finally placing the whisker in an oven at 150 DEG CAnd (5) drying.
Step 2.SiC w Shaping a biscuit: 42.67g of SiC was added w 5.547g of SiO 2 Powder, 22.53g deionized water, 0.057g PAA-NH 4 Putting 1.696g of TMAH into a ball milling tank for ball milling for 8 hours, adding 4.33g of AM and 0.289g of MBAM, and continuing ball milling for 1 hour to obtain slurry with good fluidity; adding 0.18g of APS into the obtained slurry, stirring in vacuum to remove bubbles for 20s, vibrating to remove bubbles for 3min, pouring into a mold, completely curing at 80 ℃, and demolding to obtain SiC w And (5) biscuit.
Step 3.SiC w Drying the biscuit: siC obtained in step 2 w Naturally drying the biscuit at room temperature for 48h, then placing the biscuit into a 40 ℃ oven for drying for 12h, and finally raising the temperature to 80 ℃ to enable the SiC to be dried w The biscuit is fully dried until the quality is not obviously changed.
Step 4.SiC w Pre-strengthening of the preform: siC obtained in the step 3 w Putting the biscuit into a tubular furnace with the caliber larger than the diameter of the biscuit, introducing argon (Ar) for protection, heating from room temperature to 500 ℃ at 1 ℃/min, heating to 1300 ℃ at 3 ℃/min, preserving heat for 3 hours, heating to 1500 ℃ at 3 ℃/min, preserving heat for 2 hours, cooling to 600 ℃ at 5 ℃/min, and naturally cooling to room temperature. The process can lead SiC to w Carbon obtained by carbonizing organic matters in biscuit and SiO in biscuit 2 A small amount of SiC phase is generated by the reaction, and the reaction is carried out on SiC w The preform is initially reinforced. Then preliminary pre-strengthening the obtained SiC w Preform impregnation of SiO 2 Sol: sucrose = 11:6 mass ratio slurry, adopting a vacuum combined pressurizing and impregnating method, pressurizing and impregnating for 3 hours under the pressure of 3MPa after vacuum impregnation for 30 minutes, taking out the preform, and wiping the surface solution with paper towel; finally SiC is added w The prefabricated body is put into a tube furnace to carry out the same high-temperature carbothermic reduction reaction, and finally the pre-reinforced SiC is obtained w And (3) prefabricating a body.
Step 5.SiC w PIP densification of preform: the SiC with certain strength obtained in the step 4 is processed w The prefabricated body is subjected to PIP densification, and the concrete process is as follows: preparing PCS: the mass ratio of the dimethylbenzene is 1: 5. 1: 3. 1:1, and vacuum-pressure impregnation was performed according to the formulation sequence. Wherein, vacuum impregnationThe method is the same as that in the step 4, the pressure impregnation pressure is 3MPa, and the atmosphere is nitrogen (N) 2 ) The impregnation time was 3 hours. Proved by a large number of experiments, in order to realize the effective permeation of the precursor solution in the prefabricated body, 1-4 PIP cycles are selected to be 1:5, 5-8 PIP cycles we selected 1:3, 9-12 PIP cycles we selected 1: 1. Meanwhile, in order to improve the density of the matrix, the material is subjected to heat treatment at 1500 ℃ for 1h after PIP circulation for 3 rd, 6 th and 9 th times. The process is repeated to finally obtain the porous material with the porosity of 8.17 percent and the volume density of 2.31g/cm 3 SiC of (2) w SiC monolithic turbine disk.
Example 4
Step 1.SiC w Pretreatment: the whisker is placed in a vacuum heat treatment furnace, the temperature is raised to 1700 ℃ for 1h, then the whisker is cooled to room temperature, then the whisker is placed in a 9wt.% hydrofluoric acid aqueous solution for soaking for 5h, the hydrofluoric acid is washed to be pH=7, and finally the whisker is placed in an oven for drying at 150 ℃.
Step 2.SiC w Shaping a biscuit: 200g of SiC w 26g of SiO 2 Powder, 105.6g deionized water, 0.266g PAA-NH 4 Putting 7.948g of TMAH into a ball milling tank for ball milling for 24 hours, then adding 20.31g of AM and 1.355g of MBAM, and continuing ball milling for 1 hour to obtain slurry with good fluidity; adding 0.844g of APS into the obtained slurry, stirring in vacuum to remove bubbles for 60s, vibrating to remove bubbles for 3min, pouring into a mold, completely curing at 80 ℃, and demolding to obtain SiC w And (5) biscuit.
Step 3.SiC w Drying the biscuit: siC obtained in step 2 w Naturally drying the biscuit at room temperature for 48h, then placing the biscuit into a 40 ℃ oven for drying for 12h, and finally raising the temperature to 80 ℃ to enable the SiC to be dried w The biscuit is fully dried until the quality is not obviously changed.
Step 4.SiC w Pre-strengthening of the preform: siC obtained in the step 3 w Directly placing the biscuit into a tubular furnace with the caliber larger than the diameter of the biscuit, introducing argon (Ar) for protection, heating from room temperature to 500 ℃ at 1 ℃/min, then heating to 1300 ℃ at 3 ℃/min, preserving heat for 3 hours, heating to 1500 ℃ at 1 ℃/min, preserving heat for 2 hours, cooling to 600 ℃ at 5 ℃/min, and finally naturally cooling to room temperature. Above-mentionedThe process can make SiC w Carbon obtained by carbonizing organic matters in biscuit and SiO in biscuit 2 A small amount of SiC phase is generated by the reaction, and the reaction is carried out on SiC w The preform is initially reinforced. Then preliminary pre-strengthening the obtained SiC w Preform impregnation of SiO 2 Sol: sucrose = 11:6 mass ratio slurry, adopting a vacuum combined pressurizing and impregnating method, pressurizing and impregnating for 2 hours under the pressure of 3MPa after vacuum impregnation for 30 minutes, taking out the preform, and wiping the surface solution with paper towel; finally SiC is added w The prefabricated body is put into a tube furnace to carry out the same high-temperature carbothermic reduction reaction, and finally the pre-reinforced SiC is obtained w And (3) prefabricating a body.
Step 5.SiC w PIP densification of preform: the SiC with certain strength obtained in the step 4 is processed w The prefabricated body is subjected to PIP densification, and the concrete process is as follows: preparing PCS: the mass ratio of the dimethylbenzene is 1: 5. 1: 3. 1:1, and vacuum-pressure impregnation was performed according to the formulation sequence. Wherein, the vacuum impregnation method is the same as the step 4, the pressure impregnation pressure is 3MPa, and the atmosphere is nitrogen (N) 2 ) The impregnation time was 2h. Proved by a large number of experiments, in order to realize the effective permeation of the precursor solution in the prefabricated body, 1-4 PIP cycles are selected to be 1:5, 5-8 PIP cycles we selected 1:3, 9-12 PIP cycles we selected 1: 1. Meanwhile, in order to improve the density of the matrix, the material is subjected to heat treatment at 1500 ℃ for 1h after PIP circulation for 3 rd, 6 th and 9 th times. The process is repeated to finally obtain the porous material with the porosity of 13.46 percent and the volume density of 2.20g/cm 3 SiC of (2) w SiC monolithic turbine disk.
Claims (5)
1. A method for preparing a silicon carbide-based composite material integral turbine disk based on gel casting pre-reinforcement is characterized by comprising the following steps:
step 1, siC w Pretreatment: heating the whisker in a vacuum heat treatment furnace to 1600-1700 ℃, preserving heat for 0.5-1h, cooling to room temperature, soaking the whisker in 9wt.% hydrofluoric acid aqueous solution for 5-10h, washing off the hydrofluoric acid until the pH value is=7, and finally drying the whisker in an oven at 100-150 ℃;
step 2, siC w Shaping a biscuit: 10 to 55wt.% of SiC w And SiC (silicon carbide) w SiO with mass ratio of 13:100 2 0.05 to 0.15wt.% of dispersant ammonium polyacrylate, 4 to 6wt.% of monomer acrylamide AM, 0.3 to 0.5wt.% of cross-linking agent methylene bisacrylamide, and 0.2 to 0.5wt.% of initiator ammonium persulfate APS; and
putting the solvent and the pH regulator tetramethylammonium hydroxide into a ball mill for ball milling to obtain uniform slurry; pouring the slurry into a die of an integral turbine disk by adopting a gel casting process, and placing the die in an oven at 80-100 ℃ for curing and demolding to obtain SiC w A biscuit;
step 3, siC w Drying the biscuit: siC is subjected to w Naturally drying the biscuit at room temperature for 48-96h, then drying in a 40 ℃ oven for 12-36h, and raising the temperature to 60-80 ℃ to enable SiC w Fully drying the biscuit;
step 4, siC w Pre-strengthening of the biscuit: siC dried in step 3 w Placing the biscuit into a high-temperature tube furnace for carbothermic reaction, respectively preserving heat between three gradients of 500 ℃, 1300 ℃ and 1500 ℃, then cooling to 600 ℃, finally naturally cooling to room temperature, and finally carrying out SiC reaction on the biscuit w Performing preliminary reinforcement on the prefabricated body;
and then preliminary pre-strengthening SiC w The preform is impregnated with sucrose/SiO by vacuum combined with pressurized impregnation 2 Placing the sol mixed solution into a high-temperature tube furnace, respectively preserving heat between three gradients of 500 ℃, 1300 ℃ and 1500 ℃, cooling to 600 ℃, and naturally cooling to room temperature to obtain pre-reinforced SiC w A preform;
the process of preserving heat between three gradients of 500 ℃, 1300 ℃ and 1500 ℃, then cooling to 600 ℃ and finally naturally cooling to room temperature is as follows: argon Ar is introduced for protection, the temperature is raised to 500 ℃ from room temperature at 1 ℃/min, then the temperature is raised to 1300 ℃ at 3-5 ℃/min, the heat is preserved for 3-10 hours, the temperature is raised to 1500 ℃ at 1-3 ℃/min, the temperature is lowered to 600 ℃ at 5 ℃/min, and finally the temperature is naturally cooled to the room temperature;
step 5, siC w PIP densification of preform: the SiC with certain strength obtained in the step 4 is processed w Precursor concentration gradient PIP densification is carried out on the prefabricated body, the PIP circulation times are immersed in solutions with different precursor concentrations for a plurality of times, meanwhile, after the PIP circulation is carried out for a plurality of times, high-temperature treatment is carried out on the material to improve the open pores and the compactness of the material, and finally, dense SiC is obtained w A SiC monolithic turbine disk; the precursor solution is a mixed solution of PCS and dimethylbenzene, and the mass ratio of the PCS to the dimethylbenzene is 1:5-1 respectively;
the PIP densification process comprises the following steps: vacuum-pressure soaking according to the mass ratio of PCS to xylene of 1:5, 1:3 and 1:1 respectively, heat treating material at 1500deg.C for 1-2 hr after PIP circulation, and repeating the process to obtain compact SiC w A SiC monolithic turbine disk; the method comprises the following steps: 1-4 PIP cycles to select 1:5 solution ratio, 5-8 PIP cycles to select 1:3 solution ratio, and 9-12 PIP cycles to select 1:1 solution ratio; the material was subjected to a heat treatment at 1500 ℃ for 1-2h after the 3 rd, 6 th and 9 th PIP cycles.
2. The method for preparing the silicon carbide based composite integral turbine disk based on gel casting pre-strengthening as recited in claim 1, wherein: in the preparation of the slurry in the step 2: siC is subjected to w And SiO 2 Powder and dispersant ammonium polyacrylate PAA-NH 4 Dispersing the pH regulator tetramethylammonium hydroxide TMAH of which the weight percent is less than 3.5 in 35-88 in deionized water, and ball milling for 6-24 hours; then adding monomer acrylamide AM and cross-linking agent methylene bisacrylamide MBAM, and continuing ball milling for 0.5-2 h; adding an initiator ammonium persulfate APS into the obtained slurry, stirring in vacuum for removing bubbles for 20-60 s, vibrating for removing bubbles for 1-3 min, and pouring into a mold; demolding after complete solidification at 80 ℃ to obtain SiC w And (5) biscuit.
3. The method for preparing the silicon carbide based composite integral turbine disk based on gel casting pre-strengthening as recited in claim 1, wherein: the method for adopting vacuum combined pressurized impregnation is to pre-strengthen the obtained SiC w Preform impregnation with sucrose/SiO 2 Mixing the sol and the solution, vacuum soaking for 30min, and pressing at 3MPaAnd (5) immersing for 1-4 hours under pressure, taking out the preform, and drying.
4. The method for preparing the silicon carbide based composite integral turbine disk based on gel casting pre-strengthening as recited in claim 1, wherein: the sucrose/SiO 2 SiO in the sol mixed solution 2 Sol-to-sucrose=11:6 mass ratio.
5. The method for preparing the silicon carbide based composite integral turbine disk based on gel casting pre-strengthening as recited in claim 1, wherein: the pressure impregnation pressure is 3MPa, and the atmosphere is nitrogen N 2 The dipping time is 1-3 h.
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