CN103044056B - Technology and equipment for preparing C/C composite - Google Patents
Technology and equipment for preparing C/C composite Download PDFInfo
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- CN103044056B CN103044056B CN201310008097.6A CN201310008097A CN103044056B CN 103044056 B CN103044056 B CN 103044056B CN 201310008097 A CN201310008097 A CN 201310008097A CN 103044056 B CN103044056 B CN 103044056B
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Abstract
The invention discloses a technology and equipment for preparing a C/C (carbon/carbon) composite. The technology for rapidly preparing the C/C composite comprises the following steps that (1) a preform is pretreated; (2) tools are prepared; (3) furnace loading is conducted; (4) temperature gradient differential CVI (chemical vapor infiltration) treatment is conducted; (5) heating of a heating element and input of mixed gas are stopped sequentially after 100-300h; and (6) a cover plate, the outer tool, the preform and the inner tool are taken out to form the C/C composite with density of 1.4-1.7g/cm<3>. The invention further discloses the equipment for preparing the C/C composite. According to the technology and the equipment, the operation is simple; the densification period is short; the industrial difficulty is small; the densification rate is high; ineffective reaction can be avoided; the carbon yield can be increased; and pollution of a vacuum system can be prevented.
Description
Technical field
The present invention relates to one utilizes thermograde pressure reduction chemical vapor infiltration (CVI) to prepare fast technique and the equipment thereof of charcoal/charcoal (C/C) composite part.
Background technology
The main technique of existing preparation C/C matrix material is isothermal CVI technique, this technique is simple, easy to operate, can carry out densification to multiple precast bodies with different size and shape simultaneously, and there are potentiality aspect preparation density and the even controlled C/C matrix material of weave construction.But, in employing isothermal CVI technique preparation process, RESEARCH OF PYROCARBON meeting preferential deposition is to the surface of precast body, precast body surface pore is sealed too early, affect its inner density, conventionally need to adopt low temperature, low gas concentration reduce speed of response and repeatedly mechanical workout remove surface crust and open hole, thereby the preparation cycle of preparation high-density C/C matrix material reach one month some months even, manufacture efficiency is low, and cost is high.
At present, the technique of preparation C/C matrix material also has a kind of thermograde CVI technique, and this thermograde CVI technique is the improvement to traditional isothermal CVI technique.In this processing unit, temperature distribution gradient in precast body, presoma deposits from arrival high-temperature zone, cold zone by diffusion mass transfer, and pyrolytic deposition district is by inner side iterative method laterally, compared with traditional isothermal CVI technique, greatly improve the homogeneity of density of material.But material enters in precast body and still mainly relies on its diffusion from presoma, and gas transmission is slow, and material densification rate is low.
The disclosed thermograde chemical vapor infiltration of the disclosed Zone-limited temp .-changing prossure differental chemical gas-phase permeation process of Chinese patent 00113718.2 and Chinese patent 200510096306.2 is prepared the method for C/C matrix material fast, all relate to thermograde pressure reduction chemical vapor infiltration technique, but they are high to equipment requirements, industrialization difficulty is large.Chinese patent 200310115118.0 discloses a kind of outer thermograde chemical vapor infiltration method of carbon/carbon brake disc negative pressure oriented flow, is not suitable for the preparation of pipe but the method is only applicable to the preparation of carbon/carbon brake disc, and the scope of application is little.
Summary of the invention
Technical problem to be solved by this invention is, overcomes the above-mentioned defect that prior art exists, and provides a kind of densification rate high, preparation technology and the equipment thereof of charcoal/charcoal (C/C) matrix material of low cost of manufacture.
The technical solution adopted for the present invention to solve the technical problems is:
The preparation technology of charcoal/charcoal (C/C) matrix material of the present invention, comprises the following steps:
(1) precast body pre-treatment: be 0.45～0.8 g/cm by density
3carbon/carbon composite precast body be placed in High Temperature Furnaces Heating Apparatus, under 1000～2000 DEG C (preferably 1600～1900 DEG C, more preferably 1800 DEG C), carry out High Temperature Pre process 1.0～5.0 hours (preferably 1.5～2.5 hours, more preferably 2.0 hours);
(2) frock is prepared: according to precast body size processing built-in heating body, outer frock, interior frock, cover plate, loading plate and material pier with aspirating hole, install interior thermopair and outer thermopair, outer frock, interior frock and cover plate adopt C/C matrix material or graphite;
(3) shove charge: ready step (2) built-in heating body, interior frock, the pretreated precast body of step (1) and the ready outer frock of step (2) are put on the loading plate of chemical vapor deposition stove by the support of material pier in order successively, and precast body and outer frock spacing are the preferred 15-25mm of 5～40mm(; More preferably 20 mm), precast body and interior frock spacing are 5～40mm(15-25mm; More preferably 20 mm), in stove, air pipe outlet is placed in the region of outer frock and precast body formation, then ready step (2) cover plate that is provided with aspirating hole is placed on to outer frock top, the ready interior thermopair of step (2) and outer thermopair are placed in respectively outer frock inner side and outside;
(4) thermograde pressure reduction CVI processes: survey after Pressure Rise Rate qualified (200Pa/h), open vacuum system, with the preferred 100-200 of 50～300 DEG C/hr(DEG C/hr; More preferably 150 DEG C/hr) heat-up rate heating heating element, make its heat up 5～10 hours (preferably 7-9 hour, more preferably 8 hours), rise to 850 DEG C～1200 DEG C (preferably 1000-1100 DEG C when interior thermopair records temperature inside precast body; More preferably 1050 DEG C), when recording precast body temperature outside, outer thermopair rises to 800 DEG C～950 DEG C (preferably 900 DEG C), the thermograde in precast body inner side and outside is preferably 5～12 DEG C/mm of 3～15 DEG C/mm(); In the region that tracheae by being placed in outer frock and loading plate contact position forms to precast body and outer frock, send into the mixed gas of hydrocarbon gas and diluent gas, and ensure that mixed gas flow is the preferred 60L/Min of 50～70L/Min(), when precast body outside and inside pressure poor be preferably 2～3 KPa of 1～5KPa() time, precast body and outer frock form the guiding of the gas aspirating hole outside cover plate in region discharges from furnace shell bleeding point, and the aspirating hole guiding inside cover plate of the gas in the region that precast body and inside and outside frock form is discharged from furnace shell bleeding point;
(5) after 100～300 hours (preferably 250～280 hours), stop successively heating heating element, stop inputting mixed gas;
(6) take out cover plate, outer frock, precast body and interior frock are cut and taken out along contact surface, obtain density 1.4～1.7g/cm
3c/C matrix material.
Further, described hydrocarbon gas is Sweet natural gas, propylene or propane, and described diluent gas is nitrogen.
Further, described precast body shape preferably drum shape.
The equipment that the present invention's preparation C/C matrix material uses, comprise furnace shell, heating element, precast body, described furnace shell top is provided with bleeding point, described furnace shell inwall is provided with thermal insulation layer, the inside and outside both sides of described precast body are respectively equipped with interior thermopair and the outer thermopair of measuring the inside and outside both sides of precast body temperature, in precast body thickness direction formation temperature gradient, also comprise interior frock, outer frock and the cover plate that is provided with aspirating hole, described interior frock is placed in precast body inner side, described interior frock is placed in heating element outside, described outer frock is placed in precast body outside, aspirating hole on described cover plate is located at the top in interior frock outside and formation region, precast body inner side, described cover plate is placed in described outer frock, precast body and interior frock top, described heating element, outer frock, precast body and interior frock are all placed on the loading plate being supported by material pier, described outer frock and loading plate contact position are equipped with tracheae, the regional connectivity that described tracheae one end and precast body outside and outer frock inner side form, the other end is through thermal insulation layer and furnace shell wall.
Further, on described cover plate, in the corresponding region, space that outer frock and precast body form, be provided with 5～15 (preferably 10) aspirating holes.
Further, described precast body is 2.5D charcoal fiber preform or 3D charcoal fiber preform.
Further, described heating element, outer frock, interior frock and cover plate all adopt C/C matrix material or graphite to make.
Further, on described cover plate, in the corresponding region, space that outer frock and precast body form, the diameter of aspirating hole is the preferred 30mm of 28～32mm(), in the corresponding region, space that interior frock outside and precast body form, the diameter of aspirating hole is the preferred 18mm of 16～20mm().
The technique of the present invention's preparation C/C matrix material, simple to operate, the densification cycle is short, not high to equipment requirements, industrialization difficulty is little, be particularly useful for making round shape C/C matrix material, in the aspirating hole guiding device on cover plate, gas is discharged from furnace shell bleeding point, and hydrocarbon gas molecular energy is " purging " precast body surface effectively, improve densification rate, can avoid the generation of abortive response, improve charcoal recovery rate, prevent the pollution of vacuum system simultaneously; The equipment of the present invention's preparation C/C matrix material, simple in structure, low cost of manufacture.
Brief description of the drawings
Fig. 1 is the structural representation that the present invention prepares C/C matrix material apparatus embodiments;
Fig. 2 is the structure enlarged diagram of cover plate embodiment illustrated in fig. 1;
Fig. 3 is existing covering plate structure schematic diagram;
Fig. 4 is the diagrammatic cross-section of outer frock embodiment illustrated in fig. 1;
Fig. 5 is the diagrammatic cross-section of interior frock embodiment illustrated in fig. 1.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
Embodiment 1: apparatus embodiments
With reference to accompanying drawing, the present invention prepares the apparatus embodiments of C/C matrix material, comprise furnace shell, heating element 6, precast body 3, described furnace shell top is provided with bleeding point 8, described furnace shell inwall is provided with thermal insulation layer 7, the inside and outside both sides of described precast body 3 are respectively equipped with interior thermopair 13 and the outer thermopair 12 of measuring precast body 3 inside and outside both sides temperature, the thermograde forming for detection of precast body 3 thickness directions, also comprise interior frock 5, outer frock 4 and cover plate 9, described interior frock 5 is placed in precast body 3 inner sides, described interior frock 5 is placed in heating element 6 outsides, described outer frock 4 is placed in precast body 3 outsides, aspirating hole 10 on described cover plate 9 is located at the top in interior frock outside and formation region, precast body inner side, described outer frock 4, cover plate 9 is stamped in precast body 3 and interior frock 5 tops, described heating element 6, outer frock 4, precast body 3 and interior frock 5 are all placed on the loading plate 2 being supported by material pier 1, described outer frock 4 is equipped with tracheae 11 with loading plate 2 contact positions, the regional connectivity that described tracheae 11 one end and precast body 3 outsides and outer frock 4 inner sides form, the other end is through thermal insulation layer 7 and furnace shell wall.
On described cover plate 9, in the corresponding region, space that outer frock 4 and precast body 3 form, be provided with 10 aspirating holes.
Described precast body 3 is 2.5D charcoal fiber preform.
Described outer frock 4, interior frock 5, heating element 6 and cover plate 9 all adopt graphite to make.
Embodiment 2: preparation technology embodiment 1.
The present invention prepares round shape C/C composite technology embodiment and comprises the following steps:
(1) precast body 3 pre-treatment: be 0.5 g/cm by density
3, the round shape 2.5D charcoal fiber preform 3 that is of a size of Φ 660mm × Φ 600mm × 300mm is placed in High Temperature Furnaces Heating Apparatus, at 1800 DEG C, carry out High Temperature Pre and process 2 hours;
(2) frock is prepared: according to precast body 3 shapes, size processing heating element 6,4,7 precast bodies 3 of outer frock, in the corresponding region, space that interior frock 5 and precast body 3 form, have 20 diameters and be in the corresponding region, space that 30mm and outer frock 4 and precast body 3 form and have cover plate 9, loading plate 2 and the material pier 1 that 10 diameters are 18mm aspirating hole 10, install interior thermopair 13 and outer thermopair 12, outer frock 4, interior frock 5 and cover plate 9 are made up of graphite;
(3) shove charge: by ready step (2) built-in heating body 6, interior frock 5, the ready outer frock 4 of the pretreated precast body 3 of step (1) and step (2) is put into chemical vapor deposition stove in order successively by the loading plate 2 that supports of material pier 1, precast body 3 is 15mm with outer frock 4 spacing, precast body 3 is 15mm with interior frock 5 spacing, tracheae 11 air outlets are placed in the ring groove that outer frock 4 and precast body 3 form in stove, then ready step (2) band aspirating hole 10 cover plates 9 are placed on to outer frock 4 tops, the ready interior thermopair 13 of step (2) and outer thermopair 12 are located at respectively outer frock 4 inner sides and outside,
(4) thermograde pressure reduction CVI processes: survey after Pressure Rise Rate qualified (200Pa/h), open vacuum system, with the heat-up rate heating heating element 6 of 150 DEG C/hr, it is heated up 8 hours, when recording precast body 3 inner side temperature, interior thermopair 13 rises to 1050 DEG C, when recording precast body 3 temperature outside, outer thermopair 12 rises to 900 DEG C, the thermograde in precast body 3 inner sides and outside is 5 DEG C/mm, in the region that tracheae by being placed in outer frock and loading plate contact position forms to precast body and outer frock, send into the mixed gas of hydrocarbon gas and diluent gas, and ensure that mixed gas flow is 60L/Min, when precast body outside with inside pressure is poor while being 2KPa, start deposition, gas in the ring groove that precast body 3 and outer frock 4 form is discharged from furnace shell bleeding point 8 through cover plate 9 outside aspirating hole guiding, gas in the ring groove that precast body 3 and interior frock 5 form is discharged from furnace shell bleeding point 8 through cover plate 9 inner side aspirating hole guiding,
(5), after 250 hours, stop successively heating heating element, stop inputting mixed gas;
(6) take out cover plate, outer frock 4, precast body 3 and interior frock 5, obtain 7 round shape density 1.5g/cm
3c/C matrix material.
Embodiment 2: preparation technology embodiment 2.
(1) precast body 3 pre-treatment: be 0.4 g/cm by density
3, the round shape 2.5D charcoal fiber preform 3 that is of a size of Φ 660mm × Φ 600mm × 300mm is placed in High Temperature Furnaces Heating Apparatus, at 1600 DEG C, carry out High Temperature Pre and process 4 hours;
(2) frock is prepared: according to precast body 3 shapes, size processing heating element 6,4,7 precast bodies 3 of outer frock, in the corresponding region, space that interior frock 5 and precast body 3 form, have 20 diameters and be in the corresponding region, space that 30mm and outer frock 4 and precast body 3 form and have cover plate 9, loading plate 2 and the material pier 1 that 10 diameters are 18mm aspirating hole 10, install interior thermopair 13 and outer thermopair 12, outer frock 4, interior frock 5 and cover plate 9 are made up of graphite;
(3) shove charge: by ready step (2) built-in heating body 6, interior frock 5, the ready outer frock 4 of the pretreated precast body 3 of step (1) and step (2) is put into chemical vapor deposition stove in order successively by the loading plate 2 that supports of material pier 1, precast body 3 is 20mm with outer frock 4 spacing, precast body 3 is 20mm with interior frock 5 spacing, tracheae 11 air outlets are placed in the ring groove that outer frock 4 and precast body 3 form in stove, then ready step (2) band aspirating hole 10 cover plates 9 are placed on to outer frock 4 tops, the ready interior thermopair 13 of step (2) and outer thermopair 12 are located at respectively outer frock 4 inner sides and outside.
(4) thermograde pressure reduction CVI processes: survey after Pressure Rise Rate qualified (200Pa/h), open vacuum system, with the heat-up rate heating heating element 6 of 250 DEG C/hr, it is heated up 8 hours, when recording precast body 3 inner side temperature, interior thermopair 13 rises to 1020 DEG C, when recording precast body 3 temperature outside, outer thermopair 12 rises to 870 DEG C, the thermograde in precast body 3 inner sides and outside is 4 DEG C/mm, in the region that tracheae by being placed in outer frock and loading plate contact position forms to precast body and outer frock, send into the mixed gas of hydrocarbon gas and diluent gas, and ensure that mixed gas flow is 68L/Min, when precast body outside with inside pressure is poor while being 3KPa, start deposition, gas in the ring groove that precast body 3 and outer frock 4 form is discharged from furnace shell bleeding point 8 through cover plate 9 outside aspirating hole guiding, gas in the ring groove that precast body 3 and interior frock 5 form is discharged from furnace shell bleeding point 8 through cover plate 9 inner side aspirating hole guiding,
(5), after 280 hours, stop successively heating heating element, stop inputting mixed gas;
(6) take out cover plate 9, outer frock 4, precast body 3 and interior frock 5, obtain 7 round shape density 1.6g/cm
3c/C matrix material.
Claims (9)
1. a technique of preparing C/C matrix material, is characterized in that, comprises the following steps:
(1) precast body pre-treatment: be 0.45～0.8 g/cm by density
3precast body at 1000～2000 DEG C, carry out High Temperature Pre process 1～5 hour;
(2) frock is prepared: according to precast body size processing built-in heating body, outer frock, interior frock, cover plate, loading plate and material pier with aspirating hole, install interior thermopair and outer thermopair, outer frock, interior frock and cover plate adopt C/C matrix material or graphite;
(3) shove charge: by ready step (2) built-in heating body, interior frock, the pretreated precast body of step (1) and the ready outer frock of step (2) are put on the loading plate of equipment by the support of material pier in order successively, precast body and outer frock spacing are 5～40mm, precast body and interior frock spacing are 5～40mm, in stove, air pipe outlet is placed in the region of outer frock and precast body formation, then the ready band aspirating hole of step (2) cover plate is placed on to outer frock top, the ready interior thermopair of step (2) and outer thermopair are located at respectively precast body inner side and outside,
(4) thermograde pressure reduction CVI processes: after survey Pressure Rise Rate is qualified, open vacuum system, with the heat-up rate heating heating element of 50～300 DEG C/hr, it is heated up 5～10 hours, when recording temperature inside precast body, interior thermopair rises to 980～1080 DEG C, outer thermopair records precast body temperature outside and rises to 800～950 DEG C, and the thermograde in precast body inner side and outside is 3～15 DEG C/mm; In the region that tracheae by being placed in outer frock and loading plate contact position forms to precast body and outer frock, send into the mixed gas of hydrocarbon gas and diluent gas, and ensure that mixed gas flow is 50-70L/min, precast body outside and inside pressure is poor while being 1～5KPa, starts to deposit; Precast body and outer frock form the guiding of the gas aspirating hole outside cover plate in region discharges from furnace shell bleeding point, and the aspirating hole guiding inside cover plate of the gas in the region that precast body and interior frock form is discharged from furnace shell bleeding point; Described hydrocarbon gas is Sweet natural gas, propylene or propane, and described diluent gas is nitrogen;
(5), after 100～300 hours, stop successively heating heating element, stop inputting mixed gas;
(6) take out cover plate, outer frock, precast body and interior frock, obtain density 1.4～1.7g/cm
3c/C matrix material.
2. the technique of preparation C/C matrix material according to claim 1, is characterized in that, in described step (1), the temperature of precast body pyroprocessing is 1600～1900 DEG C, and the pretreated time is 1.5～2.5 hours.
3. the technique of preparation C/C matrix material according to claim 1, is characterized in that, in described step (3), described outer frock and precast body spacing are 15-25mm, and interior frock and precast body spacing are 15-25mm.
4. the technique of preparation C/C matrix material according to claim 1, it is characterized in that, described step (4), after survey Pressure Rise Rate is qualified, open vacuum system, with the heat-up rate heating heating element of 100-200 DEG C/hr, make its intensification 7-9 hour, rise to 1000-1100 DEG C when interior thermopair records temperature inside precast body, rise to 900 DEG C when outer thermopair records precast body temperature outside, the thermograde in precast body inner side and outside is 5～12 DEG C/mm; In the region that tracheae by being placed in outer frock and loading plate contact position forms to precast body and outer frock, send into the mixed gas of hydrocarbon gas and diluent gas, and ensure that mixed gas flow is 60L/Min, when precast body outside with inside pressure is poor while being 2～3 KPa, precast body and outer frock form the guiding of the gas aspirating hole outside cover plate in region discharges from furnace shell bleeding point, and the aspirating hole guiding inside cover plate of the gas in the region that precast body and inside and outside frock form is discharged from furnace shell bleeding point.
5. prepare the equipment of C/C matrix material for one kind, comprise furnace shell, heating element, precast body, described furnace shell top is provided with bleeding point, described furnace shell inwall is provided with thermal insulation layer, it is characterized in that, the inside and outside both sides of described precast body are respectively equipped with interior thermopair and the outer thermopair of measuring the inside and outside both sides of precast body temperature, in precast body thickness direction formation temperature gradient, also comprise interior frock, outer frock and cover plate, described interior frock is placed in precast body inner side, described interior frock is placed in heating element outside, described outer frock is placed in precast body outside, aspirating hole on described cover plate is located at the top in interior frock outside and formation region, precast body inner side, described outer frock, cover plate is stamped in precast body and interior frock top, described heating element, outer frock, precast body and interior frock are all placed on the loading plate being supported by material pier, described outer frock and loading plate contact position are equipped with tracheae, the regional connectivity that described tracheae one end and precast body outside and outer frock inner side form, the other end is communicated with the mixed gas of hydrocarbon gas and diluent gas through thermal insulation layer and furnace shell wall, described hydrocarbon gas is Sweet natural gas, propylene or propane, and described diluent gas is nitrogen.
6. the equipment of preparation C/C matrix material according to claim 5, is characterized in that, on described cover plate, in the corresponding region, space that outer frock and precast body form, is provided with 5～15 aspirating holes.
7. the equipment of preparation C/C matrix material according to claim 6, is characterized in that 10 of the numbers of described aspirating hole.
8. the equipment of preparation C/C matrix material according to claim 5, it is characterized in that, described precast body is 2.5D charcoal fiber preform or 3D charcoal fiber preform, and described heating element, outer frock, interior frock and cover plate all adopt C/C matrix material or graphite to make.
9. according to the equipment of the preparation C/C matrix material described in claim 5 or 6, it is characterized in that, on described cover plate, in the corresponding region, space that outer frock and precast body form, the diameter of aspirating hole is 28～32mm, and in the corresponding region, space that interior frock outside and precast body form, the diameter of aspirating hole is 16～20mm.
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Families Citing this family (9)
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| CN103934043A (en) * | 2014-04-16 | 2014-07-23 | 烟台沃克斯炉窑开发有限公司 | Sintering technology of SCR (Selective Catalytic Reduction) honeycomb catalyst |
| CN103993292B (en) * | 2014-04-30 | 2017-01-04 | 洛阳八佳电气科技股份有限公司 | A kind of carbon carbon composite fast preparation method and device |
| CN107793172B (en) * | 2017-11-22 | 2020-05-15 | 山东国晶新材料有限公司 | Preparation method of long-fiber carbon ceramic fastener |
| CN108048817A (en) * | 2017-12-12 | 2018-05-18 | 湖南顶立科技有限公司 | A kind of chemical vapor deposition stove |
| CN108220913B (en) * | 2018-01-24 | 2020-01-14 | 航天睿特碳材料有限公司 | Rapid low-cost CVD (chemical vapor deposition) densification method for carbon/carbon composite material |
| CN109279908B (en) * | 2018-10-30 | 2021-06-01 | 中南大学 | Clamp for preparing ultrathin carbon/carbon composite material panel |
| CN111574237A (en) * | 2020-05-22 | 2020-08-25 | 中南大学 | Oversized carbon/carbon composite material sheet and equipment for preparing same |
| CN113173799B (en) * | 2021-04-28 | 2022-05-10 | 嵊州市西格玛科技有限公司 | Carbon/carbon composite material production system and method |
| CN113845370B (en) * | 2021-12-01 | 2022-02-22 | 中南大学 | Variable-density carbon/carbon composite material heat-insulating barrel and preparation method thereof |
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