CN107827477A - Based on Ti3SiC2Al mixed-powders are the carbon carbon composite reactive diffusion bonding method in intermediate layer - Google Patents

Based on Ti3SiC2Al mixed-powders are the carbon carbon composite reactive diffusion bonding method in intermediate layer Download PDF

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Publication number
CN107827477A
CN107827477A CN201711062538.5A CN201711062538A CN107827477A CN 107827477 A CN107827477 A CN 107827477A CN 201711062538 A CN201711062538 A CN 201711062538A CN 107827477 A CN107827477 A CN 107827477A
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sic
mixed
powders
powder
intermediate layer
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CN107827477B (en
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贾建刚
高昌琦
安亮
季根顺
郝相忠
杨兆庆
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Lanzhou University of Technology
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Lanzhou University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
    • C04B37/006—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts consisting of metals or metal salts
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
    • C04B2237/12—Metallic interlayers
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/32—Ceramic
    • C04B2237/36—Non-oxidic
    • C04B2237/363—Carbon

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Powder Metallurgy (AREA)
  • Ceramic Products (AREA)

Abstract

The invention discloses one kind to be based on Ti3SiC2Al mixed-powders are the carbon carbon composite reactive diffusion bonding method in intermediate layer, are comprised the following steps：By Al powder and Ti3SiC2Powder is mixed evenly by a certain percentage, obtains Ti3SiC2Al mixed-powders；By the Ti of gained3SiC2Al mixed-powders are uniformly layered between two blocks of once purged C/C composites, and powder pine dress thickness is 1mm；Ti is housed by above-mentioned3SiC2The C/C composites in Al mixed-powders intermediate layer temperature under protective atmosphere is 1450 DEG C, and pressure is pressure heat-preserving 30min under conditions of 10 20Mpa.The present invention is with Ti3SiC2Powder is main component, adds appropriate Al powder, and the high-temp and high-strength that the stabilization between C/C composites is realized by the method for solid-state diffusion and reaction-sintered connects.

Description

Based on Ti3SiC2- Al mixed-powders are the carbon carbon composite Reaction-diffusion terms in intermediate layer Connection method
Technical field
The present invention relates to material processing field, and in particular to one kind is based on Ti3SiC2- Al mixed-powders are the carbon in intermediate layer Carbon composite reactive diffusion bonding method.
Background technology
At present, C/C composites are widely used in the fields such as new material research and development, military project, and it has high-modulus, intensity Many premium properties such as greatly, high temperature resistant, corrosion-resistant, rub resistance wear, density is small, and C/C composites are effective with its own It is stably connected with significant.Existing connected mode includes mechanical (such as bolt) connection, active metal brazing connection, glass Connection and diffusion welding, each way have respective advantage and disadvantage.As active soldering connection exist solder largely penetrate into carbon/ Carbon base body and the shortcomings that especially strong joint face can not be formed, between glass linkage interface material element phase counterdiffusion easily there is gas The defects of hole, so as to have influence on the performance of C/C composite element superior functions.
Ti3SiC2Material combine metal and it is ceramic the advantages of, both high-yield strengths with ceramic material, high-melting-point is high Heat endurance and good inoxidizability, keep high intensity at high temperature, have the performance of metal again, have good electric conductivity With thermal conductivity and high temperature plasticity.
The content of the invention
To solve the above problems, the invention provides one kind to be based on Ti3SiC2- Al mixed-powders are answered for the carbon carbon in intermediate layer Condensation material reactive diffusion bonding method.
To achieve the above object, the technical scheme taken of the present invention is：
Based on Ti3SiC2- Al mixed-powders are the carbon carbon composite reactive diffusion bonding method in intermediate layer, including as follows Step：
S1, by Al powder and Ti3SiC2Powder is mixed evenly by a certain percentage, obtains Ti3SiC2- Al mixed-powders；
S2, the Ti by gained3SiC2- Al mixed-powders are uniformly layered between two blocks of once purged C/C composites, powder Last pine dress thickness is 1mm；
S3, by above-mentioned Ti is housed3SiC2The C/C composites in-Al mixed-powders intermediate layer are warm under argon gas or vacuum environment Spend for 1450 DEG C, pressure is pressure heat-preserving 30min under conditions of 10-20Mpa.
Wherein, Al powder accounts for the 5%~20% of mixed-powder percentage by weight in the step S1.
The invention has the advantages that：
With Ti3SiC2Powder is main component, adds appropriate Al powder, is realized by the method for solid-state diffusion and reaction-sintered The high-temp and high-strength connection of stabilization between C/C composites.
Brief description of the drawings
C/C composite articulamentum patterns and EDS spectrograms when Fig. 1 is containing 5wt%Al.
C/C composites articulamentum SEM patterns and EDS spectrograms when Fig. 2 is containing 10wt%Al.
Fig. 3 is the XRD spectra containing sample after the original powders of 10wt%Al and 1450 DEG C of sintering.
Fig. 4 is carbon carbon articulamentum SEM patterns and EDS spectrograms containing 20wt%Al contents.
Embodiment
In order that objects and advantages of the present invention are more clearly understood, the present invention is carried out with reference to embodiments further Describe in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair It is bright.
In following examples, used carbon carbon composite is the carbon fiber that Gansu Haoshi Carbon Fiber Co., Ltd. provides Cloth impregnation carbonization laminate；Used Ti3SiC2Powder and Al powder are commercially available prod.
Embodiment
Based on Ti3SiC2- Al mixed-powders are the carbon carbon composite reactive diffusion bonding method in intermediate layer, including as follows Step：
S1, by Al powder and Ti3SiC2Powder is mixed evenly by a certain percentage, obtains Ti3SiC2- Al mixed-powders, wherein Al powder accounts for percentage by weight 5%~20%；
S2, by Ti3SiC2- Al mixed-powders are uniformly layered between two blocks of cleaned C/C composites, and powder pine dress is thick Spend about 1mm；
S3, by above-mentioned Ti is housed3SiC2The C/C composites in-Al mixed-powders intermediate layer are warm under argon gas or vacuum environment Spend for 1450 DEG C, under conditions of pressure is 10-20Mpa after pressure heat-preserving 30min, you can complete the connection of composite.
C/C composite articulamentum patterns and EDS spectrograms when Fig. 1 is containing 5wt%Al.It can be seen that between composite Articulamentum thickness it is uniform, and densification is combined with basal body interface, the defects of between the two without obvious hole.Analyzed using EDS It was found that the boundary layer region Si contents for adjoining matrix material are also relatively middle apparently higher than other regions, the relative amount of Al elements Region is high, shows that aluminium generates diffusion to matrix in connection procedure is spread.Central area Ti, C, Si constituent content and original powder Each element ratio difference is larger in end, illustrates under the conditions of solid-state diffusion, in addition to the diffusion enrichment of Al element phase boundaries surface layer, Ti3SiC2No longer it is stabilized, but is decomposed with single-phase, and Si elements diffusions is near interface.
C/C composite articulamentum patterns and EDS spectrograms when Fig. 2 is containing 10wt%Al.It can be seen that between composite Articulamentum thickness it is uniform, and densification is combined with basal body interface, the defects of without obvious hole.Boundary when with Al content being 5wt% Surface layer is similar, and it is substantially high compared with intermediate region to adjoin boundary layer region Si and the Al content of matrix material, shows to connect in diffusion Aluminium generates diffusion to matrix in journey, as shown in Fig. 2 (b) and (c).
Fig. 3 is the XRD spectra containing sample after the original powders of 10wt%Al and 1450 DEG C of sintering.It can be seen that original powder Only contain Ti in body3SiC2, two independent phases of Al spectral peak, it was demonstrated that material composition is pure, without obvious impurity.After hot pressed sintering, Ti3SiC2Completely Al is generated with the anti-raw reactions of Al4SiC4, SiC, but still with the presence of a small amount of Al with elemental.Al4SiC4, SiC two Mutually there is excellent high-temperature behavior, therefore the mutually coordinated effect of two-phase material can improve articulamentum performance to a certain extent.Simple substance Al presence promotes solid-state diffusion and densified sintering product.
Fig. 4 is carbon carbon articulamentum SEM patterns and EDS spectrograms containing 20wt%Al contents.It is clear that, articulamentum It is well combined with matrix.EDS analyses find to be up to more than 90% with matrix junction Al, and remaining is then Si, illustrates interface still So two kinds of enrichment of element of Al and Si, but in this example Al elements exceed certain amount after, its enrichment phenomenon especially severe.
In summary, by Al powder by weight percentage 5%~20% and Ti3SiC2Powder mixes, available for carbon carbon composite wood Expect solid-state diffusion intermediate layer；Even compact is can obtain through being incubated 30min under 1450 DEG C, 10~20Mpa, is well combined with matrix Diffusion Bonding Joint.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (3)

1. it is based on Ti3SiC2- Al mixed-powders are the carbon carbon composite reactive diffusion bonding method in intermediate layer, it is characterised in that Comprise the following steps：
S1, by Al powder and Ti3SiC2Powder is mixed evenly by a certain percentage, obtains Ti3SiC2- Al mixed-powders；
S2, the Ti by gained3SiC2- Al mixed-powders are uniformly layered between two blocks of once purged C/C composites, powder pine Dress thickness is 1mm；
S3, by above-mentioned Ti is housed3SiC2The C/C composites in-Al mixed-powders intermediate layer temperature under protective atmosphere is 1450 DEG C, pressure is pressure heat-preserving 30min under conditions of 10-20Mpa.
2. it is based on Ti as claimed in claim 13SiC2- Al mixed-powders connect for the carbon carbon composite Reaction-diffusion terms in intermediate layer Connect method, it is characterised in that Al powder accounts for the 5%~20% of mixed-powder percentage by weight in the step S1.
3. it is based on Ti as claimed in claim 13SiC2- Al mixed-powders connect for the carbon carbon composite Reaction-diffusion terms in intermediate layer Connect method, it is characterised in that the protective atmosphere of the step S3 uses argon gas or vacuum environment.
CN201711062538.5A 2017-10-27 2017-10-27 Based on Ti3SiC2Reaction diffusion bonding method for carbon-carbon composite material with-Al mixed powder as intermediate layer Expired - Fee Related CN107827477B (en)

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Citations (5)

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CN1594213A (en) * 2004-06-23 2005-03-16 北京交通大学 Titanium silicon carbon block material using aluminium as additive and its preparing method
CN1800100A (en) * 2006-01-12 2006-07-12 上海大学 Ceramet Ti3SiC2 powder preparation method
CN101050116A (en) * 2007-03-20 2007-10-10 北京交通大学 Powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon, and preparation method
CN102584311A (en) * 2012-02-21 2012-07-18 内蒙古工业大学 Ceramic connection method by using high-temperature interlayer material

Patent Citations (5)

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Publication number Priority date Publication date Assignee Title
JPH01197374A (en) * 1987-12-24 1989-08-09 Kernforschungsanlage Juelich Gmbh Method for bonding silicon carbide molded body to silicon carbide or metal molded body
CN1594213A (en) * 2004-06-23 2005-03-16 北京交通大学 Titanium silicon carbon block material using aluminium as additive and its preparing method
CN1800100A (en) * 2006-01-12 2006-07-12 上海大学 Ceramet Ti3SiC2 powder preparation method
CN101050116A (en) * 2007-03-20 2007-10-10 北京交通大学 Powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon, and preparation method
CN102584311A (en) * 2012-02-21 2012-07-18 内蒙古工业大学 Ceramic connection method by using high-temperature interlayer material

Non-Patent Citations (10)

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FAN XIAOMENG ET AL.: "Friction and wear behaviors of C/C-SiC composites containing Ti3SiC2", 《WEAR》 *
LAN F T ET AL.: "Joining of carbon/carbon composites for nuclear applications", 《JOURNAL OF MATERIALS SCIENCE》 *
W.L.GU ET AL.: "Reactions between Al and Ti3SiC2 in temperature range of 600-650 °C", 《SCRIPTA MATERIALIA》 *
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