CN101143397A - C/C and C/SiC composite material and metal connecting method - Google Patents
C/C and C/SiC composite material and metal connecting method Download PDFInfo
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Abstract
The invention is a method of binding compound materials of the C/SiC and C/C, which belongs to the technology field of binding heterogeneous materials. The processing procedures are as following: 1. The surface of the e compound materials of the C/SiC and C/Cis pretreated, which comprise the surface of the connecting are grinding, cleaning, vacuum biscuit firing, preparation of double-layer metal film and microvacum heat treatment and so on. 2. The transition layer of the connecting area surface gradient of the compound materials of the C/SiC is coated and sintered. 3. The compound materials with the gradient transition layer as the felted phase is brazed with the metal in vacuum. The invention is characterized in that the gradient transition layer is directly used as the materials that bind the compound materials with the metal; the gradient transition layer is double-layered or multilayered (sub-layered) structure; from the inner basal body to the outer part of the compound materials, the melting points of active brazing alloy adopted by each sub-layer gradually lower, the coefficient of heat expansion that adjust volume percentage composition gradually lower and the coefficient of heat expansion of the sub-layers gradually rise. The brazing ceramic metal connecting piece of the invention has good strength, air tightness and wide application field, which is suitable for various non-metallic fibers, such as ceramics of SiC, Si<SUB>3</SUB>N<SUB>4</SUB>, Al<SUB>2</ SUB>O<SUB>3</SUB>, AlN and so on and applicable for connecting the ceramic matrix compound materials with particulate reinforced with the metal.
Description
Technical field
The present invention relates to the method for attachment of a kind of C/C, C/SiC composite and metal, belong to dissimilar materials and connect (welding) technical field.
Background technology
The aerospace craft dynamical system requires its thrust chamber (appearance motor power chamber etc. is repaiied at missile propulsive plant thrust chamber, the attitude of satellite, track control thrust chamber, long-range missile warhead end) to possess: characteristics such as light weight, response is fast, size is little, reliability height.Such thrust chamber is by jet pipe (body portion) and propellant ejector filler (head) formation that is tightly connected.C fiber reinforcement SiC (C/SiC), C fiber reinforced graphite (C/C) composite have a series of excellent properties as: density little (density 1.75-2.10g/cm
3), light weight, high-temperature behavior characteristics such as outstanding (intensity height, modulus are big, fracture toughness and anti-wear performance excellence, antiscour, thermostability is good, thermal coefficient of expansion is low, the capacity of heat transmission is high).Such material is under 1000-1300 ℃ of condition, and intensity index increases than under the normal temperature; 1650 ℃, the strength and stiffness in the time of can keeping room temperature; 2000 ℃, still have higher mechanical property, be desirable spacecraft thrust chamber jet pipe material.Traditional C/SiC, C/C composite jet pipe and generally adopt mechanical seal to connect being connected of metal head (propellant spray device).This method of attachment, not only complex structure, thrust chamber weight increase, but also have that poor sealing performance, reliability are low, degradation shortcoming under the specific impulse.The composite jet pipe adopts Welding Structure can overcome above-mentioned shortcoming effectively with being connected of metal ejector filler, but because the physicochemical properties of C/C, C/SiC composite and metal, especially thermal expansion coefficient difference is bigger, and conventional ceramic-metal method of attachment is difficult to realize the reliable connection of the two.
Summary of the invention
The new method that is connected that the purpose of this invention is to provide a kind of C/C, C/SiC composite and metal, realize reliable connection the (welding) of C/SiC, C/C composite jet pipe and metal ejector filler, poor sealing performance, complex structure, the reliability that effectively solves the mechanical connection method is low, degradation problem under the thrust chamber specific impulse.
Technology path of the present invention (scheme) general overview is: at first prepare certain thickness, densification,, thermal coefficient of expansion graded firm with matrix bond and with C/SiC, C/C composite and connected the buffer layer material that metal is complementary on C/SiC, C/C matrices of composite material, utilize the welding transition layer of this material, realize that the soldering of the two connects as C/SiC, C/C jet pipe and metal ejector filler.
For achieving the above object, the present invention takes following technical scheme, and concrete steps are as follows:
(1) C/C, the surface preparation of C/SiC composite welding region
1. adopt the above skive of granularity 200 orders that grinding is carried out on C/C, C/SiC composite welding region surface, processing capacity is 0.1-0.5mm.After machining, the oil removing of composite integral ultrasonic, cleaning, hot-air seasoning (scavenging period, 30-120min; Solvent is carbon tetrachloride or acetone).After the cleaning, vacuum heat (vacuum 1-10Pa; Temperature: 1000-1300 ℃; Time: 30-120min).
2. C/C, the double-layer metal film preparation of C/SiC welding region surface.Bottom be Ti, Zr, Hf, V one of them, thickness 1-5 micron; The top layer be W, Mo, Ta, Nb one of them, thickness 1-5 micron.Process using PVD, CVD film preparing technology.After the weld zone bilayer film deposition, (vacuum is better than 10 * 10 to the heat treatment of composite overall vacuum
-3Pa; Temperature: 900-1300 ℃; Time: 15-90min).
(2) C/C, the preparation of C/SiC weld zone gradient welding transition layer.
The present invention is bonding phase with two or more active solders of can wetting C/C, C/SiC composite and having fusing point difference, with the lower SiC of the coefficient of expansion, SiC whisker, C fiber, W, Mo wherein one or more combination be that thermal coefficient of expansion is regulated phase, adopt not have and press or pressure sintering technology, prepare C/C, the C/SiC gradient welding transition layer of two-layer or multilayer (sublayer) structure.
Concrete steps are as follows:
1. gradient welding transition layer structure and material system design.0.5-5mm thick gradient transitional lay is two-layer or multilayer (sublayer) structure.Outside by matrices of composite material, the fusing point of the bonding phase in each sublayer (active solder) that 0.1-2.5mm is thick reduces successively with the volume fraction that the coefficient of expansion is regulated mutually.
2. gradient welding transition sublayer is joined cream.The palladium base of granularity-100 order, 20-80% percentage by volume, copper base, auri, titanium base, money base active solder one of them and 20-80% percentage by volume, granularity-100 purpose SiC, W, Mo, Al
2O
3Or the SiC whisker of length below 500 microns, C fiber wherein one or more batch mixings join cream and (join paste and adopt percentage by volume 40-70% guncotton solution, 10-30% butyl acetate, 10-30% diethy-aceto oxalate mixed solution.The viscosity of cream is in the 500-2000PaS scope).
3. the coating of each sublayer and sintering.Adopt craft or silk-screen printing technique, in C/C, the coating of C/SiC welding region, each sublayer of sintering gradient transitional lay.Outside by matrices of composite material, after the sublayer coating in adjacent of outer sublayer, sintering are finished, coating, sintering in its surface again, by that analogy.Each sublayer sintering process: the sintering environment, vacuum-sintering, vacuum is better than 10 * 10
-3Pa; Sintering temperature is higher than 20-60 ℃ of this layer active solder flow point; Pressure, 0-100MPa; Time, 5-60min.
(3) and solder bonding metal.
The C/C that the preparation of gradient welding transition layer finished, C/SiC composite can be connected with solder bonding metal by gradient welding transition layer.The welding temperature of soldering is lower than the fusing point of the bonding phase in gradient welding transition layer outer surface sublayer.
The specific embodiment
The invention will be further described below in conjunction with embodiment
Embodiment 1:
C/SiC is connected with Ti6Al4V's.
(1) C/SiC surface preparation
1. adopting granularity is that 200 purpose skives carry out grinding to C/SiC composite welding region surface, and processing capacity is 0.2mm.After finishing, integral ultrasonic oil removing, cleaning, hot-air seasoning (scavenging period, 60min; Solvent, carbon tetrachloride).After the cleaning, vacuum heat (vacuum 5Pa; Temperature, 1100 ℃; Time, 60min).
2. adopt magnetron sputtering technique on C/SiC welding region surface at first sputter one deck 3 micron thickness Ti films, the W film of sputter one deck 3 micron thickness subsequently.After finishing, (vacuum is better than 3.0 * 10 to the heat treatment of composite overall vacuum
-3Pa; Temperature, 1000 ℃; Time, 30min).
(2) C/SiC weld zone gradient transitional lay preparation
1. cream, coating, sintering are joined in gradient welding transition layer first sublayer.Volume fraction 40% ,-100 order PdNiTi (Ti, 3wt%; Ni, 38wt%; Pd, surplus.Flow point, about 1250 ℃) active solder and 60% volume fraction, granularity 200 purpose SiC particle batch mixings join cream (diluent is the mixed solution of guncotton solution, butyl acetate, diethy-aceto oxalate, and three's volume ratio is: 60: 25: 15).The viscosity of cream is controlled at about 1300PaS.After this, adopt manual mode to be coated with the creme of above-mentioned 2 millimeters thick at the C/SiC welding region.After finishing, whole 1290 ℃ of vacuum-sinterings, vacuum is better than 5.0 * 10
-3Pa; Temperature retention time, 15min.
2. cream, coating, sintering are joined in gradient welding transition layer second sublayer.Volume fraction 60% ,-100 order CuAlSiTi (Ti, 3wt%; Al, 1.0wt%; Si, 2.0wt%; Cu, surplus flow point, about 1030 ℃) active solder and 40% volume fraction, granularity 200 purpose SiC particle batch mixings join cream (diluent is the mixed solution of guncotton solution, butyl acetate, diethy-aceto oxalate, and three's volume ratio is: 60: 25: 15).The viscosity of cream is controlled at about 1300PaS.After this, adopt manual mode on the surface of C/SiC welding region first sublayer, to be coated with the creme of above-mentioned 2 millimeters thick.After finishing, 1050 ℃ of integral body, nothing are pressed, vacuum-sintering, and vacuum is better than 5.0 * 10
-3Pa; Temperature retention time, 15min.
(3) with the Ti6Al4V soldering.
After the preparation of C/SiC gradient welding transition layer finished, adopt TiCuNi (fusing point, 910 ℃; Flow point, 960 ℃) active solder and the soldering of Ti6Al4V titanium alloy.
(4) C/SiC and the performance test of Ti6Al4V connector
Shear strength:
Room temperature is greater than 55MPa; 600 ℃, greater than 43MPa.
Air-tightness:
2Mpa, gas medium, leakage detection by bubble emission method, join domain does not have visible bubble in bubble.
Embodiment 2:
C/C is connected with the C103 niobium alloy.
(1) C/C surface preparation
1. adopting granularity is that 200 purpose skives carry out grinding to C/C composite welding region surface, and processing capacity is 0.2mm.After finishing, integral ultrasonic oil removing, cleaning, hot-air seasoning (scavenging period, 60min; Solvent, carbon tetrachloride).After the cleaning, vacuum heat (vacuum 5Pa; Temperature, 1100 ℃; Time, 60min).
2. adopt magnetron sputtering technique on C/C welding region surface at first sputter one deck 3 micron thickness Ti films, the W film of sputter one deck 3 micron thickness subsequently.After finishing, (vacuum is better than 3.0 * 10 to the heat treatment of composite overall vacuum
-3Pa; Temperature, 1000 ℃; Time, 30min).
(2) C/C weld zone gradient transitional lay preparation
1. cream, coating, sintering are joined in gradient welding transition layer first sublayer.Volume fraction 40% ,-100 order PdNiTi (Ti, 3wt%; Ni, 38wt%; Pd, surplus.Flow point, about 1250 ℃) active solder and 60% volume fraction, granularity 200 purpose SiC particle batch mixings join cream (diluent is the mixed solution of guncotton solution, butyl acetate, diethy-aceto oxalate, and three's volume ratio is: 60: 25: 15).The viscosity of cream is controlled at about 1300PaS.After this, adopt manual mode to be coated with the creme of above-mentioned 2 millimeters thick at the C/SiC welding region.After finishing, whole 1290 ℃ of vacuum-sinterings, vacuum is better than 5.0 * 10
-3Pa; Temperature retention time, 15min.
2. cream, coating, sintering are joined in gradient welding transition layer second sublayer.Volume fraction 60% ,-100 order CuAlSiTi (Ti, 3wt%; Al, 1.0wt%; Si, 2.0wt%; Cu, surplus flow point, about 1030 ℃) active solder and 40% volume fraction, granularity 200 purpose SiC particle batch mixings join cream (diluent is the mixed solution of guncotton solution, butyl acetate, diethy-aceto oxalate, and three's volume ratio is: 60: 25: 15).The viscosity of cream is controlled at about 1300PaS.After this, adopt manual mode on the surface of C/C welding region first sublayer, to be coated with the creme of above-mentioned 2 millimeters thick.After finishing, 1050 ℃ of integral body, nothing are pressed, vacuum-sintering, and vacuum is better than 5.0 * 10
-3Pa; Temperature retention time, 15min.
(3) with the soldering of C103 niobium alloy.
After the preparation of C/SiC gradient welding transition layer finished, adopt TiCuNi (fusing point, 910 ℃; Flow point, 960 ℃) active solder and the soldering of C103 niobium alloy.
(4) C/C and the performance test of C103 connector
Shear strength:
Room temperature is greater than 60MPa; 600 ℃, greater than 48MPa.
Air-tightness:
2Mpa, gas medium, leakage detection by bubble emission method, join domain does not have visible bubble in bubble.
Embodiment 3:
C/SiC is connected with Ti6Al4V's.
(1) C/SiC surface preparation
1. adopting granularity is that 200 purpose skives carry out grinding to C/SiC composite welding region surface, and processing capacity is 0.2mm.After finishing, integral ultrasonic oil removing, cleaning, hot-air seasoning (scavenging period, 60min; Solvent, carbon tetrachloride).After the cleaning, vacuum heat (vacuum 5Pa; Temperature, 1100 ℃; Time, 60min).
2. adopt magnetron sputtering technique on C/SiC welding region surface at first sputter one deck 3 micron thickness Ti films, the W film of sputter one deck 3 micron thickness subsequently.After finishing, (vacuum is better than 3.0 * 10 to the heat treatment of composite overall vacuum
-3Pa; Temperature, 1000 ℃; Time, 30min).
(2) C/SiC weld zone gradient transitional lay preparation
1. cream, coating, sintering are joined in gradient welding transition layer first sublayer.Volume fraction 40% ,-100 order PdNiTi (Ti, 3wt%; Ni, 38wt%; Pd, surplus.Flow point, about 1250 ℃) active solder and 60% volume fraction, granularity 200 purpose SiC particle batch mixings join cream (diluent is the mixed solution of guncotton solution, butyl acetate, diethy-aceto oxalate, and three's volume ratio is: 60: 25: 15).The viscosity of cream is controlled at about 1300PaS.After this, adopt manual mode to be coated with the creme of above-mentioned 2 millimeters thick at the C/SiC welding region.After finishing, whole 1290 ℃ of vacuum-sinterings, vacuum is better than 5.0 * 10
-3Pa; Temperature retention time, 15min.
2. cream, coating, sintering are joined in gradient welding transition layer second sublayer.Volume fraction 55% ,-100 order CuAlSiTi (Ti, 3wt%; Al, 1.0wt%; Si, 2.0wt%; Cu, surplus flow point, about 1030 ℃) active solder and 45% volume fraction, granularity 200 purpose SiC particle batch mixings join cream (diluent is the mixed solution of guncotton solution, butyl acetate, diethy-aceto oxalate, and three's volume ratio is: 60: 25: 15).The viscosity of cream is controlled at about 1300PaS.After this, adopt manual mode on the surface of C/SiC welding region first sublayer, to be coated with the creme of above-mentioned 2 millimeters thick.After finishing, 1050 ℃ of integral body, nothing are pressed, vacuum-sintering, and vacuum is better than 5.0 * 10
-3Pa; Temperature retention time, 15min.
3. cream, coating, sintering are joined in gradient welding transition layer the 3rd sublayer.Volume fraction 70% ,-100 order TiCuNi (Ti, 70wt%; Cu, 15wt%; Ni, 15wt%; Flow point, about 960 ℃) the W powder batch mixing of 3 microns of active solder and 30% volume fraction, average grain diameters joins cream (diluent is the mixed solution of guncotton solution, butyl acetate, diethy-aceto oxalate, and three's volume ratio is: 60: 25: 15).The viscosity of cream is controlled at about 1300PaS.After this, adopt manual mode on the surface of C/SiC welding region second sublayer, to be coated with the creme of above-mentioned 2 millimeters thick.After finishing, 950 ℃ of integral body, nothing are pressed, vacuum-sintering, and vacuum is better than 5.0 * 10
-3Pa; Temperature retention time, 15min.
(3) with the Ti6Al4V soldering.
After the preparation of C/SiC gradient welding transition layer finished, adopt AgCuTi (fusing point, 780 ℃; Flow point, 820 ℃) active solder and the soldering of Ti6Al4V titanium alloy.
(4) C/SiC and the performance test of Ti6Al4V connector
Shear strength:
Room temperature is greater than 65MPa; 600 ℃, greater than 50MPa.
Air-tightness:
2Mpa, gas medium, leakage detection by bubble emission method, join domain does not have visible bubble in bubble.
Claims (7)
1. the method for attachment of a C/C, C/SiC composite and metal, it is characterized in that: it may further comprise the steps:
(1) C/C, the surface preparation of C/SiC composite welding region
1. adopt the above skive of granularity 200 orders that grinding is carried out on C/C, C/SiC composite welding region surface, processing capacity is 0.1-0.5mm, after machining, the oil removing of composite integral ultrasonic, cleaning, hot-air seasoning, scavenging period: 30-120min; Solvent is carbon tetrachloride or acetone; After the cleaning, vacuum heat, vacuum 1-10Pa; Temperature: 1000-1300 ℃; Time: 30-120min;
2. C/C, the double-layer metal film preparation of C/SiC welding region surface
Bottom be Ti, Zr, Hf, V one of them, thickness 1-5 micron; The top layer be W, Mo one of them, thickness 1-5 micron; Process using PVD, CVD film preparing technology; After the weld zone bilayer film deposition, the heat treatment of composite overall vacuum, vacuum is better than 10 * 10
-3Pa; Temperature: 900-1300 ℃; Time: 15-90min;
(2) C/C, the preparation of C/SiC weld zone gradient welding transition layer
The present invention is bonding phase with two or more active solders of can wetting C/C, C/SiC composite and having fusing point difference, with the lower SiC of the coefficient of expansion, SiC whisker, C fiber, W, Mo wherein one or more combination be that thermal coefficient of expansion is regulated phase, adopt not have and press or pressure sintering technology, prepare C/C, the C/SiC gradient welding transition layer of two-layer or multilayer (sublayer) structure;
Concrete steps are as follows:
1. gradient welding transition layer structure and material system design: the gradient transitional lay that 0.5-5mm is thick is two-layer or multilayer (sublayer) structure; Outside by matrices of composite material, the fusing point of the bonding phase in each sublayer (active solder) that 0.1-2.5mm is thick reduces successively with the volume fraction that the coefficient of expansion is regulated mutually;
2. gradient welding transition sublayer is joined cream: the palladium base of granularity-100 order, 20-80% percentage by volume, copper base, auri, titanium base, money base active solder one of them and 20-80% percentage by volume, granularity-100 purpose SiC, W, Mo, Al
2O
3Or the SiC whisker of length below 500 microns, C fiber wherein one or more batch mixings join cream, join paste and adopt percentage by volume 40-70% guncotton solution, 10-30% butyl acetate, 10-30% diethy-aceto oxalate mixed solution, the viscosity of cream is in the 500-2000PaS scope;
3. the coating of each sublayer and sintering: adopt craft or silk-screen printing technique, in the coating of C/C, C/SiC welding region, each sublayer of sintering gradient transitional lay, after outside by matrices of composite material, sublayer adjacent in, outer sublayer is coated with, sintering finishes, again in its surface the coating, sintering, by that analogy; Each sublayer sintering process: the sintering environment, vacuum-sintering, vacuum is better than 10 * 10
-3Pa; Sintering temperature: be higher than 20-60 ℃ of this layer active solder flow point; Pressure, 0-100MPa; Time: 5-60min;
(3) and solder bonding metal
The C/C that gradient welding transition layer preparation finished, C/SiC composite can be connected with solder bonding metal by gradient welding transition layer, select for use the brazing temperature of solder to be lower than the fusing point of the bonding phase in gradient welding transition layer outer surface sublayer.
2. according to the method for attachment of the described a kind of C/C of claim 1, C/SiC composite and metal, it is characterized in that in the described step (1): in C/C, C/SiC welding region surface preparation double-layer metal film and follow-up vacuum heat; Bottom be Ti, Zr, Hf, V one of them, thickness 1-5 micron; The top layer be W, Mo one of them, thickness 1-5 micron.
3. according to the method for attachment of the described a kind of C/C of claim 1, C/SiC composite and metal, it is characterized in that in the described step (2): gradient welding transition coating systems design, cohere mutually in palladium base, copper base, auri, titanium base, the money base system active solder one or more; It is SiC, W, Mo, Al mutually that thermal coefficient of expansion is regulated
2O
3, in the SiC whisker, C fiber one or more; Gradient welding transition layer is two-layer or multilayer (sublayer) structure, and is outside by matrices of composite material, and each sublayer is cohered the phase fusing point and reduced successively with the volume fraction that thermal coefficient of expansion is regulated mutually.
4. according to the method for attachment of the described a kind of C/C of claim 1, C/SiC composite and metal, it is characterized in that in the described step (2): gradient welding transition sublayer is joined cream; Granularity-100 order, percentage by volume 20-80% active solder and granularity-100 order, percentage by volume 20-80% thermal coefficient of expansion are regulated the phase batch mixing and are joined cream; Join paste and adopt percentage by volume 40-70% guncotton solution, 10-30% butyl acetate, 10-30% diethy-aceto oxalate mixed solution; The viscosity of cream is in the 500-2000PaS scope.
5. according to the method for attachment of the described a kind of C/C of claim 1, C/SiC composite and metal, it is characterized in that in the described step (2): the coating of each sublayer and sintering, adopt craft or silk-screen printing technique, in C/C, the coating of C/SiC welding region, each sublayer of sintering gradient transitional lay, outside by matrices of composite material, after the sublayer coating in adjacent of outer sublayer, sintering are finished, coating, sintering in its surface again, by that analogy; Each sublayer sintering process: the sintering environment, vacuum-sintering, vacuum is better than 10 * 10
-3Pa; Sintering temperature is higher than 20-60 ℃ of this layer active solder flow point; Pressure, 0-100MPa; Time: 5-60min.
6. according to the method for attachment of the described a kind of C/C of claim 1, C/SiC composite and metal, it is characterized in that described step (3): connect metal and comprise titanium alloy, niobium alloy.
7. according to the method for attachment of the described a kind of C/C of claim 1, C/SiC composite and metal, it is characterized in that described step (3): the welding transition layer is connected with solder bonding metal, selects for use the brazing temperature of solder to be lower than the fusing point of the bonding phase in gradient welding transition layer outer surface sublayer.
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