CN1990920B - Enhancement ablation thermal protection composite material and preparation method thereof - Google Patents
Enhancement ablation thermal protection composite material and preparation method thereof Download PDFInfo
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- CN1990920B CN1990920B CN2005101353497A CN200510135349A CN1990920B CN 1990920 B CN1990920 B CN 1990920B CN 2005101353497 A CN2005101353497 A CN 2005101353497A CN 200510135349 A CN200510135349 A CN 200510135349A CN 1990920 B CN1990920 B CN 1990920B
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Abstract
The invention relates to a thermal protective composite with enhancing ablation and the manufacturing method. It is the novel heat insulation composite, whose manufacturing technology is that PSA fabric cloth or/and Si-based fiber mixed weaved cloth is dipped in phenolic resin and is solidified to mould. The composite in invention is widely applied in the structuring with heat insulation and protection and is provided with better intensity, stability of dimension and machining technology. It breaks through the demand that prior material can not be ablated for a long time and can not insulate heat. It finds a better solved path for realizing integration of ablative heat protection and heat insulation of material.
Description
Technical field
The present invention relates to a kind of composite and preparation method thereof, refer to a kind of polysulphonamide fiber especially and strengthen ablation thermal protection composite material and processing method thereof with silicon based fiber shuffling cloth with low-heat conduction and high temperature resistance airflow scouring function.
Background technology
Under the occasion of High Temperature And Velocity airflow scouring, a kind of ablation thermal protection composite material is generally adopted on the structure surface, it be issue in the hot-fluid effect by material estrangedly separate, melt, the physics and the chemical change of multiple heat absorption such as evaporation, distillation and heat radiation, a large amount of heat energy are taken away in quality consumption with self, prevent that heat from importing internal structure into, thereby reach the heat insulation purpose of solar heat protection.As manned spaceship when the reentry; violent friction takes place with air; the surface temperature of airship will reach more than 1000 ℃; in order to protect the safety of astronaut and instrument and equipment; at outer surface parcel one deck thermal-protect ablation material of airship, when reentering, the ablation effect takes place and takes away heat in it; stopped importing into of heat, even make the hull-skin temperature of airship reach thousands of degree and cabin body temperature inside still maintains in the temperature range that the people can survive.
The kind of ablation thermal protection composite material has much at present, and it is one of them that cloth strengthens phenolic resins, and it is that fiber is made into cloth earlier, makes pre-impregnated fabric behind the impregnated phenolic resin, makes composite product by winding or mold pressing then.Technical maturity, the efficient of this class material are higher, thereby application is wider, and used this class material mainly contains 5 kinds both at home and abroad, is respectively carbon/phenolic aldehyde, high silicone, glass/phenolic aldehyde and nylon/phenolic aldehyde, terylene/phenolic aldehyde.Preceding 3 kinds of materials are that inorfil cloth strengthens phenolic resins, and its anti-ablation scouring capability is strong, but the heat-proof quality relative deficiency of material, are applicable to that environment for use is serious but occasion that the time is short; The 2 kinds of materials in back strengthen phenolic resins for organic fiber cloth, its thermal diffusivity is low, heat-proof quality is excellent, but heat resistance is relative with ablation property relatively poor, be applicable to the occasion that not high but time of serviceability temperature is long, the material that is between above-mentioned two classes in the heat-resistant composite material that cloth strengthens is a blank at present.
The major function of thermal-protect ablation material requires to reduce as much as possible the back side temperature rise of material, this is relevant with properties of materials (as thermal diffusivity, decomposition temperature, linear ablative rate, scour resistance, thickness etc.) with the environmental condition of using (as temperature, wash away shearing force, time etc.), is the result of above variant factors effect.The occasion higher in some environmental condition and service time is long, used material or ablation amount are excessive, or thermal diffusivity is bigger than normal, can not meet the demands simultaneously.Therefore, develop a kind ofly at ablating rate, the composite that aspects such as erosion resistibility and thermal diffusivity have better combination property is the task of top priority.
Summary of the invention
According to background technology, the object of the present invention is to provide a kind of heat-barrier material that can be used as, also can be used as thermal-protect ablation material, has higher intensity simultaneously, rigidity and better manufacturability can satisfy the long-time heat insulation requirement of ablating, the composite of ablative thermal protection and heat-insulation integrative.
To achieve these goals, the present invention is achieved through the following technical solutions:
A kind of enhancing ablation thermal protection composite material mainly is made up of following material: polysulphonamide fiber cloth or and the shuffling cloth of silicon based fiber.
Wherein, silicon based fiber comprises glass fibre, high silica fiber and quartz fibre.
Select different yarns for use at different service conditions, only require the high temperature insulating performance, others are not done requirement, select pure polysulphonamide fiber cloth for use; Except thermal insulation requires, also have the requirement of DIMENSIONAL STABILITY aspect, select the shuffling cloth of fragrant sulfone synthetic fibre and glass/glass fiber for use; Wash away demandingly for anti-ablation, select the shuffling cloth of fragrant sulfone synthetic fibre and high silica or quartz fibre for use.
The preparation method of above-mentioned enhancing ablation thermal protection composite material comprises the steps:
(1) fiber yarn is used in selected braiding: select different yarns for use at different service conditions;
(2) determine fabric construction:
E. fabric thickness 0.2-0.8mm, the line density by selecting yarn for use and knit close control, line density is more little, knits close more for a short time, and then fabric thickness is thin more;
F. fabric width 0.4-1.2m decides according to the drying oven width of impregnation equipment;
G. weaving manner: plain weave or twill and satin weave, fabric are thin selects plain weave for use, thicker twill or the satin weave selected for use;
H. the ratio of shuffling fiber: the weight ratio of fragrant sulfone synthetic fibre and silicon based fiber yarn is 1: 1, all evenly alternately arranges through broadwise;
(3) pre-impregnated fabric preparation: impregnated phenolic resin solution, the resin content of adhesive plaster are 30-60%, and fugitive constituent is 2-10%;
(4) moulding: sheet material adopts laminating technology, and cylindrical shell adopts winding process;
(5) solidify: by heating and cure under pressure, resin and reinforcing material are combined into one, solidification temperature 150-180 ℃, hardening time 3-6h, solidifying pressure 1-10Mpa.
Owing to adopted technique scheme, the present invention to have following advantage and effect:
1, the present invention's employing is that reinforcing material, phenolic resins are matrix with polysulphonamide fiber cloth, by flooding compound and advanced composite material (ACM) that be solidified into, its heat resistance improves about 150 ℃ than the terylene of commonly using/phenolic materials, and aspect heat-proof quality, be better than glass/phenolic materials, but processing technology is better than the aramid fiber material greatly simultaneously, for heat-resistant composite material has increased a new description of materials, now can be used on fire-resistant clothing or the fire proofing.
2, the present invention adopts polysulphonamide fiber and silicon based fiber (glass fibre or quartz fibre etc.) shuffling to weave cotton cloth, compound and the curing molding with phenolic resins then, made the advanced composite material (ACM) that has low thermal conductance and high temperature resistance airflow scouring concurrently, new material not only can be used as heat-barrier material, use but also can be used as thermal-protect ablation material, also have intensity, DIMENSIONAL STABILITY and processing technology preferably simultaneously, broken through current material and can not satisfy the anti-heat insulation requirement of long-time ablation, for ablative thermal protection and the heat-insulation integrative function that realizes material found solution route preferably.
Description of drawings
Fig. 1 is a process chart of the present invention
The specific embodiment
A kind of enhancing ablation thermal protection composite material mainly is made up of following material: polysulphonamide fiber cloth or and the shuffling cloth of silicon based fiber.Wherein, silicon based fiber comprises glass fibre, high silica fiber and quartz fibre.
The preparation method of above-mentioned enhancing ablation thermal protection composite material comprises the steps:
1, fiber yarn is used in selected braiding: select different yarns for use at different service conditions, only require the high temperature insulating performance, others are not done requirement, select pure polysulphonamide fiber cloth for use; Except thermal insulation requires, also have the requirement of DIMENSIONAL STABILITY aspect, select the shuffling cloth of fragrant sulfone synthetic fibre and glass/glass fiber for use; Wash away demandingly for anti-ablation, select the shuffling cloth of fragrant sulfone synthetic fibre and high silica or quartz fibre for use;
The polysulfonamide yarns parameter
The glass fiber yarn parameter
The high silica fiber yarn parameter
The quartz fibre yarn parameter
2, determine fabric construction:
(1) fabric thickness 0.2-0.8mm, the line density by selecting yarn for use and knit close control, line density is more little, knits close more for a short time, and then fabric thickness is thin more;
(2) fabric width 0.4-1.2m decides according to the drying oven width of impregnation equipment;
(3) weaving manner: plain weave or twill and satin weave, fabric are thin selects plain weave for use, thicker twill or the satin weave selected for use;
(4) ratio of shuffling fiber: the weight ratio of fragrant sulfone synthetic fibre and silicon based fiber yarn is 1: 1, all evenly alternately arranges through broadwise;
3, pre-impregnated fabric preparation: impregnated phenolic resin solution, the resin content of adhesive plaster are 30-60%, and fugitive constituent is 2-10%;
4, moulding: sheet material adopts laminating technology, and cylindrical shell adopts winding process;
5, solidify: by heating and cure under pressure, resin and reinforcing material are combined into one, solidification temperature 150-180 ℃, hardening time 3-6h, solidifying pressure 1-10Mpa.
By Fig. 1 main technique flow chart of the present invention is shown, the technical process of making the higher novel heat insulation material of temperature resistant grade of the present invention as seen from the figure also makes the technical process that has the advanced composite material (ACM) that hangs down thermal diffusivity and high temperature resistance airflow scouring concurrently simultaneously as can be known.
In addition, composite behind the shuffling is approximated to a network, silicon based fiber is the skeleton of grid, and " grid " middle filling is polysulphonamide fiber and phenolic resins, in ablation process, polysulphonamide fiber and resin at first decompose effusion, have been equivalent to " sweating " effect and take away heat, and silicon based fiber has and resists the ability of degrading of washing away preferably, and the linear ablative rate of material is played certain control and regulating action.Made new material not only can be used as heat-barrier material, uses but also can be used as thermal-protect ablation material, also has intensity, DIMENSIONAL STABILITY and processing technology preferably simultaneously, thereby has realized satisfying the long-time anti-heat insulation requirement of ablating.
Below with three more detailed explanation manufacturing process of embodiment:
Embodiment 1:
Name of product: high temperature resistant heat insulation plate
Size: 500 * 500 * 10
Implementation step is as follows:
(1) select for use pure polysulphonamide fiber yarn to weave cotton cloth, yarn linear density 75tex, the twist 200 sth. made by twisting/m, fabric construction are plain weave, and cloth is thick to be 0.25mm, and fabric width is 1.0m.
(2) the ba phenolic resin solution of dipping heat curing-type, the resin content of adhesive plaster is controlled to be 49 ± 4%, and fugitive constituent is controlled to be 4-8%.
(3) adhesive plaster of cutting 500 * 500 is 40, is stacked together after every the limit alignment, and hot press is put into after respectively spreading one deck release cloth in top and bottom.
(4) after adjunction pressed, press heated up, and heating rate is controlled to be 30 ℃/h, and the 8MPa that pressurizes to 95 ℃ of insulation 45min is warming up to 160 ℃ again, and insulation 4h solidifies and finishes.
(5) take out sheet material, remove release cloth, get product after the finishing of four limits.
The main performance of above institute panel is as follows:
| Sequence number | Project | Performance |
| 1 | TENSILE STRENGTH MPa | 25 |
| 2 | Elongation at break % | 0.70 |
| 3 | Bending strength MPa | 50 |
| 4 | Density g/cm 3 | 1.30 |
| 5 | Puffer linear ablative rate mm/s | 0.49 |
| 6 | Specific heat capacity J/g.K (100 ℃) | 1.46 |
| 7 | Thermal conductivity W/m.K (100 ℃) | 0.25 |
| 8 | Linear expansion coefficient 10 -6/℃(100℃) | 40 |
Embodiment 2:
Name of product: cylindrical shell collet
Size: internal diameter Φ 600, thickness 5mm, long 1000mm.
Implementation step is as follows:
(1) selects the shuffling cloth of polysulphonamide fiber and glass fibre for use.Polysulfonamide yarns line density 75tex, the twist 200 sth. made by twisting/m; Glass fibre line density 72tex, the twist 55 sth. made by twisting/m, fabric construction are plain weave, and through broadwise polysulphonamide fiber and glass fibre all at interval, cloth is thick to be 0.25mm, and fabric width is 1.0m.
(2) the ba phenolic resin solution of dipping heat curing-type, the resin content of adhesive plaster is controlled to be 41 ± 4%, and fugitive constituent is controlled to be 4-8%.Adhesive plaster is cut into the wide adhesive tape of 50mm along warp-wise, falls into dish.
(3) use Cloth Tape Winding Machine wound in parallel moulding on Φ 600 mould tires.The control winding tension is 10～20kgf, and temperature is 60-130 ℃, and main shaft whenever circles, and the dolly 10mm that gos ahead repeats to twine 5 times.
(4) the wrap surface is coated successively fluorine four glass cloth, airfelt, fluorine four glass cloth, wrap vacuum bag at last, connect vacuum nozzle; Heating rate with 30 ℃/h heats up, and is forced into 1.5MPa behind the insulation 1h down at 100 ℃; Be warming up to 160 ℃ then, insulation 4h.
(5) solidify the rear surface and carry out machined, to thickness be 5mm, it is 1200m that two ends are cut to length, the demoulding gets product.
It is as follows to make the product Specifeca tion speeification:
| Sequence number | Project | Performance |
| 1 | Female to TENSILE STRENGTH MPa | 75 |
| 2 | Elongation at break % | 1.6 |
| 3 | Female to bending strength MPa | 120 |
| 4 | Density g/cm 3 | 1.45 |
| 5 | Puffer linear ablative rate mm/s | 0.40 |
| 6 | Specific heat capacity J/g.K (100 ℃) | 1.35 |
| 7 | Thermal conductivity W/m.K (100 ℃) | 0.26 |
| 8 | Linear expansion coefficient 10 -6/℃(100℃) | 12.7 |
Embodiment 3:
Name of product: the anti-heat insulation tapered sleeve of ablating
Size: small end internal diameter Φ 260 holds internal diameter Φ 600 greatly, thickness 12mm, long 1200mm.
Implementation step is as follows:
(1) selects the shuffling cloth of polysulphonamide fiber and quartz fibre for use.Polysulfonamide yarns line density 75tex, the twist 200 sth. made by twisting/m; Quartz fibre line density 85tex, the twist 50 sth. made by twisting/m, fabric construction are plain weave, and through broadwise polysulphonamide fiber and quartz fibre all at interval, cloth is thick to be 0.30mm, and fabric width is 1.1m.
(2) the ammonia phenol resin solution of dipping heat curing-type, the resin content of adhesive plaster is controlled to be 45 ± 4%, and fugitive constituent is controlled to be 4-8%.Is the wide adhesive tape of 70mm with adhesive plaster along becoming the 45o tapered cut to become width with warp-wise, sews up and is overlapped to form continuous long adhesive tape, falls into dish then.
(3) it is Wrapping formed to use Cloth Tape Winding Machine to tilt at the awl tire, and the control winding tension is 1～10kgf, and temperature is 60-130 ℃, winding angle 15o, and main shaft whenever circles, the dolly 1.5mm that gos ahead.
(4) the wrap surface is coated successively fluorine four glass cloth, airfelt, fluorine four glass cloth, wrap the sealing poly-bag at last, connect vacuum nozzle; Heating rate with 30 ℃/h heats up, and is forced into 8MPa behind the insulation 1h down at 100 ℃; Be warming up to 180 ℃ then, insulation 5h.
(5) solidify the back product surface and carry out machined, to thickness be 12mm, in the calculating location cutting at two ends, length is 1200mm, the demoulding gets product.
It is as follows to make the product Specifeca tion speeification:
| Sequence number | Project | Performance |
| 1 | Female to TENSILE STRENGTH MPa | 40 |
| 2 | Elongation at break % | 1.20 |
| 3 | Female to bending strength MPa | 75 |
| 4 | Density g/cm 3 | 1.40 |
| 5 | Puffer linear ablative rate mm/s | 0.25 |
| 6 | Specific heat capacity J/g.K (100 ℃) | 1.30 |
| 7 | Thermal conductivity W/m.K (100 ℃) | 0.30 |
| 8 | Linear expansion coefficient 10 -6/℃(100℃) | 16.0 |
Design philosophy of the present invention also can expand to reinforced fiber can adopt various organic fibers, inorfil carries out shuffling, comprise but do not limit glass fibre, high silica (quartz) fiber and polysulphonamide fiber, fabric construction includes but not limited to flat fabric, and the shuffling proportion of fibers comprises but do not limit 1: 1.
It is the various phenol of solvent and the polycondensation product of aldehyde with ethanol, methyl alcohol that the resin that the present invention is suitable for comprises various, comprises but does not limit aerospace industry commonly used barium phenolic aldehyde, high pure novolac, ammonia phenolic resins.Remove in addition, this composite molding technique also can be applied to other resin system.
Claims (2)
1. one kind strengthens ablation thermal protection composite material, and its shuffling cloth with polysulphonamide fiber and silicon based fiber is reinforcing material, and phenolic resins is matrix, by flooding compound and curing forms; It is characterized in that: silicon based fiber comprises glass fibre, high silica fiber or quartz fibre; For the situation that has thermal insulation and DIMENSIONAL STABILITY to require, select the shuffling cloth of fragrant sulfone synthetic fibre and glass fibre for use; Wash away demandingly for anti-ablation, select the shuffling cloth of fragrant sulfone synthetic fibre and high silica or quartz fibre for use; Polysulfonamide yarns density 60tex-200tex, the twist≤400 sth. made by twisting/m, ultimate strength 〉=10N, size content≤5%; Glass fiber yarn line density 60tex-200tex, the twist≤200 sth. made by twisting/m, ultimate strength 〉=30N, SiO2 content 〉=60%; High silica fiber thread density 70tex-260tex, the twist≤200 sth. made by twisting/m, ultimate strength 〉=15N, SiO2 content 〉=96%; Quartz fibre thread density 60tex-200tex, the twist≤200 sth. made by twisting/m, ultimate strength 〉=30N, SiO2 content 〉=99%.
2. the preparation method of enhancing ablation thermal protection composite material as claimed in claim 1 is characterized in that comprising the steps:
(1) fiber yarn is used in selected braiding, selects different yarns for use at different service conditions;
(2) determine fabric construction:
A. fabric thickness 0.2-0.8mm, the line density by selecting yarn for use and knit close control, line density is more little, knits close more for a short time, and then fabric thickness is thin more;
B. fabric width 0.4-1.2m decides according to the drying oven width of impregnation equipment;
C. weaving manner: plain weave or twill or satin weave, fabric are thin selects plain weave for use, thicker twill or the satin weave selected for use;
D. the ratio of shuffling fiber: the weight ratio of fragrant sulfone synthetic fibre and silicon based fiber yarn is 1: 1, all evenly alternately arranges through broadwise;
(3) pre-impregnated fabric preparation: impregnated phenolic resin solution, the resin content of adhesive plaster are 30-60%, and fugitive constituent is 2-10%;
(4) moulding: sheet material adopts laminating technology, and cylindrical shell adopts winding process;
(5) solidify: by heating and cure under pressure, resin and reinforcing material are combined into one, solidification temperature 150-180 ℃, hardening time 3-6h, solidifying pressure 1-10Mpa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2005101353497A CN1990920B (en) | 2005-12-30 | 2005-12-30 | Enhancement ablation thermal protection composite material and preparation method thereof |
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| CN2005101353497A CN1990920B (en) | 2005-12-30 | 2005-12-30 | Enhancement ablation thermal protection composite material and preparation method thereof |
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| CN1990920A CN1990920A (en) | 2007-07-04 |
| CN1990920B true CN1990920B (en) | 2011-08-17 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101440193B (en) * | 2007-11-23 | 2010-12-22 | 航天材料及工艺研究所 | Carbon / phenolic heat insulating composite material and manufacturing process thereof |
| CN105566919B (en) * | 2015-07-31 | 2019-03-15 | 沈阳理工大学 | A kind of compound heat vulcanized silicone rubber base ablation resistant material of carbon cloth and preparation method thereof |
| CN106496927B (en) * | 2016-11-03 | 2021-10-01 | 华东理工大学 | Low-density ablation heat-insulation composite material and preparation method thereof |
| US20180305846A1 (en) * | 2017-02-10 | 2018-10-25 | Asahi Kasei Kabushiki Kaisha | Glass cloth, prepreg, and printed wiring board |
| CN107523911B (en) * | 2017-09-06 | 2019-09-17 | 无锡富仕德高科特材制造有限公司 | The preparation method of the high silicon oxygen doubled yarn of type containing reinforcing rib |
| CN109707952A (en) * | 2018-12-27 | 2019-05-03 | 湖北航天技术研究院总体设计所 | A kind of solar heat protection heat insulation structural with Graded Density |
| CN110028755A (en) * | 2019-04-04 | 2019-07-19 | 北京卫星制造厂有限公司 | One kind is for escape velocity reentry thermal protection material and its preparation method and application |
| CN112321894B (en) * | 2020-11-02 | 2022-07-08 | 航天特种材料及工艺技术研究所 | Non-coating light ablation-resistant heat-insulation composite material and preparation method thereof |
| CN112553744A (en) * | 2020-11-30 | 2021-03-26 | 陕西华特新材料股份有限公司 | Glass fiber mixed fabric and weaving method thereof |
| CN112680866B (en) * | 2020-12-11 | 2022-05-10 | 江苏恒力化纤股份有限公司 | Ablation material compounded by fiber cloth and preparation method thereof |
| CN115353324B (en) * | 2022-08-30 | 2024-06-25 | 航天特种材料及工艺技术研究所 | High-heat-conductivity ablation-resistant composite material and preparation method thereof |
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| CN1072226A (en) * | 1991-06-26 | 1993-05-19 | 纳幕尔杜邦公司 | Ballistic composite |
| CN1686696A (en) * | 2005-06-10 | 2005-10-26 | 中国航空工业第一集团公司北京航空材料研究院 | Preparation method of liquid state shaping composite material preshaped body |
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