CN101265935A - Ceramic base compound material bolt preparation method - Google Patents
Ceramic base compound material bolt preparation method Download PDFInfo
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- CN101265935A CN101265935A CNA2008100180390A CN200810018039A CN101265935A CN 101265935 A CN101265935 A CN 101265935A CN A2008100180390 A CNA2008100180390 A CN A2008100180390A CN 200810018039 A CN200810018039 A CN 200810018039A CN 101265935 A CN101265935 A CN 101265935A
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Abstract
The invention discloses a preparation method for a ceramic matrix composite bolt, which is characterized in that the method comprises the following steps: producing a fiber prefabricated product by shaping with a graphite plate after alternatively laminating a 1K carbon fiber 0/90 degree positive ply and a plus/minus Theta inclined ply; depositing a pyrolysis carbon interface layer on the prefabricated product and then depositing a silicon carbide matrix on the two-dimensional sheet with a deposited pyrolysis carbon interface layer to produce a semi-finished product of ceramic matrix composite sheet which is cut to form a bolt blank; grinding wheel and tapping the bolt blank; lastly obtaining the product of C/SiC composite bolt after many times of infiltration pyrolysis of polycarbosilane and continuing CVI depositing of SiC anti-oxidation coating. By the method, the bolt is processed and tapped on the semi-finished ceramic matrix composite prefabricated product which is not fully deposited and dense, so that the diamond grinding wheel wear is slow and the production cost is reduced. The technology of CVI combining with PIP process enables the elongation breaking strength of composite bolts to improve from 180 to 190MPa in prior art to 210 to 230MPa.
Description
Technical field
The present invention relates to a kind of preparation method of ceramic base compound material bolt.
Background technique
At known space industry, be used for the bolt and nut that aerospace craft thermal protection system structural member connects, because the aerospace craft flying condition is very abominable, during atmospheric reentry and air rub, nose cone, the leading edge of a wing and fuselage flap surface maximum temperature can reach 1650 ℃, and this just requires bolt and nut to possess excellent hot physical and chemical performance and mechanical property.
Space flight has graphite, C/C composite material and C/SiC composite material with the standard bolt nut material.Series of advantages such as that graphite has is high temperature resistant, low density and wear resistance are good, but high-temperature oxidation resistance is poor, intensity is low.Series of advantages such as that the C/C composite material has is high temperature resistant, low density, height ratio are strong, resistance to wear, anti-fatigue performance is good, but high-temperature oxidation resistance is poor, is promptly beginning oxidation more than 400 ℃.The C/SiC composite material has specific strength height, specific modulus and fracture toughness height, and density is low, and advantage such as good and designability of anti-ablative can adapt to the usage requirement of space technology to the superhigh temperature member well.
With reference to Fig. 1.Document " Whale; Eric.Ceramic fasteners for high temperature applications.MaterialsTechnology 2000; 15 (4): 276-281 " discloses the method that a kind of employing thermal gradient chemical vapor infiltration (hereinafter to be referred as CVI) technology prepares two-dimentional C/SiC compound material bolt, this method is carried out 0/90 ° with carbon fiber earlier and is just being spread and ± 45 ° of oblique shops, form 0/90 ° just spreading layer fiber 3 and ± 45 ° tiltedly shop layer fiber 4 alternative stacked prepare the prefabricated carbon fiber body, reusable heat gradient CVI technology deposits SiC on fiber preform, process the bolt outside thread with diamond-impregnated wheel then.Because this method processing bolt outside thread carries out after CVI process deposits SiC finishes, C/SiC composite hardness height, the diamond-impregnated wheel wearing and tearing are very fast, the C/SiC compound material bolt difficult quality guarantee that processes, and the wearing and tearing of diamond-impregnated wheel also cause processing cost to improve.Simultaneously, the interior solid degree was poor when CVI technology was made than large diameter bolt, and bolt strength is on the low side.According to document record, the room temperature tensile rupture strength of the 2D C/SiC compound material bolt of this method preparation is about 180～190MPa.
Summary of the invention
In order to overcome the deficiency that prior art is of poor quality, cost is high, the invention provides a kind of preparation method of ceramic base compound material bolt, utilization deposits the RESEARCH OF PYROCARBON interface layer on precast body, in conjunction with CVI deposition and polymer impregnated cracking (hereinafter to be referred as PIP) preparation C/SiC compound material bolt, can improve the tensile break strength of bolt, reduce preparation cost.
The technical solution adopted for the present invention to solve the technical problems: a kind of preparation method of ceramic base compound material bolt is characterized in that comprising the steps:
(a) with the 1K carbon fiber carry out 0/90 ° just spreading and ± the oblique shop of θ (0 °≤θ≤90 °), preparation carbon fiber two dimension sheet material precast body;
(b) deposition RESEARCH OF PYROCARBON interface layer on the prefabricated carbon fiber body, process conditions are: 800～900 ℃ of depositing temperatures, pressure 0.2～0.4kPa, propylene flow 25～35ml/min, Ar throughput 250～350ml/min, sedimentation time 40～60h;
(c) depositing depositing silicon carbide matrix on the two-dimentional sheet material of RESEARCH OF PYROCARBON interface layer, process conditions are: 800～1000 ℃ of depositing temperatures, pressure 2～4kPa, H
2Throughput 150～250ml/min, Ar throughput 250～350ml/min, 25～35 ℃ of trichloromethyl silane MTS temperature, H
2Be 8～12 with the molal weight ratio of MTS, sedimentation time 220～260h, form the semi-finished product ceramic matric composite;
(d) cutting forms ' T ' font bolt blank on the semi-finished product ceramic matric composite, utilizes diamond-impregnated wheel, and attaching nut is tapping on bolt blank, forms the semi-finished product bolt;
(e) with the semi-finished product bolt at 900～1100 ℃ of infiltration pyrolysis Polycarbosilanes repeatedly, heat-treat 2～4h for 1400～1600 ℃ then;
(f) continue deposition SiC inoxidzable coating with the CVI method again, depositing temperature is 800～1000 ℃, and gas is trichloromethyl silane, and sedimentation time 50～70h obtains finished product C/SiC compound material bolt.
The invention has the beneficial effects as follows: on precast body, deposit earlier RESEARCH OF PYROCARBON because this method adopts, prepare SiC in conjunction with CVI deposition and PIP, in not fully processing bolt and tapping on the semi-finished product ceramic matric composite precast body of deposition compact, slower to the diamond-impregnated wheel wearing and tearing, the quality of processing and the intensity of C/SiC compound material bolt have been guaranteed, reduced cost of production, the room temperature tensile rupture strength of C/SiC compound material bolt has been brought up to 210～230MPa by 180～190MPa of prior art.
Below in conjunction with drawings and Examples the present invention is elaborated.
Description of drawings
Fig. 1 is a carbon fiber shop layer schematic representation in the background technique.
Fig. 2 is the photo of the prepared ceramic base compound material bolt of preparation method of the present invention.
Fig. 3 is the longitudinal section micrograph of ceramic base compound material bolt worm tooth among Fig. 2.
Among the figure, the 1-bolt, the 2-worm tooth is just being spread a layer fiber for 3-0/90 °, tiltedly spreads layer fiber for 4-± θ °.
Embodiment
With reference to accompanying drawing.
Embodiment 1: just spreading first layer with the 1K carbon fiber according to 0 °, just spreading the second layer perpendicular to first layer in the above, tiltedly spread the 3rd layer in second layer one-tenth+45 in the above, tiltedly spread the 4th layer in the 3rd layer of one-tenth-45 in the above again, and, prepare carbon fiber two dimension sheet material precast body according to the size of required bolt according to this sequence alternate shop layer.It is parallel with the screw rod center line of bolt just to spread layer fiber 3, and tiltedly layer fiber 4 in shop is parallel with 2 of the worm tooths of bolt.
Deposition RESEARCH OF PYROCARBON interface layer on carbon fiber two dimension sheet material precast body, process conditions are: 800 ℃ of depositing temperatures, pressure 0.2kPa, propylene flow 35ml/min, Ar throughput 250ml/min, sedimentation time 60h.
Depositing depositing silicon carbide matrix on the carbon fiber two dimension sheet material of RESEARCH OF PYROCARBON interface layer, process conditions are: 800 ℃ of depositing temperatures, pressure 4kPa, H
2Throughput 150ml/min, Ar throughput 250ml/min, 35 ℃ of trichloromethyl silane temperature, H
2With the molal weight ratio of MTS be 12, sedimentation time 260h forms the semi-finished product ceramic matric composite.
Cutting forms ' T ' font bolt blank on the semi-finished product ceramic matric composite, utilizes diamond-impregnated wheel, and attaching nut is tapping on bolt blank, the semi-finished product bolt of formation.The angle θ of the worm tooth of making 2 is 2 * 45 °=90 °.
The semi-finished product bolt at 900 ℃ of four infiltration pyrolysis Polycarbosilanes, is heat-treated 2h for 1400 ℃ then.
After the cleaning of the pyrolysis product between the bolt thread tooth 2, continue deposition SiC inoxidzable coating with the CVI method again, depositing temperature is 800 ℃, and gas is trichloromethyl silane, and sedimentation time 70h obtains finished product C/SiC compound material bolt.
The C/SiC compound material bolt that present embodiment is prepared, through the room temperature tensile strength test, the worm tooth of bolt does not take off the tooth phenomenon, but screw rod generation rupture failure, the bolt tension rupture strength is 220MPa.
Embodiment 2: just spreading first layer with the 1K carbon fiber according to 0 °, just spreading the second layer perpendicular to first layer in the above, tiltedly spread the 3rd layer in second layer one-tenth+45 in the above, tiltedly spread the 4th layer in the 3rd layer of one-tenth-45 in the above again, and, prepare carbon fiber two dimension sheet material precast body according to the size of required bolt according to this sequence alternate shop layer.It is parallel with the screw rod center line of bolt just to spread layer fiber 3, and tiltedly layer fiber 4 in shop is parallel with 2 of the worm tooths of bolt.
Deposition RESEARCH OF PYROCARBON interface layer on carbon fiber two dimension sheet material precast body, process conditions are: 840 ℃ of depositing temperatures, pressure 0.3kPa, propylene flow 28ml/min, Ar throughput 270ml/min, sedimentation time 45h.
Depositing depositing silicon carbide matrix on the carbon fiber two dimension sheet material of RESEARCH OF PYROCARBON interface layer, process conditions are: 850 ℃ of depositing temperatures, pressure 3kPa, H
2Throughput 170ml/min, Ar throughput 280ml/min, 27 ℃ of trichloromethyl silane temperature, H
2With the molal weight ratio of MTS be 11, sedimentation time 250h forms the semi-finished product ceramic matric composite.
Cutting forms ' T ' font bolt blank on the semi-finished product ceramic matric composite, utilizes diamond-impregnated wheel, and attaching nut is tapping on bolt blank, the semi-finished product bolt of formation.The angle θ of the worm tooth of making 2 is 2 * 45 °=90 °.
The semi-finished product bolt at 950 ℃ of five infiltration pyrolysis Polycarbosilanes, is heat-treated 3h for 1450 ℃ then.
After the cleaning of the pyrolysis product between the bolt thread tooth 2, continue deposition SiC inoxidzable coating with the CVI method again, depositing temperature is 850 ℃, and gas is trichloromethyl silane, and sedimentation time 65h obtains finished product C/SiC compound material bolt.
The C/SiC compound material bolt that present embodiment is prepared, through the room temperature tensile strength test, the worm tooth of bolt does not take off the tooth phenomenon, but screw rod generation rupture failure, the bolt tension rupture strength is 230MPa.
Embodiment 3: just spreading first layer with the 1K carbon fiber according to 0 °, just spreading the second layer perpendicular to first layer in the above, become+30 ° of angles tiltedly to spread the 3rd layer in the second layer in the above, become-30 ° of angles tiltedly to spread the 4th layer in the 3rd layer in the above again, and, prepare carbon fiber two dimension sheet material precast body according to the size of required bolt according to this sequence alternate shop layer.It is parallel with the screw rod center line of bolt just to spread layer fiber 3, and tiltedly layer fiber 4 in shop is parallel with 2 of the worm tooths of bolt.
Deposition RESEARCH OF PYROCARBON interface layer on carbon fiber two dimension sheet material precast body, process conditions are: 870 ℃ of depositing temperatures, pressure 0.3kPa, propylene flow 31ml/min, Ar throughput 310ml/min, sedimentation time 55h.
Depositing depositing silicon carbide matrix on the carbon fiber two dimension sheet material of RESEARCH OF PYROCARBON interface layer, process conditions are: 900 ℃ of depositing temperatures, pressure 3kPa, H
2Throughput 230ml/min, Ar throughput 310ml/min, 31 ℃ of trichloromethyl silane temperature, H
2With the molal weight ratio of MTS be 9, sedimentation time 230h forms the semi-finished product ceramic matric composite.
Cutting forms ' T ' font bolt blank on the semi-finished product ceramic matric composite, utilizes diamond-impregnated wheel, and attaching nut is tapping on bolt blank, the semi-finished product bolt of formation.The angle θ of the worm tooth of making 2 is 2 * 30 °=60 °.
The semi-finished product bolt at 1000 ℃ of six infiltration pyrolysis Polycarbosilanes, is heat-treated 3h for 1550 ℃ then.
After the cleaning of the pyrolysis product between the bolt thread tooth 2, continue deposition SiC inoxidzable coating with the CVI method again, depositing temperature is 950 ℃, and gas is trichloromethyl silane, and sedimentation time 55h obtains finished product C/SiC compound material bolt.
The C/SiC compound material bolt that present embodiment is prepared, through the room temperature tensile strength test, the worm tooth of bolt does not take off the tooth phenomenon, but screw rod generation rupture failure, the bolt tension rupture strength is 210MPa.
Embodiment 4: just spreading first layer with the 1K carbon fiber according to 0 °, just spreading the second layer perpendicular to first layer in the above, become+30 ° of angles tiltedly to spread the 3rd layer in the second layer in the above, become-30 ° of angles tiltedly to spread the 4th layer in the 3rd layer in the above again, and, prepare carbon fiber two dimension sheet material precast body according to the size of required bolt according to this sequence alternate shop layer.It is parallel with the screw rod center line of bolt just to spread layer fiber 3, and tiltedly layer fiber 4 in shop is parallel with 2 of the worm tooths of bolt.
Deposition RESEARCH OF PYROCARBON interface layer on carbon fiber two dimension sheet material precast body, process conditions are: 900 ℃ of depositing temperatures, pressure 0.4kPa, propylene flow 25ml/min, Ar throughput 350ml/min, sedimentation time 40h.
Depositing depositing silicon carbide matrix on the carbon fiber two dimension sheet material of RESEARCH OF PYROCARBON interface layer, process conditions are: 1000 ℃ of depositing temperatures, pressure 2kPa, H
2Throughput 250ml/min, Ar throughput 350ml/min, 25 ℃ of trichloromethyl silane temperature, H
2With the molal weight ratio of MTS be 8, sedimentation time 220h forms the semi-finished product ceramic matric composite.
Cutting forms ' T ' font bolt blank on the semi-finished product ceramic matric composite, utilizes diamond-impregnated wheel, and attaching nut is tapping on bolt blank, the semi-finished product bolt of formation.The angle θ of the worm tooth of making 2 is 2 * 30 °=60 °.
The semi-finished product bolt at 1100 ℃ of five infiltration pyrolysis Polycarbosilanes, is heat-treated 4h for 1600 ℃ then.
After the cleaning of the pyrolysis product between the bolt thread tooth 2, continue deposition SiC inoxidzable coating with the CVI method again, depositing temperature is 1000 ℃, and gas is trichloromethyl silane, and sedimentation time 50h obtains finished product C/SiC compound material bolt.
The C/SiC compound material bolt that present embodiment is prepared, through the room temperature tensile strength test, the worm tooth of bolt does not take off the tooth phenomenon, but screw rod generation rupture failure, the bolt tension rupture strength is 215MPa.
Claims (1)
1, a kind of preparation method of ceramic base compound material bolt is characterized in that comprising the steps:
(a) with the 1K carbon fiber carry out 0/90 ° just spreading and ± the oblique shop of θ (0 °≤θ≤90 °), preparation carbon fiber two dimension sheet material precast body;
(b) deposition RESEARCH OF PYROCARBON interface layer on the prefabricated carbon fiber body, process conditions are: 800～900 ℃ of depositing temperatures, pressure 0.2～0.4kPa, propylene flow 25～35ml/min, Ar throughput 250～350ml/min, sedimentation time 40～60h;
(c) depositing depositing silicon carbide matrix on the two-dimentional sheet material of RESEARCH OF PYROCARBON interface layer, process conditions are: 800～1000 ℃ of depositing temperatures, pressure 2～4kPa, H
2Throughput 150～250ml/min, Ar throughput 250～350ml/min, 25～35 ℃ of trichloromethyl silane temperature, H
2With the molal weight ratio of MTS be 8～12, sedimentation time 220～260h forms the semi-finished product ceramic matric composite;
(d) cutting forms ' T ' font bolt blank on the semi-finished product ceramic matric composite, utilizes diamond-impregnated wheel, and attaching nut is tapping on bolt blank, forms the semi-finished product bolt;
(e) with the semi-finished product bolt at 900～1100 ℃ of infiltration pyrolysis Polycarbosilanes repeatedly, heat-treat 2～4h for 1400～1600 ℃ then;
(f) continue deposition SiC inoxidzable coating with the CVI method again, depositing temperature is 800～1000 ℃, and gas is trichloromethyl silane, and sedimentation time 50～70h obtains finished product C/SiC compound material bolt.
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| CN200810018039A CN100588844C (en) | 2008-04-25 | 2008-04-25 | Ceramic base compound material bolt preparation method |
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| CN200810018039A CN100588844C (en) | 2008-04-25 | 2008-04-25 | Ceramic base compound material bolt preparation method |
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| CN102701772A (en) * | 2012-06-07 | 2012-10-03 | 中国人民解放军国防科学技术大学 | Method for preparing bolt made of carbon fiber enhanced silicon carbide composite material |
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| CN102830001A (en) * | 2012-08-22 | 2012-12-19 | 西北工业大学 | Preparation method of ceramic-based composite material standard sample with lamination defects |
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| CN112794718A (en) * | 2021-01-27 | 2021-05-14 | 巩义市泛锐熠辉复合材料有限公司 | Ceramic matrix composite material stud and preparation method thereof |
| CN115716757A (en) * | 2022-11-21 | 2023-02-28 | 西安鑫垚陶瓷复合材料股份有限公司 | Ceramic matrix composite high-strength bolt and preparation method thereof |
| CN115716757B (en) * | 2022-11-21 | 2023-11-17 | 西安鑫垚陶瓷复合材料股份有限公司 | Ceramic matrix composite high-strength bolt and preparation method thereof |
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