CN103408316A - A connection method for a C/SiC composite material - Google Patents
A connection method for a C/SiC composite material Download PDFInfo
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- CN103408316A CN103408316A CN2013103111868A CN201310311186A CN103408316A CN 103408316 A CN103408316 A CN 103408316A CN 2013103111868 A CN2013103111868 A CN 2013103111868A CN 201310311186 A CN201310311186 A CN 201310311186A CN 103408316 A CN103408316 A CN 103408316A
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Abstract
The invention discloses a connection structure and a connection method which are capable of achieving reliable and firm connection between a C/SiC composite material (carbon-fiber-reinforced silicon carbide composite material) and other metals. According to the connection method, niobium (Nb), hydrogen and chlorine are used as raw materials, and a chemical vapor deposition (CVD) method is used to deposit the Nb on the C/SiC composite material (hereinafter referred to as CVDNb) to prepare a CVDNb/(C/SiC) composite material joint. The CVDNb, which is used as a transitional connection material, is welded with other metals (such as nickel-bases alloys, titanium alloys, niobium alloys), etc., thereby achieving assembly of other metal devices and special-shaped devices prepared from the C/SiC composite material. The CVDNb generates element diffusion and interface reactions during the deposition process on the surface of the C/SiC composite material, thereby forming good combination and avoiding subsequent thermal treatment. The connection method has low shape dimension precision requirements for the C/SiC composite material devices. The connection structure is simple and is good in air impermeability, strong in connection strength, high in using temperature and high in connection reliability. The connection method and the connection structure are particularly suitable for a connection problem of C/SiC composite material structural members used for space flight and aviation.
Description
Technical field
The present invention relates to interconnection technique and the syndeton of a kind of high temperature, high-strength, high reliability, airtight good, the C/SiC matrix material that can store for a long time.Be specially adapted to being connected of structure devices prepared by the C/SiC matrix material and other metal devices.
Background technology
At present, each big country of the world all attaches great importance to the development of the advanced weapons of system such as anti-ballistic grade, the U.S. using the development of missile defense systems and the configuration as a great state basic policy, China has also carried out the research in advance of advanced KKV.As the thrust chamber (as missile propulsive plant thrust chamber, anti-ballistic guided missile appearance control thrust chamber etc.) of power system, having adopted lightweight, high specific strength, resistant to elevated temperatures C/SiC(is carbon fibre reinforced silicon carbide) matrix material.China is through the development of more than ten years since " 95 ", broken through the gordian techniquies such as establishment moulding, the densification of C/SiC matrix material be anti-oxidant, and technology reaches its maturity, and has entered the through engineering approaches development stage.At present, C/SiC composite thrust chamber body section adopts bolt mode of connection alive to be connected with inspirator head titanium alloy, to solve engines ground test run problem.Owing to living, connecting the sealing ply adopted is graphite material, and along with the prolongation of storage period, graphite institute compression chord can discharge gradually, has gas leakage hidden danger, and reliability and security are poor.In addition, live and connect because Work fixture device is heavier, complex structure, offset the light advantage of C/SiC matrix material quality, even also improved the weight of whole thrust-chamber assembly.China effectively solves the connectivity problem of C/SiC composite thrust chamber so far not yet, becomes the maximum technology barrier of this engine through engineering approaches application.
Soldering is the more method of studying at present, but C/SiC matrix material void content is high, can discharge a large amount of gas in heat-processed, affects welding procedure and joint quality; While adopting diffusion welding to connect, need between joint interface, add some filler metal as middle connecting material, matching requirements for connecting material in the middle of meeting and C/SiC matrix material, often need C/SiC composite element apparent size is processed, the braiding structure of unavoidable damage C/SiC matrix material, so the research difficulty of diffusion welding craft is larger for some complex-shaped C/SiC composite elements.
Therefore chemical vapour deposition (CVD) is a kind of quiet forming technique, and can copy the external form of matrix, is particularly suitable for deposition material on the comparatively complicated device of external form.Present method adopts the CVD technology at C/SiC material surface deposition Nb, welding property by metal Nb excellence, by methods such as electrons leaves weldings, CVDNb and dissimilar metal (nickel-base alloy, titanium alloy, niobium alloy) are coupled together, what take CVDNb is the transition connecting material, realizes being connected of C/SiC matrix material device and other metal devices.In C/SiC composite material surface deposition Nb, the Nb atom can produce diffusion and react with body material, guarantees the stopping property of this syndeton; The use temperature of syndeton depends on the use temperature of deposition material Nb and body material C/SiC, is applicable to the connection of thermal structure spare; The short flow process operation of deposition is conducive to realize the repeatability of operation, and this interconnection technique is very advantageous when C/SiC matrix material large-scale application.
Summary of the invention
The purpose of this invention is to provide a kind of C/SiC matrix material and realize with other metallic substance the method for attachment and the syndeton that reliably are connected.Adopt the method for chemical vapour deposition, at C/SiC matrix material deposition Nb, preparation CVD Nb/(C
?/ SiC) composite joint, this composite joint can be applicable to the high-temperature engine jet pipe of space flight and aviation field and being welded to connect of other structural part.
Nb in the present invention adopts the clean forming technique preparation of CVD, adopts the open-tube process vertical reactor, adopts induction heating method to add hot basal body.With the on-the-spot chlorination process of negative pressure of vacuum, directly prepare, adopt the chloride technology deposition Nb of hydrogen reducing Nb.The C/SiC matrix material of take is matrix, and preparation and the weaving method of matrix C/SiC matrix material are not limit, and uninterrupted deposition Nb finally prepares CVD Nb/(C continuously on its surface
?/ SiC) composite structure.
Concrete depositing operation is as follows: material N b sheet, as in chlorination chambers, being heated to 200 ℃-400 ℃, being passed into to chlorine and produces chlorination reaction, produce NbCl
5, gaseous state NbCl
5With hydrogen, enter sediment chamber, by induction heating, the C/SiC matrices of composite material is heated to 900 ℃-1300 ℃, NbCl
5Under the reductive action of hydrogen, form the Nb atomic deposition at the C/SiC composite material surface.The Adsorption and desorption process of gas occurs in C/SiC composite material base surface under high temperature, at the matrix surface nucleation and growth process, is formed the solid deposited layer by the Nb of hydrogen reducing.
The Presence of an interface diffusion simultaneously of the Nb that the CVD legal system is standby and composite material interface and surface reaction, produce mutual diffusion between Nb and body material in preparation process, and generate Nb
3Si, NbC and Nb
5Si
3Deng middle phase, play the effect of interfacial seal.The average sedimentation rate of CVD Nb can reach 0.1mm/h, and depositing time is longer, and the niobium layer thickness is thicker, and thickness of diffusion layer is wider, and moderate interfacial diffusion and surface reaction help to improve sealing property and the intensity of composite-joint.In order to improve the bonding strength of C/SiC and CVDNb, can or be processed as step and groove structure by the preparation of C/SiC matrix material external surface, at complex configuration face deposition Nb, can further improve both due to the mechanical bond power of expanding with heat and contract with cold and producing.
CVDNb/(C/SiC prepared by the present invention) constitutional features of matrix material is: Nb crystal grain is perpendicular to the column crystal of matrix surface direction growth; CVDNb/(C/SiC) interface shape depends on C/SiC matrix material external surface; Between matrix and CVDNb, Elements Diffusion occurs, phase in the middle of forming, realize the sealing combination; Along with the prolongation of depositing time, thickness of diffusion layer is widened gradually, is conducive within the specific limits improve stopping property and the intensity of composite-joint.
CVDNb density of material prepared by the present invention reaches theoretical density more than 99.8%; CVDNb/(C/SiC) the composite structure interface bond strength reaches 180MPa; Under 2MPa pressure, being placed in alcohol and carrying out aeration test, overflows without bubble in interface.
Another object of the present invention is: this interconnection technique is except being applied in the C/SiC matrix material, but also expanded application to other ceramic matric composite (as C/C matrix material, foamy carbon material etc.) is connected with metallic substance.Adopt the CVD technology to prepare CVD Nb/ ceramic matric composite transition jointing and mainly comprise following step:
(1) take the ceramic matric composites such as C/SiC, C/C matrix material or foamy carbon material is depositing base, adopts chlorination reduction method CVD deposition techniques Nb;
(2) with the technique successive sedimentation Nb that optimizes to certain thickness;
(3) in deposition process, by controlling depositing temperature, chlorine and hydrogen intake and passing into speed and the sedimentation effect that time control deposits.
(4) according to follow-up connection request processing CVDNb.
The accompanying drawing explanation
The square C/SiC pipe fitting of Fig. 1 matrix, the square CVDNb/ of Fig. 2 (C/SiC) transition piece, the circular C/SiC pipe fitting of Fig. 3 matrix, circular CVDNb/ (C/SiC) transition piece of Fig. 4, Fig. 5 and Fig. 6 are CVDNb/ (C/SiC) transition piece, and Fig. 7 and Fig. 8 are the industry CT photo of VDNb/ (C/SiC) transition piece.
Embodiment
For better understanding the present invention, below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.But the scope of protection of present invention is not limited to the scope of case representation.
Embodiment 1
The present invention is for the preparation of the transition connecting structure of square C/SiC matrix material.The square C/SiC tubing of take is matrix, at the Nb layer of the above thickness of its surface deposition 4mm, finally obtains CVDNb/ (C/SiC) transition piece.The technique of deposition is as follows: the niobium sheet is as starting material, and chlorine is as reactant gases, and hydrogen is as reducing gas.Sediment chamber's vacuum tightness>=10
-2Torr, 900 ℃-1300 ℃ of depositing temperatures, the negative pressure of vacuum deposition, deposit 40 hours, as Fig. 1-Fig. 2.
Embodiment 2
Matrix in the embodiment of the present invention 1 is changed to C/SiC tubing, by its surface preparation CVDNb(thickness, being 4mm), can realize equally being connected of C/SiC tubing and other device.Depositing operation is identical with embodiment 1, as Fig. 3-Fig. 4.
Embodiment 3
Body material in the embodiment of the present invention 1 is changed to special-shaped device.The special-shaped device surface deposition thickness prepared at the C/SiC matrix material is the niobium ring of 2mm, according to follow-up assemble welding dimensional requirement processing CVDNb external surface, prepare CVDNb/ (C/SiC) transition piece, as Fig. 5 and Fig. 6, this transition piece can weld with other metal devices.
Embodiment 4
The linkage interface shape of the CVDNb in the present embodiment 3 and C/SiC matrix material depends on the external surface shape of C/SiC matrix material device, no matter groove or step all have the Nb deposition, both linkage interface good seals, without macroscopic defects, the industry CT photo of transition piece such as Fig. 7 and Fig. 8.
Claims (7)
- One kind can realize that C/SiC matrix material and other metals are reliable, firmly be connected syndeton, it is characterized in that: the C/SiC matrix material of take is matrix, at matrix surface, prepare CVD Nb, CVDNb layer thickness 0.1mm-5mm, Nb crystal grain is perpendicular to the column crystal of matrix surface direction growth, CVDNb and C/SiC interface shape depend on C/SiC matrix material external surface, between matrix and CVDNb, Elements Diffusion occur, phase in the middle of forming.
- 2. the method for attachment of a C/SiC matrix material and other metals, it is characterized in that: adopting the chemical vapour deposition niobium is that CVD Nb technology realizes being connected of C/SiC material and other metal partss, the C/SiC matrix material of take is matrix, at matrix surface, prepare CVD Nb, CVDNb layer thickness 0.1mm-5mm, concrete depositing operation is as follows: material N b sheet, as in chlorination chambers, being heated to 200 ℃-400 ℃, being passed into to chlorine and produces chlorination reaction, produce NbCl 5, gaseous state NbCl 5With hydrogen, enter sediment chamber, by induction heating, the C/SiC matrices of composite material is heated to 900 ℃-1300 ℃, NbCl 5Under the reductive action of hydrogen, form the Nb atomic deposition at the C/SiC composite material surface, obtain the CVDNb/C/SiC compound connection structure, according to actual needs, CVDNb is carried out to external surface processing.
- 3. the method for attachment of a kind of C/SiC matrix material according to claim 2 and other metals, it is characterized in that: described Nb adopts the clean forming technique preparation of CVD, adopt the open-tube process vertical reactor, adopt induction heating method to add hot basal body, with the on-the-spot chlorination process of negative pressure of vacuum, directly prepare, adopt the chloride technology deposition Nb of hydrogen reducing Nb, the C/SiC matrix material of take is matrix, preparation and the weaving method of matrix C/SiC matrix material are not limit, and uninterrupted deposition Nb finally prepares CVD Nb/(C continuously on its surface ?/ SiC) composite structure.
- 4. the method for attachment of a kind of C/SiC matrix material according to claim 2 and other metals is characterized in that:The average sedimentation rate of described CVD Nb can reach 0.1mm/h.
- 5. the method for attachment of a kind of C/SiC matrix material according to claim 2 and other metals is characterized in that: described C/SiC matrix material external surface preparation or be processed as step or groove structure.
- 6. a ceramic matric composite and method of attachment metallic substance is characterized in that: after adopting the CVD technology to prepare CVD Nb/ ceramic matric composite transition jointing, be connected with metallic substance, comprise following step:(1) take the ceramic matric composites such as C/SiC, C/C matrix material or foamy carbon material is depositing base, adopts chlorination reduction method CVD deposition techniques Nb;(2) with the technique successive sedimentation Nb that optimizes to certain thickness;(3) in deposition process, by controlling depositing temperature, chlorine and hydrogen intake and passing into speed and the sedimentation effect that time control deposits;(4) according to follow-up connection request processing CVDNb.
- 7. ceramic matric composite according to claim 6 and method of attachment metallic substance, it is characterized in that: described ceramic matric composite is C/C matrix material or foamy carbon material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108863425A (en) * | 2018-07-30 | 2018-11-23 | 西北工业大学 | The connection method of silicon carbide ceramics and its composite material |
| CN111138206A (en) * | 2020-01-11 | 2020-05-12 | 西安交通大学 | Amorphous carbon modified SiC nanowire continuous three-dimensional network structure wave-absorbing foam and preparation method thereof |
| CN113845377A (en) * | 2021-07-30 | 2021-12-28 | 陕西宏大空天新材料研究院有限责任公司 | Graphite-based niobium metal coating alloy material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101143397A (en) * | 2007-11-06 | 2008-03-19 | 北京有色金属研究总院 | C/C and C/SiC composite material and metal connecting method |
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2013
- 2013-07-23 CN CN2013103111868A patent/CN103408316A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101143397A (en) * | 2007-11-06 | 2008-03-19 | 北京有色金属研究总院 | C/C and C/SiC composite material and metal connecting method |
Non-Patent Citations (2)
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| ***等: "Al2O3陶瓷/Cu界面晶***向关系对断裂性能的影响", 《大连铁道学院学报》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108863425A (en) * | 2018-07-30 | 2018-11-23 | 西北工业大学 | The connection method of silicon carbide ceramics and its composite material |
| CN111138206A (en) * | 2020-01-11 | 2020-05-12 | 西安交通大学 | Amorphous carbon modified SiC nanowire continuous three-dimensional network structure wave-absorbing foam and preparation method thereof |
| CN111138206B (en) * | 2020-01-11 | 2021-04-20 | 西安交通大学 | Amorphous carbon modified SiC nanowire continuous three-dimensional network structure wave-absorbing foam and preparation method thereof |
| CN113845377A (en) * | 2021-07-30 | 2021-12-28 | 陕西宏大空天新材料研究院有限责任公司 | Graphite-based niobium metal coating alloy material and preparation method thereof |
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Application publication date: 20131127 |