CN103724032B - A kind of two-dimensional fiber cloth strengthens silicon nitride-silicon carbide ceramic composite and preparation method thereof - Google Patents
A kind of two-dimensional fiber cloth strengthens silicon nitride-silicon carbide ceramic composite and preparation method thereof Download PDFInfo
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Abstract
A kind of two-dimensional fiber cloth strengthens silicon nitride-silicon carbide ceramic matric composite and preparation method thereof, the feature of this matrix material is that matrix is the hybrid ceramic of silicon nitride and silicon carbide, strongthener is carbon cloth or silicon carbide fiber cloth, and the volume fraction of strongthener is 30 ~ 45%.Preparation method be by silica flour and carborundum powder are added water and tackiness agent make mud, pretreated two-dimensional fiber cloth floods for some time in the slurry, is wound on mould after midge, dries, then nitriding treatment, last densification matrix material just obtains this matrix material.This processing method preparation cost is low, and the cycle is short.The two-dimensional fiber cloth that obtained by this processing method strengthens silicon nitride-silicon carbide ceramic matric composite, and to have thermal expansivity low, good in thermal shock, intensity and the high advantage of density.
Description
Technical field
The present invention relates to a kind of ceramic matric composite and preparation method thereof, particularly relate to a kind of two-dimensional fiber cloth and strengthen silicon nitride-silicon carbide ceramic composite and preparation method thereof.
Background technology
Silicon nitride ceramics thermal expansivity (CTE) is 2.5 ~ 3.0 × 10
-6/ K, thermal conductivity 18.4w/mK, thermal expansion is low, and thermal conductivity is high, thus makes its thermal shock resistance very excellent.Silicon nitride ceramics has high strength, high rigidity, erosion resistant, anti-oxidant and good heat shock resistance and mechanical shock performance, is once thought high comprehensive performance in structural ceramics field by material supply section educational circles, is hopeful a kind of type material that alternative nickel-base alloy obtains widespread use in high-tech, high-temperature field most.But there is creep at 1200 DEG C in it, brittle ductile transition temperature is low, is difficult to use in the condition of high temperature separately.
Silicon carbide ceramics CTE is 4 ~ 5 × 10
-6/ K, more than 1600 DEG C still have high intensity, are one of potteries that current high-temperature behavior of generally acknowledging is the most excellent, are widely used as the body material etc. of bulletproof ceramic plate, Neodymium iron boron magnetic functional materials sintering refractory slab, ceramic matric composite.
Application number be 200810030554.0 Chinese patent disclose a kind of two-dimensional fiber cloth reinforced composite material and preparation technology thereof, this matrix material is for wild phase with two-dimensional fiber cloth, with ceramic powder or refractory metal powder for filler, with carbon, silicon carbide etc. for matrix, contain the slurry of different ceramic powder and metal-powder by first brushing on two-dimensional fiber cloth, then carry out the processing step such as lamination, the puncture of puncture fiber, repeatedly densification and prepare described two-dimensional fiber cloth reinforced composite material.This matrix material interlayer shearing resistance is high, Stability Analysis of Structures, reliability are high.But because the difference of thermal expansion coefficient of two-dimensional fiber cloth and carbon, silicon carbide is larger, thermal shocking process easily causes the increase of interfacial thermal stress peak value to cause material thermal damage, the large thermal stresses peak value that interface produces in addition makes interface bond strength increase, run counter to the principle of design at ceramic matric composite weak binding interface, thus brittle rupture may occur.
The Chinese patent of application number 200810030555.5 discloses a kind of refractory ceramics based composites and preparation method thereof, this matrix material is for wild phase with carbon cloth or boron nitride fibre cloth, with high-melting-point ceramic powder or refractory metal powder for filler, with carbon or silicon carbide for matrix.By by sizing agent and powder stuffing mixing and ball milling, by the slurry brushing that obtains after ball milling in wild phase cloth, then obtain this matrix material through the step such as lamination, mold pressing, crosslinked, Pintsch process, repeatedly densification.Although this matrix material has, thermal shock resistance excellence, density are low, the advantages such as ablation rate is low in hyperthermal environments.But have carborundum-based ceramic material high temperature to still have very high strength, fragility is large.Therefore this composite material toughness is not enough, high temperature fracture should diminish, and easily brittle rupture occurs.
And silicon nitride-silicon carbide complex phase ceramic has higher than silicon nitride CTE, the feature lower than silicon carbide CTE, the heat expansion difference between carbon fiber and matrix can be reduced as ceramic matric composite matrix, thus reduce the interfacial thermal stress peak value of matrix material, improve the thermal shock resistance of ceramic matric composite.In addition, silicon nitride brittle ductile transition temperature 1200 DEG C, thus more than 1200 DEG C, hard and crisp single silicon nitride matrix may have certain toughness, is combined with to be beneficial to improves matrix material high temperature fracture and strain and work of rupture with silicon carbide.
Summary of the invention
The technical problem to be solved in the present invention overcomes the deficiencies in the prior art, a kind of two-dimensional fiber cloth is provided to strengthen silicon nitride-silicon carbide ceramic composite, it is characterized in that using the hybrid ceramic of silicon carbide and silicon nitride as matrix, using carbon cloth or silicon carbide fiber cloth as wild phase, cloth of reinforcement fibers volume fraction is 30 ~ 45%.
For solving the problems of the technologies described above, a kind of two-dimensional fiber cloth is provided to strengthen the preparation method of silicon nitride-silicon carbide ceramic composite.It is characterized in that, comprise the preparation process of following order:
1. silica flour and carborundum powder add water and tackiness agent make mud;
2. carbon cloth or silicon carbide fiber cloth carry out pre-treatment, in vacuum or rare gas element, put into High Temperature Furnaces Heating Apparatus and heat up 600 ~ 800 DEG C, be incubated 40 ~ 80 minutes, cool for subsequent use to room temperature after taking-up;
3. pretreated carbon cloth or silicon carbide fiber cloth are put into vacuum impregnation and are filled with, after vacuumizing, carbon cloth or silicon carbide fiber cloth are immersed in the mud of body material, flood 5 ~ 30 minutes, in the process of dipping, body material is deep in carbon cloth or silicon carbide fiber cloth lentamente;
4. the carbon cloth after midge or silicon carbide fiber cloth are wound on mould, dry in 110 ~ 150 DEG C of baking ovens;
5. then carry out nitriding treatment, nitriding process is 1100 ~ 1300 DEG C of preliminary nitrogenize, and 1350-1450 DEG C of secondary nitrogenize obtains, and has the low advantage of sintering temperature with pure silicon nitride ceramic powder compared with sintering;
6. finally by chemical vapor infiltration (CVI) technique, densification is carried out to matrix material, CVI silicon carbide is carried out to CMC, CVI20 ~ 30 hour, obtain densification two-dimensional fiber cloth and strengthen silicon nitride-silicon carbide ceramic matric composite.
The invention has the advantages that: 1. with silicon nitride and carborundum composite-phase ceramic for body material, improve matrix material high temperature toughness; 2. matrix material of the present invention has that thermal expansivity is low, good in thermal shock, intensity advantages of higher; 3. preparation cost is low, and the cycle is short.
Embodiment
Below in conjunction with specific embodiment, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims and limited.
Embodiment 1
1. silica flour and carborundum powder add water and tackiness agent make mud;
2. carbon cloth or silicon carbide fiber cloth carry out pre-treatment, in vacuum or rare gas element, put into High Temperature Furnaces Heating Apparatus and heat up 600 DEG C, be incubated 80 minutes, cool for subsequent use to room temperature after taking-up;
3. pretreated carbon cloth or silicon carbide fiber cloth are put into vacuum impregnation and are filled with, after vacuumizing, carbon cloth or silicon carbide fiber cloth are immersed in the mud of body material, flood 15 minutes, in the process of dipping, body material is deep in carbon cloth or silicon carbide fiber cloth lentamente;
4. the carbon cloth after midge or silicon carbide fiber cloth are wound on mould, dry in 110 DEG C of baking ovens;
5. then carry out nitriding treatment, nitriding process is 1250 DEG C of preliminary nitrogenize, and 1400 DEG C of secondary nitrogenize obtain, and have the low advantage of sintering temperature with pure silicon nitride ceramic powder compared with sintering;
6. finally by chemical vapor infiltration (CVI) technique, densification is carried out to matrix material, CVI silicon carbide is carried out to CMC, CVI20 hour, obtain densification two-dimensional fiber cloth and strengthen silicon nitride-silicon carbide ceramic matric composite.
Embodiment 2
1. silica flour and carborundum powder add water and tackiness agent make mud;
2. carbon cloth or silicon carbide fiber cloth carry out pre-treatment, in vacuum or rare gas element, put into High Temperature Furnaces Heating Apparatus and heat up 800 DEG C, be incubated 60 minutes, cool for subsequent use to room temperature after taking-up;
3. pretreated carbon cloth or silicon carbide fiber cloth are put into vacuum impregnation and are filled with, after vacuumizing, carbon cloth or silicon carbide fiber cloth are immersed in the mud of body material, flood 30 minutes, in the process of dipping, body material is deep in carbon cloth or silicon carbide fiber cloth lentamente;
4. the carbon cloth after midge or silicon carbide fiber cloth are wound on mould, dry in 150 DEG C of baking ovens;
5. then carry out nitriding treatment, nitriding process is 1200 DEG C of preliminary nitrogenize, and 1450 DEG C of secondary nitrogenize obtain, and have the low advantage of sintering temperature with pure silicon nitride ceramic powder compared with sintering;
6. finally by chemical vapor infiltration (CVI) technique, densification is carried out to matrix material, CVI silicon carbide is carried out to CMC, CVI25 hour, obtain densification two-dimensional fiber cloth and strengthen silicon nitride-silicon carbide ceramic matric composite.
Above are only two embodiments of the present invention, but design concept of the present invention is not limited thereto, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should belong to the behavior of invading the scope of protection of the invention.In every case be the content not departing from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (1)
1. a preparation method for the silicon nitride-silicon carbide ceramic matric composite of two-dimensional fiber cloth enhancing, is characterized in that, comprise the preparation process of following order:
1. silica flour and carborundum powder add water and tackiness agent make mud;
2. carbon fiber or silicon carbide fiber cloth carry out pre-treatment, in vacuum or rare gas element, put into High Temperature Furnaces Heating Apparatus and heat up 600 ~ 800 DEG C, be incubated 40 ~ 80 minutes, cool for subsequent use to room temperature after taking-up;
3. pretreated carbon fiber or silicon carbide fiber cloth are put into vacuum impregnation and are filled with, after vacuumizing, carbon fiber or silicon carbide fiber cloth are immersed in the mud of body material, flood 5 ~ 30 minutes, in the process of dipping, body material is deep in carbon fiber or silicon carbide fiber cloth lentamente;
4. the carbon fiber after midge or silicon carbide fiber cloth are wound on mould, dry in 110 ~ 150 DEG C of baking ovens;
5. then carry out nitriding treatment, nitriding process is 1100 ~ 1300 DEG C of preliminary nitrogenize, and 1350-1450 DEG C of secondary nitrogenize obtains, and has the low advantage of sintering temperature with pure silicon nitride ceramic powder compared with sintering;
6. finally by chemical vapor infiltration (CVI) technique, densification is carried out to matrix material, CVI silicon carbide is carried out to CMC, CVI20 ~ 30 hour, obtain densification two-dimensional fiber cloth and strengthen silicon nitride-silicon carbide ceramic matric composite.
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| CN104961477A (en) * | 2015-06-10 | 2015-10-07 | 马鞍山金晟工业设计有限公司 | Modified fiber refractory material and preparation method thereof |
| CN105481451B (en) * | 2016-01-11 | 2018-06-26 | 山东理工大学 | Close the preparation method of fat dispersion hafnium boride boron carbide-carbon fiber friction material |
| TWI602794B (en) * | 2016-03-14 | 2017-10-21 | National Chung-Shan Institute Of Science And Tech | Ceramic composite materials production methods |
| CN106007764B (en) * | 2016-04-22 | 2019-02-15 | 苏州宏久航空防热材料科技有限公司 | A kind of two-dimensional fiber cloth enhancing silicon carbide-diamond composite preparation method |
| CN106747546A (en) * | 2016-12-04 | 2017-05-31 | 淄博精诚专利信息咨询有限公司 | A kind of high-strength and high ductility ceramic composite and its application |
| CN109721377B (en) * | 2019-01-30 | 2020-06-30 | 湖南兴晟新材料科技有限公司 | Carbon fiber reinforced silicon carbide ceramic matrix composite and preparation method thereof |
| CN114645226B (en) * | 2020-12-21 | 2023-04-14 | 南京航空航天大学 | Unidirectional laminated structure carbon fiber reinforced silicon carbide/aluminum-based composite material and preparation method thereof |
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