CN1377855A - Process for preparing C/C composite material fastly using super critical fluid technology - Google Patents
Process for preparing C/C composite material fastly using super critical fluid technology Download PDFInfo
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- CN1377855A CN1377855A CN 02114554 CN02114554A CN1377855A CN 1377855 A CN1377855 A CN 1377855A CN 02114554 CN02114554 CN 02114554 CN 02114554 A CN02114554 A CN 02114554A CN 1377855 A CN1377855 A CN 1377855A
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Abstract
The present invention provides a supercritical fluid technological process of preparing C/C composite material fast. On the basis of chemical liquid-gas phase deposition process to prepare composite C/C material, supercritical fluid technology is introduced to infiltrate fine SiC or C grains into the surface and interior of porous prefabricated C/C material body and through crakcing C/C omposite material is prepared with strong antioxidant performance, excellent friction and wear performance and homogeneous density of 1.75-1.85 g/cu cm. The process has short period and low cost, and may be used in preparing other densified porous composite material.
Description
One, affiliated field
The present invention relates to a kind of quick preparation of matrix material, particularly a kind of using super critical fluid technology prepares the method for C/C matrix material fast.
Two, background technology
Preparation C/C matrix material, external research and application are all Zao than China, as, United States Patent (USP) (U.S.Patent:5035921) discloses and a kind of supercritical fluid technology is used for the C/C composite material and preparation method thereof, the technical scheme that this United States Patent (USP) adopts is impregnation technology repeatedly, be that Polycarbosilane, polysilane, hexyl silicon borine etc. are dissolved in the supercutical fluid, changing temperature or pressure makes its infiltration in the porous precast body, through 3~6 times the dipping, cure cycle, cracking obtains the C/C matrix material.
But, United States Patent (USP) (U.S.Patent:5035921) is impregnation technology repeatedly, Zhi Bei the C/C matrix material cycle is longer in this way, energy consumption is big, and cost is higher, for this reason, adopt supercritical fluid technology, in conjunction with fast densified metallization processes, both can shorten preparation time greatly, make the C/C matrix material of acquisition have higher density again.
Three, summary of the invention
Defective or deficiency according to above-mentioned prior art exists the objective of the invention is, and provide a kind of using super critical fluid technology to prepare the method for C/C matrix material fast.
To achieve these goals, the technical solution used in the present invention is, using super critical fluid technology prepares the method for C/C matrix material fast, be characterized in, tiny SiC or C particulate etc. is dissolved in the supercutical fluid, makes its infiltration in the C/C precast body, again in conjunction with chemical liquids-gas-phase deposition by adjusting temperature or pressure, carry out fast deposition, whole process is only carried out once; The detailed process step is as follows:
1) with micron or nano level SiC or C particles dispersed in polysiloxane solution;
2) mixing solutions is packed in the pressurized vessel, feed propane gas and sealed vessel;
3) speed with 1 ℃/min~5 ℃/min, 50kPa~200kPa heats up respectively, pressurizes, and temperature to 90 ℃~150 ℃, pressure can observe propane and reach the supercutical fluid state during to 4000kPa~9000kPa.
4) under the supercutical fluid state, keep 0.5hour~10hour, again with the speed cooling of 1 ℃/min~5 ℃/min, or with the speed step-down of 20kPa~100kPa, or decrease temperature and pressure simultaneously, make the infiltration of SiC or C particulate in the prefabricated intravital space of C/C;
5) with in low hydrocarbon solution (kerosene, hexanaphthene etc.) the homemade rapid chemical liquid-vapour deposition container of packing into of liquid state, again micron or nano level SiC or C powder are scattered in the low hydrocarbon solution, after machinery or ultrasonic stirring, the C/C precast body of packing into and infiltrating, vacuumize after the sealing, vacuum tightness is-200kPa;
6) adjust the load coil frequency, temperature rises to 900 ℃~1500 ℃ rapidly in 3min~8min, makes the precast body surfaces externally and internally form big thermograde;
7) at state 6) keep 0.5hour~2hour down, make the SiC or the C particulate cracking deposition of infiltration;
8) reduce the heating element temperature to room temperature, take out the C/C material;
9) with the C/C material under 2300 ℃ of-2600 ℃ of conditions, insulation 1hour heat-treats, and makes its greying, final obtains fine and close C/C matrix material.
Adopt the C/C composite density of the present invention's preparation can reach 1.75g/cm
3~1.85g/cm
3, 2D C/C material open porosity is below 5%, and the material preparation time is 20 to thirties hours, has shortened preparation cycle greatly, has reduced cost, and material structure is comparatively fine and close.According to the quick method for preparing the C/C matrix material of the present invention, both can shorten preparation time greatly, make the C/C matrix material of acquisition have higher density again.
Four, embodiment
The contriver has provided following embodiment, and the present invention is described in further detail below in conjunction with embodiment, but the invention is not restricted to these embodiment.
Embodiment 1: according to technical scheme of the present invention, using super critical fluid technology prepares the method for C/C matrix material fast, tiny SiC or C particulate etc. is dissolved in the supercutical fluid, make its infiltration in the C/C precast body by adjusting temperature or pressure, again in conjunction with chemical liquids-gas-phase deposition, carry out fast deposition, whole process is only carried out once; The detailed process step is as follows:
1) with micron or nano level SiC or C particles dispersed in polysiloxane solution;
2) mixing solutions is packed in the pressurized vessel, feed propane gas and sealed vessel;
3) speed with 1 ℃/min, 50kPa heats up respectively, pressurizes, and temperature to 90 ℃, pressure can observe propane and reach the supercutical fluid state during to 9000kPa;
4) under the supercutical fluid state, keep 10hour, again with the cooling of the speed of 1 ℃/min, or with the speed step-down of 20kPa, or decrease temperature and pressure simultaneously, make the infiltration of SiC or C particulate in the prefabricated intravital space of C/C;
5) with in low hydrocarbon solution (kerosene, hexanaphthene etc.) the homemade rapid chemical liquid-vapour deposition container of packing into of liquid state, again micron or nano level SiC or C powder are scattered in the low hydrocarbon solution, after machinery or ultrasonic stirring, the C/C precast body of packing into and infiltrating, vacuumize after the sealing, vacuum tightness is-200kPa;
6) adjust the load coil frequency, temperature rises to 900 ℃ rapidly in the 3min, makes the precast body surfaces externally and internally form big thermograde;
7) at state 6) keep 2hour down, make the SiC or the C particulate cracking deposition of infiltration;
8) reduce the heating element temperature to room temperature, take out the C/C material;
9) with the C/C material under 2600 ℃ of conditions, insulation 1hour heat-treats, and makes its greying, final obtains fine and close C/C matrix material.
Embodiment 2: according to technical scheme of the present invention, using super critical fluid technology prepares the method for C/C matrix material fast, tiny SiC or C particulate etc. is dissolved in the supercutical fluid, make its infiltration in the C/C precast body by adjusting temperature or pressure, again in conjunction with chemical liquids-gas-phase deposition, carry out fast deposition, whole process is only carried out once; The detailed process step is as follows:
1) with micron or nano level SiC or C particles dispersed in polysiloxane solution;
2) mixing solutions is packed in the pressurized vessel, feed propane gas and sealed vessel;
3) speed with 5 ℃/min, 200kPa heats up respectively, pressurizes, and temperature to 150 ℃, pressure can observe propane and reach the supercutical fluid state during to 4000kPa;
4) under the supercutical fluid state, keep 0.5hour, again with the cooling of the speed of 5 ℃/min, or with the speed step-down of 100kPa, or decrease temperature and pressure simultaneously, make the infiltration of SiC or C particulate in the prefabricated intravital space of C/C;
5) with in low hydrocarbon solution (kerosene, hexanaphthene etc.) the homemade rapid chemical liquid-vapour deposition container of packing into of liquid state, again micron or nano level SiC or C powder are scattered in the low hydrocarbon solution, after machinery or ultrasonic stirring, the C/C precast body of packing into and infiltrating, vacuumize after the sealing, vacuum tightness is-200kPa;
6) adjust the load coil frequency, temperature rises to 1500 ℃ rapidly in the 8min, makes the precast body surfaces externally and internally form big thermograde;
7) at state 6) keep 0.5hour down, make the SiC or the C particulate cracking deposition of infiltration;
8) reduce the heating element temperature to room temperature, take out the C/C material;
9) with the C/C material under 2300 ℃ of conditions, insulation 1hour heat-treats, and makes its greying, final obtains fine and close C/C matrix material.
Embodiment 3: according to technical scheme of the present invention, using super critical fluid technology prepares the method for C/C matrix material fast, tiny SiC or C particulate etc. is dissolved in the supercutical fluid, make its infiltration in the C/C precast body by adjusting temperature or pressure, again in conjunction with chemical liquids-gas-phase deposition, carry out fast deposition, whole process is only carried out once; The detailed process step is as follows:
1) with micron or nano level SiC or C particles dispersed in polysiloxane solution;
2) mixing solutions is packed in the pressurized vessel, feed propane gas and sealed vessel;
3) speed with 3 ℃/min, 100kPa heats up respectively, pressurizes, and temperature to 120 ℃, pressure can observe propane and reach the supercutical fluid state during to 6500kPa;
4) under the supercutical fluid state, keep 5hour, again with the cooling of the speed of 3 ℃/min, or with the speed step-down of 60kPa, or decrease temperature and pressure simultaneously, make the infiltration of SiC or C particulate in the prefabricated intravital space of C/C;
5) with in low hydrocarbon solution (kerosene, hexanaphthene etc.) the homemade rapid chemical liquid-vapour deposition container of packing into of liquid state, again micron or nano level SiC or C powder are scattered in the low hydrocarbon solution, after machinery or ultrasonic stirring, the C/C precast body of packing into and infiltrating, vacuumize after the sealing, vacuum tightness is-200kPa;
6) adjust the load coil frequency, temperature rises to 1200 ℃ rapidly in the 6min, makes the precast body surfaces externally and internally form big thermograde;
7) at state 6) keep 1hour down, make the SiC or the C particulate cracking deposition of infiltration;
8) reduce the heating element temperature to room temperature, take out the C/C material;
9) with the C/C material under 2400 ℃ of conditions, insulation 1hour heat-treats, and makes its greying, final obtains fine and close C/C matrix material.
Embodiment 4: according to technical scheme of the present invention, using super critical fluid technology prepares the method for C/C matrix material fast, tiny SiC or C particulate etc. is dissolved in the supercutical fluid, make its infiltration in the C/C precast body by adjusting temperature or pressure, again in conjunction with chemical liquids-gas-phase deposition, carry out fast deposition, whole process is only carried out once; The detailed process step is as follows:
1) with micron or nano level SiC or C particles dispersed in polysiloxane solution;
2) mixing solutions is packed in the pressurized vessel, feed propane gas and sealed vessel;
3) speed with 4 ℃/min, 120kPa heats up respectively, pressurizes, and temperature to 100 ℃, pressure can observe propane and reach the supercutical fluid state during to 5000kPa;
4) under the supercutical fluid state, keep 4hour, again with the cooling of the speed of 3 ℃/min, or with the speed step-down of 80kPa, or decrease temperature and pressure simultaneously, make the infiltration of SiC or C particulate in the prefabricated intravital space of C/C;
5) with in low hydrocarbon solution (kerosene, hexanaphthene etc.) the homemade rapid chemical liquid-vapour deposition container of packing into of liquid state, again micron or nano level SiC or C powder are scattered in the low hydrocarbon solution, after machinery or ultrasonic stirring, the C/C precast body of packing into and infiltrating, vacuumize after the sealing, vacuum tightness is-200kPa;
6) adjust the load coil frequency, temperature rises to 1050 ℃ rapidly in the 5min, makes the precast body surfaces externally and internally form big thermograde;
7) at state 6) keep 1hour down, make the SiC or the C particulate cracking deposition of infiltration;
8) reduce the heating element temperature to room temperature, take out the C/C material;
9) with the C/C material under 2500 ℃ of conditions, insulation 1hour heat-treats, and makes its greying, final obtains fine and close C/C matrix material.
Concrete application example:
The PAN 1k plain weave carbon cloth of producing with Jilin Carbon Factory is woven into 2D C/C precast body, adopt method of the present invention and step, nano level SiC powder is scattered in the polysiloxane solution, carry out supercutical fluid infiltration and rapid chemical liquid-vapour deposition, the final 2D C/C density of material that obtains is 1.80g/cm
3, the material open porosity is 5%, arrives by SEM, tem observation, has nano level SiC tissue between fiber and matrix carbon interface.
Claims (5)
1. a using super critical fluid technology prepares the method for C/C matrix material fast, it is characterized in that, tiny SiC or C particulate etc. is dissolved in the supercutical fluid, make its infiltration in the C/C precast body by adjusting temperature or pressure, again in conjunction with chemical liquids-gas-phase deposition, carry out fast deposition, whole process is only carried out once; The detailed process step is as follows:
1) with micron or nano level SiC or C particles dispersed in polysiloxane solution;
2) mixing solutions is packed in the pressurized vessel, feed propane gas and sealed vessel;
3) speed with 1 ℃/min~5 ℃/min, 50kPa~200kPa heats up respectively, pressurizes, and temperature to 90 ℃~150 ℃, pressure can observe propane and reach the supercutical fluid state during to 4000kPa~9000kPa.
4) under the supercutical fluid state, keep 0.5hour~10hour, again with the speed cooling of 1 ℃/min~5 ℃/min, or with the speed step-down of 20kPa~100kPa, or decrease temperature and pressure simultaneously, make the infiltration of SiC or C particulate in the prefabricated intravital space of C/C;
5) with in low hydrocarbon solution (kerosene, hexanaphthene etc.) the homemade rapid chemical liquid-vapour deposition container of packing into of liquid state, again micron or nano level SiC or C powder are scattered in the low hydrocarbon solution, after machinery or ultrasonic stirring, the C/C precast body of packing into and infiltrating, vacuumize after the sealing, vacuum tightness is-200kPa;
6) adjust the load coil frequency, temperature rises to 900 ℃~1500 ℃ rapidly in 3min~8min, makes the precast body surfaces externally and internally form big thermograde;
7) at state 6) keep 0.5hour~2hour down, make the SiC or the C particulate cracking deposition of infiltration;
8) reduce the heating element temperature to room temperature, take out the C/C material;
9) with the C/C material under 2300 ℃ of-2600 ℃ of conditions, insulation 1hour heat-treats, and makes its greying, final obtains fine and close C/C matrix material.
2. using super critical fluid technology according to claim 1 prepares the method for C/C matrix material fast, it is characterized in that, tiny SiC, C particulate etc. is dissolved in the supercutical fluid, make its infiltration in the C/C precast body by adjusting temperature or pressure, again in conjunction with chemical liquids-gas-phase deposition, carry out fast deposition, whole process is only carried out once; The detailed process step is as follows:
1) with micron or nano level SiC or C particles dispersed in polysiloxane solution;
2) mixing solutions is packed in the pressurized vessel, feed propane gas and sealed vessel;
3) speed with 1 ℃/min, 50kPa heats up respectively, pressurizes, and temperature to 90 ℃, pressure can observe propane and reach the supercutical fluid state during to 9000kPa;
4) under the supercutical fluid state, keep 10hour, again with the cooling of the speed of 1 ℃/min, or with the speed step-down of 20kPa, or decrease temperature and pressure simultaneously, make the infiltration of SiC or C particulate in the prefabricated intravital space of C/C;
5) with in low hydrocarbon solution (kerosene, hexanaphthene etc.) the homemade rapid chemical liquid-vapour deposition container of packing into of liquid state, again micron or nano level SiC or C powder are scattered in the low hydrocarbon solution, after machinery or ultrasonic stirring, the C/C precast body of packing into and infiltrating, vacuumize after the sealing, vacuum tightness is-200kPa;
6) adjust the load coil frequency, temperature rises to 900 ℃ rapidly in the 3min, makes the precast body surfaces externally and internally form big thermograde;
7) at state 6) keep 2hour down, make the SiC or the C particulate cracking deposition of infiltration;
8) reduce the heating element temperature to room temperature, take out the C/C material;
9) with the C/C material under 2600 ℃ of conditions, insulation 1hour heat-treats, and makes its greying, final obtains fine and close C/C matrix material.
3. the method for preparing the C/C matrix material according to the described using super critical fluid technology of claim fast, it is characterized in that, tiny SiC or C particulate etc. is dissolved in the supercutical fluid, make its infiltration in the C/C precast body by adjusting temperature or pressure, again in conjunction with chemical liquids-gas-phase deposition, carry out fast deposition, whole process is only carried out once; The detailed process step is as follows:
1) with micron or nano level SiC or C particles dispersed in polysiloxane solution;
2) mixing solutions is packed in the pressurized vessel, feed propane gas and sealed vessel;
3) speed with 5 ℃/min, 200kPa heats up respectively, pressurizes, and temperature to 150 ℃, pressure can observe propane and reach the supercutical fluid state during to 4000kPa;
4) under the supercutical fluid state, keep 0.5hour, again with the cooling of the speed of 5 ℃/min, or with the speed step-down of 100kPa, or decrease temperature and pressure simultaneously, make the infiltration of SiC or C particulate in the prefabricated intravital space of C/C;
5) with in low hydrocarbon solution (kerosene, hexanaphthene etc.) the homemade rapid chemical liquid-vapour deposition container of packing into of liquid state, again micron or nano level SiC or C powder are scattered in the low hydrocarbon solution, after machinery or ultrasonic stirring, the C/C precast body of packing into and infiltrating, vacuumize after the sealing, vacuum tightness is-200kPa;
6) adjust the load coil frequency, temperature rises to 1500 ℃ rapidly in the 8min, makes the precast body surfaces externally and internally form big thermograde;
7) at state 6) keep 0.5hour down, make the SiC or the C particulate cracking deposition of infiltration;
8) reduce the heating element temperature to room temperature, take out the C/C material;
9) with the C/C material under 2300 ℃ of conditions, insulation 1hour heat-treats, and makes its greying, final obtains fine and close C/C matrix material.
4. using super critical fluid technology according to claim 1 prepares the method for C/C matrix material fast, it is characterized in that, tiny SiC or C particulate etc. is dissolved in the supercutical fluid, make its infiltration in the C/C precast body by adjusting temperature or pressure, again in conjunction with chemical liquids-gas-phase deposition, carry out fast deposition, whole process is only carried out once; The detailed process step is as follows:
1) with micron or nano level SiC or C particles dispersed in polysiloxane solution;
2) mixing solutions is packed in the pressurized vessel, feed propane gas and sealed vessel;
3) speed with 3 ℃/min, 100kPa heats up respectively, pressurizes, and temperature to 120 ℃, pressure can observe propane and reach the supercutical fluid state during to 6500kPa;
4) under the supercutical fluid state, keep 5hour, again with the cooling of the speed of 3 ℃/min, or with the speed step-down of 60kPa, or decrease temperature and pressure simultaneously, make the infiltration of SiC or C particulate in the prefabricated intravital space of C/C;
5) with in low hydrocarbon solution (kerosene, hexanaphthene etc.) the homemade rapid chemical liquid-vapour deposition container of packing into of liquid state, again micron or nano level SiC or C powder are scattered in the low hydrocarbon solution, after machinery or ultrasonic stirring, the C/C precast body of packing into and infiltrating, vacuumize after the sealing, vacuum tightness is-200kPa;
6) adjust the load coil frequency, temperature rises to 1200 ℃ rapidly in the 6min, makes the precast body surfaces externally and internally form big thermograde;
7) at state 6) keep 1hour down, make the SiC or the C particulate cracking deposition of infiltration;
8) reduce the heating element temperature to room temperature, take out the C/C material;
9) with the C/C material under 2400 ℃ of conditions, insulation 1hour heat-treats, and makes its greying, final obtains fine and close C/C matrix material.
5. using super critical fluid technology according to claim 1 prepares the method for C/C matrix material fast, it is characterized in that, tiny SiC or C particulate etc. is dissolved in the supercutical fluid, make its infiltration in the C/C precast body by adjusting temperature or pressure, again in conjunction with chemical liquids-gas-phase deposition, carry out fast deposition, whole process is only carried out once; The detailed process step is as follows:
1) with micron or nano level SiC or C particles dispersed in polysiloxane solution;
2) mixing solutions is packed in the pressurized vessel, feed propane gas and sealed vessel;
3) speed with 4 ℃/min, 120kPa heats up respectively, pressurizes, and temperature to 100 ℃, pressure can observe propane and reach the supercutical fluid state during to 5000kPa;
4) under the supercutical fluid state, keep 4hour, again with the cooling of the speed of 3 ℃/min, or with the speed step-down of 80kPa, or decrease temperature and pressure simultaneously, make the infiltration of SiC or C particulate in the prefabricated intravital space of C/C;
5) with in low hydrocarbon solution (kerosene, hexanaphthene etc.) the homemade rapid chemical liquid-vapour deposition container of packing into of liquid state, again micron or nano level SiC or C powder are scattered in the low hydrocarbon solution, after machinery or ultrasonic stirring, the C/C precast body of packing into and infiltrating, vacuumize after the sealing, vacuum tightness is-200kPa;
6) adjust the load coil frequency, temperature rises to 1050 ℃ rapidly in the 5min, makes the precast body surfaces externally and internally form big thermograde;
7) at state 6) keep 1hour down, make the SiC or the C particulate cracking deposition of infiltration;
8) reduce the heating element temperature to room temperature, take out the C/C material;
9) with the C/C material under 2500 ℃ of conditions, insulation 1hour heat-treats, and makes its greying, final obtains fine and close C/C matrix material.
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Cited By (9)
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WO2007003813A2 (en) | 2005-05-13 | 2007-01-11 | Snecma Propulsion Solide | Method for the rapid densification of a porous substrate, comprising the formation of a solid deposit within the porosity of the substrate |
CN1328215C (en) * | 2005-07-18 | 2007-07-25 | 西安交通大学 | Method for preparing carbon/carbon composite material |
CN100370055C (en) * | 2005-11-07 | 2008-02-20 | 西安交通大学 | Method for quick-speed preparing carbon/carbon composite material using heat gradient chemical gas phase infiltration |
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WO2007003813A2 (en) | 2005-05-13 | 2007-01-11 | Snecma Propulsion Solide | Method for the rapid densification of a porous substrate, comprising the formation of a solid deposit within the porosity of the substrate |
CN1328215C (en) * | 2005-07-18 | 2007-07-25 | 西安交通大学 | Method for preparing carbon/carbon composite material |
CN100370055C (en) * | 2005-11-07 | 2008-02-20 | 西安交通大学 | Method for quick-speed preparing carbon/carbon composite material using heat gradient chemical gas phase infiltration |
CN109142408A (en) * | 2018-08-06 | 2019-01-04 | 华东师范大学 | A kind of method of the TEM sample of dry process two-dimensional material |
CN109142408B (en) * | 2018-08-06 | 2021-02-26 | 华东师范大学 | Method for preparing TEM sample of two-dimensional material by dry method |
CN109175355A (en) * | 2018-08-17 | 2019-01-11 | 宁波瑞丰汽车零部件有限公司 | A kind of iron-based connection pressing plate |
CN109175355B (en) * | 2018-08-17 | 2020-10-27 | 宁波瑞丰汽车零部件有限公司 | Iron-based connecting pressing plate |
CN111687406A (en) * | 2020-04-14 | 2020-09-22 | 西安融烯科技新材料有限公司 | Preparation method and application of high-toughness aluminum alloy composite material |
CN111690848A (en) * | 2020-04-14 | 2020-09-22 | 西安融烯科技新材料有限公司 | Preparation method and application of low-thermal-expansion-rate aluminum alloy composite material |
CN111446154A (en) * | 2020-05-06 | 2020-07-24 | 西安交通大学 | 4H-SiC/SiO2 interface low-temperature improvement method based on supercritical CO2 treatment and application thereof |
CN111446154B (en) * | 2020-05-06 | 2023-05-16 | 西安交通大学 | Supercritical CO2 treatment-based 4H-SiC/SiO2 interface low-temperature improvement method and application thereof |
CN111575515A (en) * | 2020-06-09 | 2020-08-25 | 西安融烯科技新材料有限公司 | Preparation method and application of nano carbon-aluminum alloy composite material |
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