CN103011874A - Connection method of carbon/silicon carbide composite component - Google Patents
Connection method of carbon/silicon carbide composite component Download PDFInfo
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- CN103011874A CN103011874A CN2012105216978A CN201210521697A CN103011874A CN 103011874 A CN103011874 A CN 103011874A CN 2012105216978 A CN2012105216978 A CN 2012105216978A CN 201210521697 A CN201210521697 A CN 201210521697A CN 103011874 A CN103011874 A CN 103011874A
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Abstract
The invention relates to a connection method of a carbon/silicon carbide composite component. According to the method, the carbon/silicon carbide component is subjected to CVI (chemical vapor infiltration) deposition in a vacuum furnace through a CVI deposition preparation method. Carbon/silicon carbide composite connection rods and a connected piece are assembled, and SiC is deposited between the connected piece and the connection rods by a chemical vapor infiltration method so as to realize connection finally. The deposition process includes pretreatment CVI and final CVI deposition. SiC is deposited between the connection rods and a parent material in the carbon/silicon carbide material compounding process so as to integrate the connection rods having equal strength to the parent material with the parent material finally, thus realizing connection. The method provided in the invention has the characteristics of bonding and fastening connection.
Description
Technical field
The present invention relates to field of compound material, specifically a kind of method of attachment of member of carbon/composite material of silicon carbide.
Background technology
Carbon/composite material of silicon carbide, has high temperature resistant, low density, high than strong, good in oxidation resistance, corrosion-resistant and the advantage such as calamitous damage do not occur, become long lifetime below 1650 ℃, 1900 ℃ of following finite life and the heat structure/functional materials in instantaneous life-span below 2800 ℃, have wide practical use in fields such as aircraft engine hot-end component, space shuttle thermal protection system (TPS) and rocket nozzles, be successfully applied to aerospace field.
But because the restriction of carbon/composite material of silicon carbide weaving, realize large-scale, accurate, complex component is very difficult.Therefore, research and develop reliable interconnection technique, significant to the application of carbon/composite material of silicon carbide.The coupling method of existing carbon/composite material of silicon carbide comprises substantially that solder bonding metal, transition liquid-phase diffusion connect, online liquid infiltration joining or the self-deformation by material produce pressing etc., and above-mentioned several methods of attachment have following characteristics:
1, solder bonding metal is because braze material joint thermal expansivity is different from fertile material, cause easily producing stress concentration at joining zone, and because the solder fusing point is lower, the use temperature of brazed joint is no more than 500 ℃, and the application of temperature of this and matrix material is that can not using of larger gap arranged.
2, to connect be to adopt to make intermediate course than the low-melting metallic substance of mother metal to transition liquid-phase diffusion, when being heated to certain temperature intermediate course instantaneous time liquid phase and in insulating process the even scattering and permeating of liquid phase molecule solidify at mother metal, thereby be integrally connected.And break-off just occurs in metal intermediate layer in the time of 1250 ℃, and obvious above-mentioned method of attachment use temperature is low, can not satisfy the high temperature conjunction requirement more than 1600 ℃ of carbon/composite material of silicon carbide.
3, online liquid infiltration joining connects by infiltrating after the linking agent fusing to form in the material hole in the matrix material preparation process.Linking agent is generally the Ni base, wherein contains an amount of Ti, Cr, Zr isoreactivity element, and connecting temperature is 1300 ℃, and Bonding pressure is 20MPa, and the tie-time is 45min, vacuum protection.Online liquid infiltration joining method is a kind of high temperature conjunction method, and the tie-time is short, and web member physical bond ability is strong and can alleviate to a certain extent the thermal stresses that produces in the connection procedure.It is high that but the method connects temperature, and whole connection procedure must carry out under vacuum condition, high to equipment requirements, therefore link cost is higher, and the applicable surface of linking agent is narrow, needs exploitation to be applicable to the high temperature resistant linking agent of different composite material, thereby has hindered the practice of this method.
4, the self-deformation generation pressing metallic substance by material has good ductility, can produce the connection that pressing realizes member by self-deformation, but carbon/composite material of silicon carbide does not possess good ductility, and effect is relatively poor when adopting this kind method of attachment to connect carbon/composite material of silicon carbide member.
In sum, several methods of attachment are not the best approaches that carbon/composite material of silicon carbide connects more than.
Summary of the invention
In order to overcome existing carbon/composite material of silicon carbide method of attachment poor reliability, especially can not satisfy the service requirements under carbon/composite material of silicon carbide hot environment, be difficult to simultaneously satisfy the industrial deficiency of mass of carbon/composite material of silicon carbide member, the present invention proposes the method for attachment of a kind of carbon/composite material of silicon carbide member.
The present invention includes following steps:
Step 1 is made web member; Feeding and be processed into a plurality of shaft-like carbon/composite material of silicon carbide web member on carbon/composite material of silicon carbide plate; The density of described carbon/composite material of silicon carbide plate is 1.65~1.75g/cm
3
Step 2 is processed connecting hole at the plate that is connected; The aperture of connecting hole is identical with the diameter of described web member; Spacing between each adjacent connecting hole center is 10mm; Fall 7 °~8 ° angles at the two ends in described hole, with the mating surface between the plate that strengthens web member and be connected, making the deposit thickness between the described mating surface is 0.12~0.17 millimeter.
Step 3, pre-connection; Plate piece is stacked, and each web member packed in the connecting hole on the plate piece one by one, and the difference of altitude that makes each web member top finishes the pre-connection of web member and plate piece in ± 0.15mm, obtains the pre-connection member that is comprised of web member and plate piece.
Step 4 is carried out pre-deposition to the pre-connection member; It is to carry out the CVI deposition in the vacuum oven of 600mm that described pre-connection member is placed diameter, and processing condition are: 900~1100 ℃ of depositing temperatures are evacuated to pressure 2~4kPa, H
2Airshed 150~250ml/min, Ar airshed 250~350ml/min, 25~35 ℃ of trichloromethyl silane temperature, H
2Be 8~12 with the molar mass ratio of trichloromethyl silane, depositing time 80~100h.
Step 5 is excised the web member termination that is exposed at through the pre-connection component surface behind the pre-deposition by the mode of mechanical workout.
Step 6, deposition pre-connection member; To again depositing through the pre-connection member behind the pre-deposition of mechanical workout, make the further densification of pre-connection component surface; The process of deposition pre-connection member is identical with the processing parameter of the processing parameter that adopts and step 4 pre-deposition; Obtain post-depositional carbon/silicon carbide pre-connection member.
Step 7, surperficial ground finish obtains carbon/silicon carbide transom.
The present invention considers the characteristic of carbon/carbon/silicon carbide ceramic matrix composite, utilize chemical vapor infiltration (being called for short CVI) preparation technology, realized the on-line joining process method that the manufacturing with carbon/composite material of silicon carbide is connected together with connection, namely the control porosity is proceeded the densification of matrix material to realize Best link after connection is finished in carbon/composite material of silicon carbide manufacturing processed.This method of attachment is finished in the material preparation process, has taken into full account the requirement that connects, and makes connection procedure be reduced to minimum to the damaging action of material; The CVI densification process in later stage is not only finished material preparation, simultaneously can provide inoxidzable coating for whole material and connection, has strengthened the resistance of oxidation of member, has embodied really that to connect preparation processing integrated; Connect finish after, the pore in the former connected piece precast body has reduced 70%~85%, and web member adopts the carbon consistent with being connected member/composite material of silicon carbide to prepare, and has improved strength of joint, use temperature and the thermal shock resistance of transom; Web member can prepare in enormous quantities, saves the manufacturing cost of carbon/silicon carbide transom, realizes mass production.
Description of drawings
Fig. 1 is CVI vapour deposition synoptic diagram;
Fig. 2 is the metallographic structure figure of pre-connection member before the deposition;
Fig. 3 is pre-connection member front view;
Fig. 4 is the metallographic structure figure that deposits transom behind two stoves through CVI;
Fig. 5 is the harmless photo of the X ray of transom;
Fig. 6 is schema of the present invention.
Embodiment
With reference to accompanying drawing
Embodiment 1:
Present embodiment is the method for attachment of a kind of carbon/composite material of silicon carbide member.
Step 1 is made web member.Be 1.65g/cm in density
3Carbon/composite material of silicon carbide plate on feeding and be processed into 32 shaft-like carbon/composite material of silicon carbide web members.
Step 2 is processed connecting hole at the plate that is connected.Described plate piece is of a size of 80 * 50mm, and the aperture of connecting hole is identical with the diameter of described web member, and the spacing between each adjacent connecting hole center is 10mm.Fall 7 ° of angles at the two ends in described hole, with the mating surface between the plate that strengthens web member and be connected, making the deposit thickness between the described mating surface is 0.12mm.
Step 3, pre-connection.Plate piece is stacked, and each web member packed in the connecting hole on the plate piece one by one, and the difference of altitude that makes each web member top finishes the pre-connection of web member and plate piece in ± 0.15mm, obtains the pre-connection member that is comprised of web member and plate piece.
Step 4 is carried out pre-deposition to the pre-connection member.It is to carry out the CVI deposition in the vacuum oven of 600mm that described pre-connection member is placed diameter, and processing condition are: 900 ℃ of depositing temperatures are evacuated to pressure 2kPa, H
2Airshed 150ml/min, Ar airshed 250ml/min, 25 ℃ of trichloromethyl silane temperature, H
2Be 8 with the molar mass ratio of trichloromethyl silane, depositing time 80h.
Step 5, processing.Excise the web member termination that is exposed at through the pre-connection component surface behind the pre-deposition by the mode of mechanical workout.
Step 6, deposition pre-connection member.To again depositing through the pre-connection member after the mechanical workout, make the further densification of pre-connection member, obtain post-depositional carbon/silicon carbide pre-connection member, the processing parameter that this step deposition process adopts is identical with step 4.
Step 7, surperficial ground finish obtains carbon/silicon carbide transom.
After the carbon that present embodiment obtains/silicon carbide transom process X ray nondestructive testing, can see that combination closely connects reliable between web member and the connected piece; Through the electronic universal tester test, three-point bending strength is 362MPa; Through 700 ℃, 10 hours high temperature oxidation experiment, oxidative mass loss was 2.1%.
Embodiment 2:
Present embodiment is the method for attachment of a kind of carbon/composite material of silicon carbide member.
Step 1 is made web member.Be 1.70g/cm in density
3Carbon/composite material of silicon carbide plate on feeding and be processed into 32 shaft-like carbon/composite material of silicon carbide web members.
Step 2 is processed connecting hole at the plate that is connected.Described plate piece is of a size of 80 * 50mm, and the aperture of connecting hole is identical with the diameter of described web member, and the spacing between each adjacent connecting hole center is 10mm.Fall 8 ° of angles at the two ends in described hole, with the mating surface between the plate that strengthens web member and be connected, making the deposit thickness between the described mating surface is 0.15mm.
Step 3, pre-connection.Plate piece is stacked, and each web member packed in the connecting hole on the plate piece one by one, and the difference of altitude that makes each web member top finishes the pre-connection of web member and plate piece in ± 0.15mm, obtains the pre-connection member that is comprised of web member and plate piece.
Step 4 is carried out pre-deposition to the pre-connection member.It is to carry out the CVI deposition in the vacuum oven of 600mm that described pre-connection member is placed diameter, and processing condition are: 1000 ℃ of depositing temperatures are evacuated to pressure 3kPa, H
2Airshed 200ml/min, Ar airshed 300ml/min, 30 ℃ of trichloromethyl silane temperature, H
2Be 10 with the molar mass ratio of trichloromethyl silane, depositing time 90h.
Step 5, processing.Excise the web member termination that is exposed at through the pre-connection component surface behind the pre-deposition by the mode of mechanical workout.
Step 6, deposition pre-connection member.To again depositing through the pre-connection member after the mechanical workout, make the further densification of pre-connection member, obtain post-depositional carbon/silicon carbide pre-connection member, the processing parameter that this step deposition process adopts is identical with step 4.
Step 7, surperficial ground finish obtains carbon/silicon carbide transom.
After the carbon that present embodiment obtains/silicon carbide transom process X ray nondestructive testing, can see that combination closely connects reliable between web member and the connected piece; Through the electronic universal tester test, three-point bending strength is 375MPa; Through 700 ℃, 10 hours high temperature oxidation experiment, oxidative mass loss was 2.3%.
Embodiment 3:
Present embodiment is the method for attachment of a kind of carbon/composite material of silicon carbide member.
Step 1 is made web member.Be 1.75g/cm in density
3Carbon/composite material of silicon carbide plate on feeding and be processed into 32 shaft-like carbon/composite material of silicon carbide web members.
Step 2 is processed connecting hole at the plate that is connected.Described plate piece is of a size of 80 * 50mm, and the aperture of connecting hole is identical with the diameter of described web member, and the spacing between each adjacent connecting hole center is 10mm.Fall 7 ° of angles at the two ends in described hole, with the mating surface between the plate that strengthens web member and be connected, making the deposit thickness between the described mating surface is 0.18mm.
Step 3, pre-connection.Plate piece is stacked, and each web member packed in the connecting hole on the plate piece one by one, and the difference of altitude that makes each web member top finishes the pre-connection of web member and plate piece in ± 0.15mm, obtains the pre-connection member that is comprised of web member and plate piece.
Step 4 is carried out pre-deposition to the pre-connection member.It is to carry out the CVI deposition in the vacuum oven of 600mm that described pre-connection member is placed diameter, and processing condition are: 1100 ℃ of depositing temperatures are evacuated to pressure 4kPa, H
2Airshed 250ml/min, Ar airshed 350ml/min, 35 ℃ of trichloromethyl silane temperature, H
2Be 12 with the molar mass ratio of trichloromethyl silane, depositing time 100h.
Step 5, processing.Excise the web member termination that is exposed at through the pre-connection component surface behind the pre-deposition by the mode of mechanical workout.
Step 6, deposition pre-connection member.To again depositing through the pre-connection member after the mechanical workout, make the further densification of pre-connection member, obtain post-depositional carbon/silicon carbide pre-connection member, the processing parameter that this step deposition process adopts is identical with step 4.
Step 7, surperficial ground finish obtains carbon/silicon carbide transom.
After the carbon that present embodiment obtains/silicon carbide transom process X ray nondestructive testing, can see that combination closely connects reliable between web member and the connected piece; Through the electronic universal tester test, three-point bending strength is 378MPa; Through 700 ℃, 10 hours high temperature oxidation experiment, oxidative mass loss was 1.9%.
Claims (2)
1. the method for attachment of carbon/composite material of silicon carbide member is characterized in that, may further comprise the steps:
Step 1 is made web member; Feeding and be processed into a plurality of shaft-like carbon/composite material of silicon carbide web member on carbon/composite material of silicon carbide plate;
Step 2 is processed connecting hole at the plate that is connected; The aperture of connecting hole is identical with the diameter of described web member;
Spacing between each adjacent connecting hole center is 10mm; Fall 7 °~8 ° angles at the two ends in described hole, with the mating surface between the plate that strengthens web member and be connected, making the deposit thickness between the described mating surface is 0.12~0.17 millimeter;
Step 3, pre-connection; Plate piece is stacked, and each web member packed in the connecting hole on the plate piece one by one, and the difference of altitude that makes each web member top finishes the pre-connection of web member and plate piece in ± 0.15mm, obtains the pre-connection member that is comprised of web member and plate piece;
Step 4 is carried out pre-deposition to the pre-connection member; It is to carry out the CVI deposition in the vacuum oven of 600mm that described pre-connection member is placed diameter, and processing condition are: 900~1100 ℃ of depositing temperatures are evacuated to pressure 2~4kPa, H2 airshed 150~250ml/min, Ar airshed 250~350ml/min, 25~35 ℃ of trichloromethyl silane temperature, H
2Be 8~12 with the molar mass ratio of trichloromethyl silane, depositing time 80~100h;
Step 5 is excised the web member termination that is exposed at through the pre-connection component surface behind the pre-deposition by the mode of mechanical workout;
Step 6, deposition pre-connection member; To again depositing through the pre-connection member behind the pre-deposition of mechanical workout, make the further densification of pre-connection component surface; The process of deposition pre-connection member is identical with the processing parameter of the processing parameter that adopts and step 4 pre-deposition; Obtain post-depositional carbon/silicon carbide pre-connection member;
Step 7, surperficial ground finish obtains carbon/silicon carbide transom.
2. the as claimed in claim 1 method of attachment of carbon/composite material of silicon carbide member is characterized in that, the density of described carbon/composite material of silicon carbide plate is 1.65~1.75g/cm
3
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Cited By (6)
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CN103232255A (en) * | 2013-05-07 | 2013-08-07 | 湖南友缘新材料有限公司 | Preparation method of carbon/carbon composite material flat plate with carbide coating on surface |
CN103557221A (en) * | 2013-10-11 | 2014-02-05 | 航天特种材料及工艺技术研究所 | Online connection preparation method for C/SiC materials |
CN104831351A (en) * | 2015-05-29 | 2015-08-12 | 西安鑫垚陶瓷复合材料有限公司 | Crucible cover plate for polysilicon ingot furnace and cover plate surface coating method |
CN107879756A (en) * | 2017-11-15 | 2018-04-06 | 西安鑫垚陶瓷复合材料有限公司 | A kind of method that original position online inside carbon ceramic composite material prepares silica whisker |
CN109516828A (en) * | 2018-10-15 | 2019-03-26 | 广东工业大学 | The silicon carbide ceramics of a kind of connection method and its preparation of nucleus silicon carbide ceramics and application |
CN112552068A (en) * | 2020-11-26 | 2021-03-26 | 西安鑫垚陶瓷复合材料有限公司 | Protection tool and method for rivet welding of C/SiC-ZrC and C/SiC ceramic matrix composite |
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CN1597621A (en) * | 2004-07-27 | 2005-03-23 | 西北工业大学 | Connecting method of ceramic-base composite |
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- 2012-12-07 CN CN2012105216978A patent/CN103011874A/en active Pending
Patent Citations (1)
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CN1597621A (en) * | 2004-07-27 | 2005-03-23 | 西北工业大学 | Connecting method of ceramic-base composite |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103232255A (en) * | 2013-05-07 | 2013-08-07 | 湖南友缘新材料有限公司 | Preparation method of carbon/carbon composite material flat plate with carbide coating on surface |
CN103557221A (en) * | 2013-10-11 | 2014-02-05 | 航天特种材料及工艺技术研究所 | Online connection preparation method for C/SiC materials |
CN104831351A (en) * | 2015-05-29 | 2015-08-12 | 西安鑫垚陶瓷复合材料有限公司 | Crucible cover plate for polysilicon ingot furnace and cover plate surface coating method |
CN107879756A (en) * | 2017-11-15 | 2018-04-06 | 西安鑫垚陶瓷复合材料有限公司 | A kind of method that original position online inside carbon ceramic composite material prepares silica whisker |
CN107879756B (en) * | 2017-11-15 | 2019-11-15 | 西安鑫垚陶瓷复合材料有限公司 | A method of silica whisker is prepared in situ online inside carbon ceramic composite material |
CN109516828A (en) * | 2018-10-15 | 2019-03-26 | 广东工业大学 | The silicon carbide ceramics of a kind of connection method and its preparation of nucleus silicon carbide ceramics and application |
CN109516828B (en) * | 2018-10-15 | 2021-03-30 | 广东工业大学 | Novel connection method of silicon carbide ceramic for core, silicon carbide ceramic prepared by connection method and application of silicon carbide ceramic |
CN112552068A (en) * | 2020-11-26 | 2021-03-26 | 西安鑫垚陶瓷复合材料有限公司 | Protection tool and method for rivet welding of C/SiC-ZrC and C/SiC ceramic matrix composite |
CN112552068B (en) * | 2020-11-26 | 2022-12-20 | 西安鑫垚陶瓷复合材料有限公司 | Protection tool and method for rivet welding of C/SiC-ZrC and C/SiC ceramic matrix composite |
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Application publication date: 20130403 |