CN107311684A - A kind of dissipation heat-resistant composite material and preparation method thereof - Google Patents
A kind of dissipation heat-resistant composite material and preparation method thereof Download PDFInfo
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Abstract
A kind of dissipation heat-resistant composite material and preparation method thereof, the present invention relates to the resistance to ablative composite material field of lightweight.The invention solves the problems that existing preparation technology is complicated, the high technical problem of cost.The composite, as matrix, under the conditions of vacuum high-temperature, in the impregnant that matrix is immersed to melting, is made impregnant be immersed in matrix and forms composite by carbon material using the capillary force of micropore in matrix.Method：First, impregnant is prepared；2nd, matrix material is handled；3rd, graphite crucible is handled；4th, high temperature infiltrates.The dissipation heat-resistant composite material technique of the invention for preparing the resistance to ablation of lightweight is simple, the cycle is short, composite can carry out electric machining and machining, and manufacturing cost is low, ablation resistance is good.Larynx lining, jet vane for manufacturing solid rocket motor nozzle, it can also be used to manufacture the components such as end cap, nose of wing, tail vane and the steering orifice plate for manufacturing guided missile of hypersonic vehicle.
Description
Technical field
The present invention relates to the resistance to ablative composite material field of lightweight.
Background technology
Ablation resistant material is the important engineering material of national defence, field of aerospace, it is acted on be heating part in high temperature and
It is operationally interior to be able to maintain that aerodynamic configuration makes aircraft normal work under high velocity air Scouring Condition.With Aero-Space
Continuing to develop for technology proposes increasingly harsher requirement to ablation resistant material.Traditional ablation resistant material mainly includes infusibility
Metal and its composite, ceramic matric composite material, polymer matrix composites, tungsten ooze copper and carbon/carbon compound material etc..Its
These materials of resistance to ablative mechanism have their own characteristics each.Refractory metal such as tungsten, molybdenum, niobium and its composite are mainly heat sink heat absorption, but close
Degree is high, is unsatisfactory for the light-weight requirements of aircraft component；Ceramic matric composite is mainly radiative thermal protection mechanism, but ceramic heat resistant is rushed
Hitting property is poor, and machining is difficult；Polymer matrix composites are general to absorb external heat by being pyrolyzed, thus ablating rate is big；Tungsten oozes
The solar heat protection mechanism of copper product is sweating solar heat protection and heat sink solar heat protection；Carbon/carbon and its composite of modification are mainly radiation and ablation
Formula solar heat protection mechanism, but its preparation technology is complicated, and cost is very high.Under the conditions of oxyacetylene ablation, ablation 150s, the line of matrix material
The order of magnitude of ablating rate is 10-2um/s。
The content of the invention
The invention solves the problems that existing preparation technology is complicated, the high technical problem of cost, and a kind of dissipation solar heat protection is provided and is combined
Material and preparation method thereof.
A kind of dissipation heat-resistant composite material, by carbon material as matrix, under the conditions of vacuum high-temperature, matrix is immersed and melted
Impregnant in, impregnant is immersed in matrix using the capillary force of micropore in matrix and form composite.
A kind of preparation method of dissipation heat-resistant composite material, is specifically carried out according to the following steps：
First, 6~9 parts of silicon and 1~5 part of metal is weighed by mass fraction, is well mixed, obtains impregnant；
2nd, porous matrix is processed into component, is cleaned by ultrasonic, then dries；
3rd, graphite crucible is put into the induction coil for the intermediate frequency furnace that can be verted, fixed using quartz sand, in graphite crucible
Inwall coats BN；
4th, the impregnant that the component and step one handled step 2 is obtained is put into the graphite crucible of step 3 processing；
Under vacuum, it is 30~100 DEG C/min to control heating rate, is warming up to reactive infiltration temperature for 1400~2200 DEG C, consumption
It is 0.2~0.5 atmospheric pressure that argon gas to pressure is filled with after powder melting；Then keeping temperature infiltrates 20~30min, and vert graphite earthenware
Crucible pours out remaining dissipation agent in crucible, obtains dissipation heat-resistant composite material.
The beneficial effects of the invention are as follows：A kind of traditional material solar heat protection mechanism of the present invention, it is proposed that new mechanism of dissipation solar heat protection.
The solar heat protection mechanism of dissipation heat-resistant composite material is in the matrix of porous graphite or low density carbon carbon, to penetrate into gibbs oxidation certainly
By can less than matrix material as dissipation agent, during high temperature ablation, dissipation agent liquefaction, gasification absorb certain pneumatic
Heat, forms heat dissipation；Dissipation agent is reacted prior to matrix and the oxygen in boundary layer, and the oxygen formation oxygen in consumption boundary layer dissipates；Meanwhile,
The liquid ceramic of dissipation agent oxidation generation can further improve the ablation resistance of matrix in matrix surface formation protective layer.
Under high pressure and high-velocity particles stream Scouring Condition, the ceramic layer of liquid can be constantly washed, meanwhile, the dissipation agent of intrinsic silicon is not
Disconnected overflows chargeable heat and oxygen and the new ceramic layer of formation, forms the dissipation agent knot of nonequilibrium thermodynamics within a certain period of time
Structure.It is an object of the present invention to provide one kind can under high temperature, high pressure and high-velocity particles stream Scouring Condition ablating rate is low, aerodynamic configuration
Change the good and with low cost heat-resistant composite material of small, machinability.Dissipation heat-resistant composite material is a kind of new resistance to burning
Corrosion material, can meet hypersonic vehicle nose of wing, rocket chamber, the guided missile steering structure such as orifice plate and jet vane
The use demand of part.
The dissipation heat-resistant composite material preparation technology of the resistance to ablation of lightweight involved in the present invention is simple, the cycle is short, composite wood
Material can carry out electric machining and machining, and manufacturing cost is low, ablation resistance is good.
Resistance to ablative composite material prepared by the present invention is used for larynx lining, the jet vane for manufacturing solid rocket motor nozzle,
Available for components such as the manufacture end cap of hypersonic vehicle, nose of wing, tail vane and steering orifice plates for manufacturing guided missile.
Embodiment
Technical solution of the present invention is not limited to the embodiment of act set forth below, in addition to each embodiment it
Between any combination.
Embodiment one：A kind of dissipation heat-resistant composite material of present embodiment, by carbon material as matrix, in vacuum
Under hot conditions, in the impregnant that matrix is immersed to melting, the capillary force using micropore in matrix makes impregnant be immersed in base
Composite is formed in body.
Embodiment two：Present embodiment from unlike embodiment one：Matrix is graphite or low-density
C/C composites.It is other identical with embodiment one.
Embodiment three：Present embodiment from unlike embodiment one or two：Impregnant presses mass parts
Number is prepared by 6~9 parts of silicon and 1~5 part of metal, and wherein metal is one or more mixing in molybdenum, zirconium and aluminium.It is other
It is identical with embodiment one or two.
Embodiment four：A kind of preparation method of dissipation heat-resistant composite material described in embodiment one, tool
Body is carried out according to the following steps：
First, 6~9 parts of silicon and 1~5 part of metal is weighed by mass fraction, is well mixed, obtains impregnant；
2nd, porous matrix is processed into component, is cleaned by ultrasonic, then dries；
3rd, graphite crucible is put into the induction coil for the intermediate frequency furnace that can be verted, fixed using quartz sand, in graphite crucible
Inwall coats BN；
4th, the impregnant that the component and step one handled step 2 is obtained is put into the graphite crucible of step 3 processing；
Under vacuum, it is 30~100 DEG C/min to control heating rate, is warming up to reactive infiltration temperature for 1400~2200 DEG C, consumption
It is 0.2~0.5 atmospheric pressure that argon gas to pressure is filled with after powder melting；Then keeping temperature infiltrates 20~30min, and vert graphite earthenware
Crucible pours out remaining dissipation agent in crucible, obtains dissipation heat-resistant composite material.
Embodiment five：Present embodiment from unlike embodiment four：Metal is molybdenum, zirconium in step one
With one or more mixing in aluminium.It is other identical with embodiment four.
Embodiment six：Present embodiment from unlike embodiment four or five：Porous base in step 2
The porosity of body is 15~40%.It is other identical with embodiment four or five.
Embodiment seven：Unlike one of present embodiment and embodiment four to six：It is many in step 2
Hole matrix is graphite or low-density C/C composites.It is other identical with one of embodiment four to six.
Embodiment eight：Unlike one of present embodiment and embodiment four to seven：Dried in step 2
Dry temperature is 80~100 DEG C, and drying time is 2~4h.It is other identical with one of embodiment four to seven.
Embodiment nine：Unlike one of present embodiment and embodiment four to eight：Soaked in step one
Penetration enhancer is 6~9 parts of silicon and 1~4 part of metal molybdenum, and matrix material is high purity graphite in step 2, and density is 1.65~1.82g/
cm3, reactive infiltration temperature is 1800~2000 DEG C in step 4.It is other identical with one of embodiment four to eight.
Embodiment ten：Unlike one of present embodiment and embodiment four to nine：Soaked in step one
Penetration enhancer is 6~7 parts of silicon, 1~3 part of metal molybdenum and 1~2 part of metal zirconium, and matrix material is C/C composites, density in step 2
For 1.6~1.8g/cm3, reactive infiltration temperature is 1900~2200 DEG C in step 4.It is other with embodiment four to nine it
One is identical.
Embodiment 11：Unlike one of present embodiment and embodiment four to ten：In step one
Impregnant is 6~8 parts of silicon and 2~4 parts of metallic aluminiums, and reactive infiltration temperature is 1400~1700 DEG C in step 4.It is other with it is specific
One of embodiment four to ten is identical.
Embodiment 12：Present embodiment from unlike embodiment four to one of 11：Step one
Middle impregnant is 6~7 parts of silicon, 1~3 part of metal molybdenum and 1~2 part of metallic aluminium, in step 4 reactive infiltration temperature be 1700~
1900℃.It is other identical with embodiment four to one of 11.
Embodiment 13：Present embodiment from unlike embodiment four to one of 12：Step one
Middle impregnant is 6~9 parts of silicon and 1~4 part of metal zirconium, and matrix material is high purity graphite in step 2, density is 1.65~
1.82g/cm3, reactive infiltration temperature is 1700~1950 DEG C in step 4.It is other with the phase of embodiment four to one of 12
Together.
Embodiment 14：Present embodiment from unlike embodiment four to one of 13：Step one
Middle impregnant is 6~7 parts of silicon, 1~3 part of metal zirconium and 1~2 part of metallic aluminium, in step 4 reactive infiltration temperature be 1700~
1900℃.It is other identical with embodiment four to one of 13.
Embodiment 15：Present embodiment from unlike embodiment four to one of 14：Step one
Middle impregnant is 6~9 parts of silicon and 1~4 part of metal zirconium, and matrix material is C/C composites in step 2, density is 1.6~
1.8g/cm3, reactive infiltration temperature is 1700~1950 DEG C in step 4.It is other with the phase of embodiment four to one of 14
Together.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：
A kind of preparation method of dissipation heat-resistant composite material of the present embodiment, is specifically carried out according to the following steps：
First, 6 parts of silicon, 2 parts of metal molybdenums and 2 parts of metal zirconiums are weighed by mass fraction, is well mixed, obtains impregnant；
2nd, it is that 25% porous matrix is processed into component by porosity, is cleaned by ultrasonic, then dries；Matrix material is multiple for C/C
Condensation material, density is 1.7g/cm3；Drying temperature is 80 DEG C, and drying time is 4h；
3rd, graphite crucible is put into the induction coil for the intermediate frequency furnace that can be verted, fixed using quartz sand, in graphite crucible
Inwall coats BN；
4th, the impregnant that the component and step one handled step 2 is obtained is put into the graphite crucible of step 3 processing；
Under vacuum, it is 80 DEG C/min to control heating rate, and it is 2200 DEG C to be warming up to reactive infiltration temperature, is filled after dissipation agent melting
It is 0.5 atmospheric pressure to enter argon gas to pressure；Then keeping temperature infiltrates 30min, and the graphite crucible that verts dissipates remaining in crucible
Agent is poured out, and obtains dissipation heat-resistant composite material.
Dissipation heat-resistant composite material bending strength manufactured in the present embodiment brings up to 264MPa by the 136MPa of original matrix,
Improve 94%；Under the conditions of oxyacetylene ablation, ablation 150s, linear ablative rate is by original matrix 1.5 × 10-2Um/s is reduced to
1.6×10-3Um/s, improves an order of magnitude.
Embodiment two：
A kind of preparation method of dissipation heat-resistant composite material of the present embodiment, is specifically carried out according to the following steps：
First, 8 parts of silicon and 4 parts of metallic aluminiums is weighed by mass fraction, is well mixed, obtains impregnant；
2nd, it is that 15% porous matrix is processed into component by porosity, is cleaned by ultrasonic, then dries；Matrix material is high-purity
Graphite, density is 1.75g/cm3,；Drying temperature is 80 DEG C, and drying time is 4h；
3rd, graphite crucible is put into the induction coil for the intermediate frequency furnace that can be verted, fixed using quartz sand, in graphite crucible
Inwall coats BN；
4th, the impregnant that the component and step one handled step 2 is obtained is put into the graphite crucible of step 3 processing；
Under vacuum, it is 80 DEG C/min to control heating rate, and it is 1500 DEG C to be warming up to reactive infiltration temperature, is filled after dissipation agent melting
It is 0.5 atmospheric pressure to enter argon gas to pressure；Then keeping temperature infiltrates 30min, and the graphite crucible that verts dissipates remaining in crucible
Agent is poured out, and obtains dissipation heat-resistant composite material.
Dissipation heat-resistant composite material bending strength manufactured in the present embodiment is brought up to by the 61.7MPa of original matrix
122.3MPa, improve 98%；Under the conditions of oxyacetylene ablation, ablation 150s, linear ablative rate is by original matrix 5.6 × 10-2um/
S reductions by 2.5 × 10-3Um/s, improves an order of magnitude.
Claims (10)
1. a kind of dissipation heat-resistant composite material, it is characterised in that the composite by carbon material as matrix, in vacuum high-temperature bar
Under part, in the impregnant that matrix is immersed to melting, impregnant is set to be immersed in shape in matrix using the capillary force of micropore in matrix
Into composite.
2. a kind of dissipation heat-resistant composite material according to claim 1, it is characterised in that matrix is graphite or low-density C/C
Composite.
3. a kind of dissipation heat-resistant composite material according to claim 1, it is characterised in that impregnant by mass fraction by 6~
Prepared by 9 parts of silicon and 1~5 part of metal, wherein metal is one or more mixing in molybdenum, zirconium and aluminium.
4. a kind of preparation method of dissipation heat-resistant composite material as claimed in claim 1, it is characterised in that this method is specifically pressed
Following steps are carried out：
First, 6~9 parts of silicon and 1~5 part of metal is weighed by mass fraction, is well mixed, obtains impregnant；
2nd, porous matrix is processed into component, is cleaned by ultrasonic, then dries；
3rd, graphite crucible is put into the induction coil for the intermediate frequency furnace that can be verted, fixed using quartz sand, in graphite crucible inwall
Coat BN；
4th, the impregnant that the component and step one handled step 2 is obtained is put into the graphite crucible of step 3 processing；True
Under empty condition, it is 30~100 DEG C/min to control heating rate, and it is 1400~2200 DEG C, dissipation agent to be warming up to reactive infiltration temperature
It is 0.2~0.5 atmospheric pressure that argon gas to pressure is filled with after melting；Then keeping temperature infiltrates 20~30min, and the graphite crucible that verts will
Remaining dissipation agent is poured out in crucible, obtains dissipation heat-resistant composite material.
5. the preparation method of a kind of dissipation heat-resistant composite material according to claim 4, it is characterised in that golden in step one
Belong to for one or more mixing in molybdenum, zirconium and aluminium.
6. the preparation method of a kind of dissipation heat-resistant composite material according to claim 4, it is characterised in that many in step 2
The porosity of hole matrix is 15~40%.
7. the preparation method of a kind of dissipation heat-resistant composite material according to claim 4, it is characterised in that many in step 2
Hole matrix is graphite or low-density C/C composites.
8. the preparation method of a kind of dissipation heat-resistant composite material according to claim 4, it is characterised in that dried in step 2
Dry temperature is 80~100 DEG C, and drying time is 2~4h.
9. the preparation method of a kind of dissipation heat-resistant composite material according to claim 4, it is characterised in that anti-in step 4
It is 1800~2000 DEG C to answer infiltration temperature.
10. the preparation method of a kind of dissipation heat-resistant composite material according to claim 4, it is characterised in that anti-in step 4
It is 1500~1700 DEG C to answer infiltration temperature.
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| CN108218427A (en) * | 2018-03-27 | 2018-06-29 | 哈尔滨工业大学 | A kind of ternary alloy three-partalloy dissipation agent for carbon-based dissipation heat-resistant composite material of resistance to ablation and method |
| CN108358636A (en) * | 2018-03-27 | 2018-08-03 | 哈尔滨工业大学 | A kind of preparation method of carbon-based dissipation heat-resistant composite material |
| CN108409359A (en) * | 2018-03-27 | 2018-08-17 | 哈尔滨工业大学 | A kind of resistance to ablation ternary dissipation agent and application |
| CN110791674A (en) * | 2019-11-13 | 2020-02-14 | 哈尔滨工业大学 | Preparation method of refractory carbide particle reinforced tungsten copper infiltrated composite material |
| CN112853250A (en) * | 2020-12-28 | 2021-05-28 | 哈尔滨工业大学 | Preparation method of combined gas rudder component |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108218427A (en) * | 2018-03-27 | 2018-06-29 | 哈尔滨工业大学 | A kind of ternary alloy three-partalloy dissipation agent for carbon-based dissipation heat-resistant composite material of resistance to ablation and method |
| CN108358636A (en) * | 2018-03-27 | 2018-08-03 | 哈尔滨工业大学 | A kind of preparation method of carbon-based dissipation heat-resistant composite material |
| CN108409359A (en) * | 2018-03-27 | 2018-08-17 | 哈尔滨工业大学 | A kind of resistance to ablation ternary dissipation agent and application |
| CN108409359B (en) * | 2018-03-27 | 2021-01-15 | 哈尔滨工业大学 | Ablation-resistant ternary consumption powder and application |
| CN108218427B (en) * | 2018-03-27 | 2021-06-15 | 哈尔滨工业大学 | Ablation-resistant ternary alloy powder consumption agent for carbon-based dissipation heat-proof composite material and method |
| CN110791674A (en) * | 2019-11-13 | 2020-02-14 | 哈尔滨工业大学 | Preparation method of refractory carbide particle reinforced tungsten copper infiltrated composite material |
| CN110791674B (en) * | 2019-11-13 | 2021-03-30 | 哈尔滨工业大学 | Preparation method of refractory carbide particle reinforced tungsten copper infiltrated composite material |
| CN112853250A (en) * | 2020-12-28 | 2021-05-28 | 哈尔滨工业大学 | Preparation method of combined gas rudder component |
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