CN102584307A - C/SiC ceramic matrix composite spring and preparation method thereof - Google Patents
C/SiC ceramic matrix composite spring and preparation method thereof Download PDFInfo
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- CN102584307A CN102584307A CN2012100053692A CN201210005369A CN102584307A CN 102584307 A CN102584307 A CN 102584307A CN 2012100053692 A CN2012100053692 A CN 2012100053692A CN 201210005369 A CN201210005369 A CN 201210005369A CN 102584307 A CN102584307 A CN 102584307A
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Abstract
The invention discloses a C/SiC ceramic matrix composite spring and a preparation method thereof. According to the spring, silicon carbide is used as a matrix, 30 to 45 volume percent of carbon fibers are used as a reinforced phase, and a SiC coating is deposited on the surface of the spring; and the rigidity of the spring is 3.5 to 8 N/mm at room temperature, and the retention rate of the rigidity in the air at the temperature of between 800 and 1,200 DEG C is 70 to 85 percent. The method for preparing the spring comprises the following steps of: impregnating, winding for forming, and crosslinking at the room temperature to obtain a spring prefabricated member; heating, so that a paraffin die is melted or is dissolved in water, sleeving the demolded spring prefabricated member on a graphite die, and cracking to obtain a spring rough blank; compacting repeatedly to obtain a semi-finished product of the spring; and performing surface antioxidation treatment through chemical vapor deposition. The preparation method is simple, low in requirement on equipment and short in period, the net forming of the product is realized, and the quality and performance of the product are high.
Description
Technical field
The invention belongs to thermal protection system elevated-temperature seal technical field, relate in particular to a kind of high temperature resistant spring and preparation method thereof.
Background technology
The hypersonic aircraft flight velocity is more than 6Ma, and solar heat protection panel inside and outside differential pressure is big in the flight course, 1500 ℃ of surface temperatures high (>).Thermal protection system is embedded in aircraft surface by polylith solar heat protection panel and constitutes, and for preventing high temperature gas flow to internal delivery, need carry out elevated-temperature seal between the panel.Adopt the excellent C/SiC matrix material pad of resistance to elevated temperatures to realize that elevated-temperature seal is a kind of good sealing method; But this method exists the compressibility and the not enough problem of rebound resilience of pad, therefore can adopt high temperature spring that the ceramic seal pad is applied preliminary tension to realize the compression and the resilience of sealed structure.This ceramic plate sealed structure has proposed high temperature resistant (> 1200 ℃ to high temperature spring), anti-oxidant, anti-thermal shock, the high requirement of work reliability.
At present, use and study more high temperature spring comprise the refractory metal spring, with Si
3N
4Ceramics springs and C/C matrix material spring for matrix.Refractory metal spring maximum operation (service) temperature is 900 ℃, and costs an arm and a leg.But like 600 ℃ of the high temperature resistant spring heatproofs of Inconel X750 of U.S. exploitation, the Nimoni90 heatproof also is merely 700 ℃, and when use temperature surpassed 1000 ℃, the metallic substance antioxidant property was poor, has high temperature creep and stress relaxation, can't satisfy application requiring.NHK Spring Co. Ltd (NHK) has developed PSZ, Si
3N
4Be the ceramics springs goods of matrix, maximum operation (service) temperature reaches 800 ℃ and 1200 ℃ respectively.Domestic Nanjing University of Technology has also carried out the partially stabilized ZrO of nano modification
2(PSZ) preparation of ceramics springs, but the stupalith hardness of ceramics springs is big, the processing and preparing difficulty, work reliability is low.The C/C matrix material spring of Japan Ah Cross Co. exploitation has lightweight, HS, high-modulus and good spring characteristic, but the C/C matrix material at high temperature antioxidant property significantly descend, limited its use in oxidizing atmosphere.
To the active demand of thermal protection system elevated-temperature seal, need a kind of better high temperature spring of exploitation, so that be that the elevated-temperature seal technical barrier that solves space industry provides technical support to high temperature resistant spring.
Summary of the invention
The technical problem that the present invention will solve is the deficiency that overcomes prior art; A kind of high temperature resistant (more than 1200 ℃), corrosion-resistant, anti-oxidant, C/SiC ceramic matric composite spring with excellent mechanical performances are provided, the also corresponding preparation method who provides that a kind of technology is simple, equipment requirements is simple, the cycle is short, cost is low, can realize the clean formed C of product/SiC ceramic matric composite spring.
For solving the problems of the technologies described above; The technical scheme that the present invention proposes is: a kind of C/SiC ceramic matric composite spring; It is characterized in that: said spring is to be matrix with silit, with volume(tric)fraction be 30%～45% thomel as wild phase, the surface deposition of said spring has the SiC coating; The rigidity of said spring reaches 3.5N/mm～8N/mm under the room temperature, and the rigidity retention rate is 70%～85% in 800 ℃～1200 ℃ air.
As a total technical conceive, the present invention also provides a kind of preparation method of C/SiC ceramic matric composite spring, may further comprise the steps:
(1) moulding of spring prefab: the thomel after will pooling capital (for example 8～30 bundle thomels are with boundling twisting or weaving manner plying) joins in the resin system and floods; Wrapping formed on paraffin mould or (being made up of polymkeric substance and ceramics powder) water-soluble mould (mould diameter is generally that 8mm～20mm), crosslinking curing obtains the spring prefab under the room temperature with the prefabricated carbon fiber spare behind the dipping;
(2) moulding of spring crude green body: utilize fusible pattern/molten modulus method; Be heated to 80 ℃～150 ℃ and make the fusion of paraffin mould, remove taking shape in spring prefab on the said paraffin mould; The spring prefab that perhaps will take shape on the said water-soluble mould (being made up of polymkeric substance and ceramics powder) places 40 ℃～70 ℃ water dissolving to remove water-soluble mould; Then the spring prefab after the demoulding is set on the graphite jig (identical with aforementioned mould diameter); And under 900 ℃～1400 ℃ temperature, make said resin system cracking, (silk footpath is generally 1mm～6mm) to obtain the spring crude green body;
(3) spring densification: above-mentioned spring crude green body is placed Polycarbosilane-YLENE system (PCS/xylene) or Polycarbosilane-Vinylstyrene system (PCS/DVB) vacuum impregnation; Cracking under 900 ℃～1400 ℃ temperature then; The a plurality of cycles of dipping-cracking technology that repeat this step make ganoid spring work in-process until accomplishing densification after the surface is cleared up;
(4) the spring surface oxidation-resistant is handled: with materials such as trichloromethyl silane (MTS) or liquid polysilanes is precursor; Adopt chemical vapor deposition method in said spring surface of semi-finished deposition SiC coating, prepare C/SiC ceramic matric composite spring finished product at last.
Among the preparation method of above-mentioned C/SiC ceramic matric composite spring; Resin system in the said step (1) is mainly used in the spring typing; It is preferably Polycarbosilane-divinyl benzole soln, epoxy resin-acetone soln or resol-ethanolic soln, also preferably contains solidifying agent in the said resin system.
The preparation method of above-mentioned C/SiC ceramic matric composite spring, the mass ratio of Polycarbosilane, Vinylstyrene, solidifying agent is preferably 1 in said Polycarbosilane-divinyl benzole soln: (0.5～2): (0.01～0.05); The mass ratio of epoxy resin, acetone, solidifying agent is preferably 1 in said epoxy resin-acetone soln: (0.5～3): (0.05～0.1); The mass ratio of resol, ethanol, solidifying agent is preferably 1 in said resol-ethanolic soln: (0.5～2): (0.02～0.1).
The preparation method of above-mentioned C/SiC ceramic matric composite spring; The mass ratio of Polycarbosilane and YLENE is preferably 1 in said Polycarbosilane-YLENE system: (0.5～2), the mass ratio of Polycarbosilane and Vinylstyrene is preferably 1 in said Polycarbosilane-Vinylstyrene system: (0.5～2).
The time of crosslinking curing is preferably 1h～5h among the preparation method of above-mentioned C/SiC ceramic matric composite spring, said step (1).
Paraffin mould fused soaking time is preferably 0.5h～1h among the preparation method of above-mentioned C/SiC ceramic matric composite spring, said step (2); Dissolve the soak time of removing water-soluble mould in the said step (2) and be preferably 3h～9h.
The preparation method of above-mentioned C/SiC ceramic matric composite spring; The vacuum impregnation time is preferably 3h～10h in the said step (3); Soaking time in the said step (3) during cracking is preferably 0.5h～2h; Required cycle life during said densification is decided according to the demand of spring rate, is preferably 7～18.
The temperature of chemical vapor deposition method is preferably 950 ℃～1100 ℃ among the preparation method of above-mentioned C/SiC ceramic matric composite spring, said step (4), and depositing time is preferably 1h～6h.
Compared with prior art, the invention has the advantages that:
(1) the invention property ground with thomel as strengthening body; SiC is a matrix; Prepare C/SiC ceramic matric composite spring in conjunction with the precursor conversion process, advantage such as that this spring has is high temperature resistant, anti-oxidant, H.T., high work reliability, performance can design;
(2) according to composite structure and the programmable characteristics of mechanical property, spring of the present invention can be realized the designability of performance perameters such as recoil of spring power, draught, spring rate;
(3) the invention property ground combines fusible pattern/molten mold technique and PIP technology; Adopt fusible pattern/molten modulus method to realize the low-temperature shaped of spring; Adopt high temperature resistant graphite jig to realize Deformation control in the spring high temperature sintering process, thereby realize the clean moulding of C/SiC ceramic matric composite spring.
Generally speaking; C/SiC ceramic matric composite spring of the present invention has characteristics such as preparation temperature is low, and preparation technology and equipment requirements are simple, and the cycle is short, cost is low; The spring of preparation has the excellent comprehensive performance, is particularly suitable for high temperature resistant (> 1200 ℃), the application under the well-oxygenated environment.
Description of drawings
Fig. 1 is the picture in kind of the C/SiC ceramic matric composite spring in the embodiment of the invention 1.
Fig. 2 is the C/SiC ceramic matric composite spring spring silk fracture apperance picture in the embodiment of the invention 1.
Embodiment
Below in conjunction with Figure of description and specific embodiment the present invention is further described.
Embodiment 1:
A kind of this spring is to be matrix with silit like Fig. 1, C/SiC ceramic matric composite spring of the present invention shown in Figure 2, and as wild phase, the surface deposition of spring has the SiC coating with the thomel of volume(tric)fraction about 34%; The rigidity of this spring reaches 3.5N/mm under the room temperature, and rigidity still reaches 2.6N/mm in 1000 ℃ air, and it is 74% that the rigidity retention rate surpasses.
The C/SiC ceramic matric composite spring of present embodiment prepares through following steps:
(1) moulding of spring prefab: 14 bundle thomel boundlings are joined in the PCS/DVB resin system that contains solidifying agent after twisted and plied flood; Wherein the mass ratio of Polycarbosilane, Vinylstyrene, solidifying agent is 1: 1: 0.02; Prefabricated carbon fiber spare behind the dipping is Wrapping formed on the paraffin mould of diameter 16mm or water-soluble mould, and crosslinking curing 3h obtains the spring prefab under the room temperature;
(2) moulding of spring crude green body: utilize permanent mo(u)lding method, put into baking oven and be heated to 100 ℃ taking shape in spring prefab on the paraffin mould, insulation 0.5h makes the fusion of paraffin mould; Remove a spring prefab that obtains silk footpath 2mm behind the deparaffnize mould, the spring prefab after the demoulding is set on the graphite jig of a diameter 14mm fixes then, guarantee that to control its high-temperature process spring is indeformable; The spring prefab of band graphite jig is placed in the high-temperature cracking furnace; Be evacuated to below the 1000Pa, feed nitrogen, and in flowing nitrogen atmosphere, be rapidly heated to 1200 ℃; 10 ℃/min of temperature rise rate; Make said resin system cracking behind the insulation 1h, cooling obtains the spring crude green body naturally;
(3) spring densification: above-mentioned spring crude green body is put into the vacuum impregnation jar, be evacuated to-0.1MPa after, placing mass ratio is 1: 1 Polycarbosilane-YLENE system vacuum impregnation 5h; Crude green body after the vacuum impregnation is placed in the high-temperature cracking furnace; Be evacuated to below the 1000Pa, feed nitrogen, in flowing nitrogen atmosphere, be rapidly heated then to 1200 ℃ of temperature and carry out cracking; 10 ℃/min of temperature rise rate, cooling naturally behind the insulation 1h; 9 cycles of dipping-cracking technology that repeat this step make spring reach predetermined stiffness until accomplishing densification, remove graphite jig then, make ganoid spring work in-process after the spring surface is cleared up;
(4) the spring surface oxidation-resistant is handled: with trichloromethyl silane (MTS) is precursor; Adopt chemical vapor deposition method in the spring surface of semi-finished; In 1000Pa pressure, 1050 ℃ of condition deposit SiC coatings; Depositing time is 2h, prepares C/SiC ceramic matric composite spring finished product at last.
Embodiment 2:
A kind of C/SiC ceramic matric composite spring of the present invention, this spring is to be matrix with silit, with volume(tric)fraction about 42% thomel as wild phase, the surface deposition of spring has the SiC coating; The rigidity of this spring reaches 7.5N/mm under the room temperature, and rigidity still reaches 6.3N/mm in 1000 ℃ air, and the rigidity retention rate reaches 84%.
The C/SiC ceramic matric composite spring of present embodiment prepares through following steps:
(1) moulding of spring prefab: the original position braiding on the paraffin mould of diameter 20mm of 20 bundle thomels is Wrapping formed; Join then in the epoxy resin-acetone soln that contains solidifying agent and flood; Wherein the mass ratio of epoxy resin, acetone, solidifying agent is 1: 1.5: 0.1, with the dipping after prefabricated carbon fiber spare at room temperature crosslinking curing 5h obtain the spring prefab;
(2) moulding of spring crude green body: utilize permanent mo(u)lding method, put into baking oven and be heated to 100 ℃ taking shape in spring prefab on the paraffin mould, insulation 0.5h makes the fusion of paraffin mould; Remove a spring prefab that obtains silk footpath 4mm behind the deparaffnize mould, the spring prefab after the demoulding is set on the graphite jig of a diameter 20mm fixes then, guarantee that to control its high-temperature process spring is indeformable; The spring prefab of band graphite jig is placed in the high-temperature cracking furnace; Be evacuated to below the 1000Pa, feed nitrogen, and in flowing nitrogen atmosphere, be rapidly heated to 1200 ℃; 10 ℃/min of temperature rise rate; Make said resin system cracking behind the insulation 1h, cooling obtains the spring crude green body naturally;
(3) spring densification: above-mentioned spring crude green body is put into the vacuum impregnation jar, be evacuated to-0.1MPa after, placing mass ratio is 1: 1 PCS/DVB system vacuum impregnation 7h; Crude green body after the vacuum impregnation is placed in the high-temperature cracking furnace; Be evacuated to below the 1000Pa, feed nitrogen, in flowing nitrogen atmosphere, be rapidly heated then to 1200 ℃ of temperature and carry out cracking; 15 ℃/min of temperature rise rate, cooling naturally behind the insulation 1.5h; 11 cycles of dipping-cracking technology that repeat this step make spring reach predetermined stiffness until accomplishing densification, remove graphite jig then, make ganoid spring work in-process after the spring surface is cleared up;
(4) the spring surface oxidation-resistant is handled: with trichloromethyl silane (MTS) is precursor; Adopt chemical vapor deposition method in the spring surface of semi-finished; In 1000Pa pressure, 1050 ℃ of condition deposit SiC coatings; Depositing time is 6h, prepares C/SiC ceramic matric composite spring finished product at last.
Embodiment 3:
A kind of C/SiC ceramic matric composite spring of the present invention, this spring is to be matrix with silit, as wild phase, the surface deposition of spring has the SiC coating with the thomel of volume(tric)fraction about 37%; The rigidity of this spring reaches 5.6N/mm under the room temperature, and rigidity still reaches 4.4N/mm in 1000 ℃ air, and the rigidity retention rate has surpassed 78%.
The C/SiC ceramic matric composite spring of present embodiment prepares through following steps:
(1) moulding of spring prefab: the original position braiding on the water-soluble mould of diameter 20mm of 16 bundle thomels is Wrapping formed; Join then in the resol-ethanolic soln that contains solidifying agent and flood; Wherein the mass ratio of resol, ethanol, solidifying agent is 1: 2: 0.05, with the dipping after prefabricated carbon fiber spare at room temperature crosslinking curing 3h obtain the spring prefab;
(2) moulding of spring crude green body: utilize to dissolve modulus method, put into 60 ℃ of warm water and dissolve 5h, make the high molecular polymer dissolving in the mould with taking shape in spring prefab on the water-soluble mould; Remove a spring prefab that obtains silk footpath 3mm behind the water-soluble mould, the spring prefab after the demoulding is set on the graphite jig of a diameter 20mm fixes then, guarantee that to control its high-temperature process spring is indeformable; The spring prefab of band graphite jig is placed in the high-temperature cracking furnace; Be evacuated to below the 1000Pa, feed nitrogen, and in flowing nitrogen atmosphere, be rapidly heated to 1200 ℃; 10 ℃/min of temperature rise rate; Make said resin system cracking behind the insulation 1h, cooling obtains the spring crude green body naturally;
(3) spring densification: above-mentioned spring crude green body is put into the vacuum impregnation jar, be evacuated to-0.1MPa after, placing mass ratio is 1: 1 PCS/xylene system vacuum impregnation 5h; Crude green body after the vacuum impregnation is placed in the high-temperature cracking furnace; Be evacuated to below the 1000Pa, feed nitrogen, in flowing nitrogen atmosphere, be rapidly heated then to 1200 ℃ of temperature and carry out cracking; 10 ℃/min of temperature rise rate, cooling naturally behind the insulation 1.5h; 13 cycles of dipping-cracking technology that repeat this step make spring reach predetermined stiffness until accomplishing densification, remove graphite jig then, make ganoid spring work in-process after the spring surface is cleared up;
(4) the spring surface oxidation-resistant is handled: with trichloromethyl silane (MTS) is precursor; Adopt chemical vapor deposition method in the spring surface of semi-finished; In 1000Pa pressure, 1075 ℃ of condition deposit SiC coatings; Depositing time is 5h, prepares C/SiC ceramic matric composite spring finished product at last.
Claims (9)
1. C/SiC ceramic matric composite spring, it is characterized in that: said spring is to be matrix with silit, with volume(tric)fraction be 30%～45% thomel as wild phase, the surface deposition of said spring has the SiC coating; The rigidity of said spring reaches 3.5N/mm～8N/mm under the room temperature, and the rigidity retention rate is 70%～85% in 800 ℃～1200 ℃ air.
2. the preparation method of a C/SiC ceramic matric composite spring may further comprise the steps:
(1) moulding of spring prefab: the thomel after will pooling capital joins in the resin system and floods, and the prefabricated carbon fiber spare behind the dipping is Wrapping formed on paraffin mould or water-soluble mould, and crosslinking curing obtains the spring prefab under the room temperature;
(2) moulding of spring crude green body: will take shape in spring prefab on the said paraffin mould and be heated to 80 ℃～150 ℃ and make the fusion of paraffin mould, remove; The spring prefab that perhaps will take shape on the said water-soluble mould places 40 ℃～70 ℃ water dissolving to remove water-soluble mould; Then the spring prefab after the demoulding is set on the graphite jig; And under 900 ℃～1400 ℃ temperature, make said resin system cracking, obtain the spring crude green body;
(3) spring densification: above-mentioned spring crude green body is placed Polycarbosilane-YLENE system or Polycarbosilane-Vinylstyrene system vacuum impregnation; Cracking under 900 ℃～1400 ℃ temperature then; The a plurality of cycles of dipping-cracking technology that repeat this step make the spring work in-process until accomplishing densification;
(4) the spring surface oxidation-resistant is handled: with trichloromethyl silane or liquid polysilane is precursor, adopts chemical vapor deposition method in said spring surface of semi-finished deposition SiC coating, prepares C/SiC ceramic matric composite spring finished product at last.
3. the preparation method of C/SiC ceramic matric composite spring according to claim 2; It is characterized in that: the resin system in the said step (1) is Polycarbosilane-divinyl benzole soln, epoxy resin-acetone soln or resol-ethanolic soln, also contains solidifying agent in the said resin system.
4. the preparation method of C/SiC ceramic matric composite spring according to claim 3 is characterized in that: the mass ratio of Polycarbosilane, Vinylstyrene, solidifying agent is 1 in said Polycarbosilane-divinyl benzole soln: (0.5～2): (0.01～0.05); The mass ratio of epoxy resin, acetone, solidifying agent is 1 in said epoxy resin-acetone soln: (0.5～3): (0.05～0.1); The mass ratio of resol, ethanol, solidifying agent is 1 in said resol-ethanolic soln: (0.5～2): (0.02～0.1).
5. the preparation method of C/SiC ceramic matric composite spring according to claim 2; It is characterized in that: the mass ratio of Polycarbosilane and YLENE is 1 in said Polycarbosilane-YLENE system: (0.5～2), the mass ratio of Polycarbosilane and Vinylstyrene is 1 in said Polycarbosilane-Vinylstyrene system: (0.5～2).
6. according to the preparation method of each described C/SiC ceramic matric composite spring in the claim 2～5, it is characterized in that: the time of crosslinking curing is 1h～5h in the said step (1).
7. according to the preparation method of each described C/SiC ceramic matric composite spring in the claim 2～5, it is characterized in that: paraffin mould fused soaking time is 0.5h～1h in the said step (2); Dissolving the soak time of removing water-soluble mould in the said step (2) is 3h～9h.
8. according to the preparation method of each described C/SiC ceramic matric composite spring in the claim 2～5; It is characterized in that: the vacuum impregnation time is 3h～10h in the said step (3); Soaking time in the said step (3) during cracking is 0.5h～2h, and the required cycle life during said densification is 7～18.
9. according to the preparation method of each described C/SiC ceramic matric composite spring in the claim 2～5, it is characterized in that: the temperature of chemical vapor deposition method is 950 ℃～1100 ℃ in the said step (4), and depositing time is 1h～6h.
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| CN106090082A (en) * | 2016-06-18 | 2016-11-09 | 苏州思创源博电子科技有限公司 | A kind of preparation method of carbon carbon composite brake disc |
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| CN110937909A (en) * | 2019-11-21 | 2020-03-31 | 西北工业大学 | Preparation method of continuous fiber reinforced C/SiC ceramic spring |
| CN110937909B (en) * | 2019-11-21 | 2022-04-29 | 西北工业大学 | Preparation method of continuous fiber reinforced C/SiC ceramic spring |
| CN114196027A (en) * | 2021-12-30 | 2022-03-18 | 江西信达航科新材料科技有限公司 | High-strength silicon carbide fiber precursor modified polycarbosilane and preparation method thereof |
| CN114180981A (en) * | 2022-01-05 | 2022-03-15 | 湖南远辉复合材料有限公司 | Preparation method of precursor conversion ceramic matrix composite component |
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