CN102807369A - Method for preparing continuous silicon carbide fiber - Google Patents
Method for preparing continuous silicon carbide fiber Download PDFInfo
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- CN102807369A CN102807369A CN2012103060240A CN201210306024A CN102807369A CN 102807369 A CN102807369 A CN 102807369A CN 2012103060240 A CN2012103060240 A CN 2012103060240A CN 201210306024 A CN201210306024 A CN 201210306024A CN 102807369 A CN102807369 A CN 102807369A
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- polycarbosilane
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Abstract
The invention relates to a method for preparing a continuous silicon carbide fiber. The preparation method comprises the following steps of: first, adding a certain amount of additive in polycarbosilane through a physical blending way, obtaining a proto filament through melt spinning, and then, radiating and crosslinking by an electronic beam under inert gas, and finally, cracking under the inert gas to obtain the SiC fiber. By using the method, annular siloxane containing vinyl and silazane are added in the polycarbosilane through the physical blending way, and as the bond energy of a p electron on the vinyl is 2.4*10<5> J/mol, but the bond energy of a Si-H bond in the polycarbosilane is 3.9*10<5> J/mol, due to the difference, the crosslinking efficiency of a precursor into which the additive is not added is less than the crosslinking efficiency of a precursor into which the additive is added by several times in an infusible treatment process, so that the purposes of decreasing the difficulty of infusible treatment, reducing energy consumption and improving efficiency are achieved. The method has the advantages that the process is simple, the operation is easy, the cost is relatively lower, and the silicon carbide fiber can be bent and processed.
Description
Technical field
The present invention relates to a kind of method for preparing continuous carbofrax fibre.
Background technology
Silit (SiC) fiber is compared with oxide fibre with thomel as a kind of new ceramics fiber, in high temperature resistant, anti-oxidant, creep resistance, tensile strength and the performance that aspect the ceramic matrix excellent compatibility, all shows a series of excellences.Ceramic matric composite (SiC-CMC) Heat stability is good that continuous SiC fiber is toughness reinforcing; Thermal shock resistance is strong; Be with a wide range of applications in some high-tech sectors such as space flight, aviation, weapons, boats and ships and nuclear industry, in the thermal protection structure material system (TPS) of Aeronautics and Astronautics mover heat-resistant part, reusable vehicle (RLV) and hypersonic speed transportation propulsion system, all adopted the SiC fiber in a large number in the required refractory ceramics based composites like states such as U.S.A, day, methods.Therefore the SiC fiber is one of crucial strategic material of development advanced technological arms and Aeronautics and Astronautics cause.
SiC fiber production method mainly contains powder sintering (US Patent4908340; 1990), chemical vapor deposition (CVD) method (US Patent3433725), precursor conversion method (Chemical Letters; 1975:931), chemical gas-phase reaction method (CVR) (JP Patent58/91823,1983).Stainless Steel via Precursor Pyrolysis SiC fiber is as far back as 1975, and the Yajima of metallic substance institute of northeastern Japan university professor's research group starts, and has used for reference the preparation experience of thomel, has invented Stainless Steel via Precursor Pyrolysis SiC fiber.(Polycarbosllane PCS) is precursor, has successfully made thin footpath continuous SiC fiber through melt-spinning, non-melt processed, high temperature firing process to utilize Polycarbosilane.Since then, the precursor conversion method becomes the main flow direction of SiC fiber research and exploitation gradually, also is the industrialized preparing process of comparative maturity at present.Yet be that the fiber of extensive stockization and the continuous SiC fiber of development all exist the problem on cost and the use characteristics, effectively reducing cost and guaranteeing or improve use characteristics all is the current subject matter of studying.The research direction of current continuous SiC fiber mainly concentrates on some: 1) seek and the precursor of synthesizing new, remedy the deficiency of current general precursor Polycarbosilane spinning properties, reduce the not difficulty of melt processed; 2) adopt radiation crosslinking or unsaturated atmosphere crosslinking to improve the precursor crosslinking method, reduce oxygen level; 3) mixing different element high temperature sintering removes impurity and prepares high-purity polycrystalline Si C fiber; 4) physical blending modification.The physical blending modification is a kind of cost-effective approach that obtains the macromolecular material of excellent combination property, and two kinds or two or more polymkeric substance mix through the method for physics and form macroscopic view and go up even, successive solid macromolecule material.For PCS, the first three mode is researched and developed with preparation cost higher, and then relative cost is lower through the physical blending modification, and operability is higher, more helps accelerating the development progress of SiC fiber industry.
Summary of the invention
In order to reduce the difficulty that existing precursor legal system is equipped with the SiC fibre technology, the purpose of this invention is to provide simple, the feasible method that can improve existing preparation technology of a kind of preparation method.
Technical scheme of the present invention is at first through the mode of physical blending, in Polycarbosilane, adds certain quantity of additive, obtains precursor through melt-spinning, crosslinking electron beam irradiation under rare gas element again, and cracking obtains the SiC fiber under rare gas element at last.
The method for preparing continuous carbofrax fibre of the present invention may further comprise the steps:
(1) Polycarbosilane, additive place Banbury mixer in the certain mass ratio, behind 190-260 ℃ of banburying 5-30min, take out;
Described additive is trimethylammonium trivinyl cyclotrisiloxane (D
3 V), tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 V), pentamethyl-five vinyl D5 (D
5 V), trimethylammonium triethylene basic ring three silazane (D
3 NV) in a kind of or wherein any several kinds mixture;
The mass ratio of described Polycarbosilane and additive is 1: 0.01～0.6;
(2) presoma after the banburying is placed melt spinning device; In purity be heated under 99.999% the nitrogen protection 220-280 ℃ carry out deaeration and handle after, at 200-260 ℃, 0.2-1.2MPa; Carry out melt-spinning with 40-200m/min speed, make the precursor that diameter is 10-20 μ m;
(3) precursor with step (2) gained places the electronics booster machinery, under the flowing nitrogen protection, carries out cross-linking radiation and makes fusion-free fibre;
Described cross-linking radiation condition is: during the following dosage of 2MGy, dose rate maintains 0.3-0.5kGy/s, and dose rate is increased to 0.7-0.9kGy/s afterwards, is 3-12MGy until total dose;
(4) it is the High Temperature Furnaces Heating Apparatus of 99.999% nitrogen protection that the fusion-free fibre that step (3) is made places purity, is warming up to 900-1600 ℃ with the heat-up rate of 10-20 ℃/min, and the insulation 0.5-3h that under this temperature, lives, and promptly makes silicon carbide fiber.
The present invention compared with prior art has the following advantages:
The physical blending modification is to obtain a kind of economy of the macromolecular material of excellent combination property and valid approach.Polycarbosilane is carried out the important directions that the physical blending modification will be the development of SiC fiber.Melt processed is not one of technology that difficulty is the highest in the SiC fiber production process, is one of maximum link of energy consumption yet, and its quality has a strong impact on the performance of last fiber.Annular siloxanes, silazane that the present invention will contain vinyl join in the Polycarbosilane through the mode of physical blending.Because the bond energy of p electronics is 2.4 * 10 on the vinyl
5J/mol, and Si-H key bond energy is 3.9 * 10 in the Polycarbosilane
5J/mol, this difference is enough to make and does not add additive and two kinds of presomas that the add additive cross-linking efficiency when melt processed not and improve several times.This easy method can be implemented in than carrying out crosslinking reaction under the mild conditions, and its result can effectively overcome high radiating capacity in this link, reduces production costs, and prepared SiC fibre property is stable, can bending machining.
Embodiment
Embodiment 1
10g Polycarbosilane, 0.5g tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 V) place Banbury mixer; Behind 220 ℃ of banburying 10min, take out, the presoma after the banburying placed melt spinning device, in purity be heated under 99.999% the nitrogen protection 260 ℃ carry out deaeration and handle after; At 240 ℃; 0.5MPa down, carry out melt-spinning, make the protofibril that diameter is 15 μ m with 100m/min speed; The precursor of gained places the electronics booster machinery, under the flowing nitrogen protection, carries out cross-linking radiation.During the following dosage of 2MGy, dose rate maintains 0.4kGy/s, and dose rate is increased to 0.8kGy/s afterwards, is 4MGy until total dose.It is the High Temperature Furnaces Heating Apparatus of 99.999% nitrogen protection that the fiber of crossing through melt processed not places purity, is warming up to 1300 ℃ with the heat-up rate of 15 ℃/min, and under this temperature, is incubated 3h, promptly makes continuous carbofrax fibre.
Embodiment 2
10g Polycarbosilane, 3g tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 V) place Banbury mixer; Behind 220 ℃ of banburying 10min, take out, the presoma after the banburying placed melt spinning device, in purity be heated under 99.999% the nitrogen protection 260 ℃ carry out deaeration and handle after; At 240 ℃; 0.5MPa down, carry out melt-spinning, make the protofibril that diameter is 15 μ m with 100m/min speed; The precursor of gained places the electronics booster machinery, under the flowing nitrogen protection, carries out cross-linking radiation.During the following dosage of 2MGy, dose rate maintains 0.4kGy/s, and dose rate is increased to 0.8kGy/s afterwards, is 4MGy until total dose.It is the High Temperature Furnaces Heating Apparatus of 99.999% nitrogen protection that the fiber of crossing through melt processed not places purity, is warming up to 1300 ℃ with the heat-up rate of 15 ℃/min, and under this temperature, is incubated 3h, promptly makes continuous carbofrax fibre.
Embodiment 3
10g Polycarbosilane, 0.5g tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 V) place Banbury mixer; Behind 220 ℃ of banburying 10min, take out, the presoma after the banburying placed melt spinning device, in purity be heated under 99.999% the nitrogen protection 260 ℃ carry out deaeration and handle after; At 240 ℃; 0.5MPa down, carry out melt-spinning, make the protofibril that diameter is 15 μ m with 100m/min speed; The precursor of gained places the electronics booster machinery, under the flowing nitrogen protection, carries out cross-linking radiation.During the following dosage of 2MGy, dose rate maintains 0.4kGy/s, and dose rate is increased to 0.8kGy/s afterwards, is 8MGy until total dose.It is the High Temperature Furnaces Heating Apparatus of 99.999% nitrogen protection that the fiber of crossing through melt processed not places purity, is warming up to 1300 ℃ with the heat-up rate of 15 ℃/min, and under this temperature, is incubated 3h, promptly makes continuous carbofrax fibre.
Embodiment 4
10g Polycarbosilane, 0.5g trimethylammonium trivinyl cyclotrisiloxane (D
3 V) place Banbury mixer; Behind 220 ℃ of banburying 10min, take out, the presoma after the banburying placed melt spinning device, in purity be heated under 99.999% the nitrogen protection 260 ℃ carry out deaeration and handle after; At 240 ℃; 0.5MPa down, carry out melt-spinning, make the protofibril that diameter is 15 μ m with 100m/min speed; The precursor of gained places the electronics booster machinery, under the flowing nitrogen protection, carries out cross-linking radiation.During the following dosage of 2MGy, dose rate maintains 0.4kGy/s, and dose rate is increased to 0.8kGy/s afterwards, is 4MGy until total dose.It is the High Temperature Furnaces Heating Apparatus of 99.999% nitrogen protection that the fiber of crossing through melt processed not places purity, is warming up to 1300 ℃ with the heat-up rate of 15 ℃/min, and under this temperature, is incubated 3h, promptly makes continuous carbofrax fibre.
Embodiment 5
10g Polycarbosilane, 0.5g pentamethyl-five vinyl D5 (D
5 V) place Banbury mixer; Behind 220 ℃ of banburying 10min, take out, the presoma after the banburying placed melt spinning device, in purity be heated under 99.999% the nitrogen protection 260 ℃ carry out deaeration and handle after; At 240 ℃; 0.5MPa down, carry out melt-spinning, make the protofibril that diameter is 15 μ m with 100m/min speed; The precursor of gained places the electronics booster machinery, under the flowing nitrogen protection, carries out cross-linking radiation.During the following dosage of 2MGy, dose rate maintains 0.4kGy/s, and dose rate is increased to 0.8kGy/s afterwards, is 4MGy until total dose.It is the High Temperature Furnaces Heating Apparatus of 99.999% nitrogen protection that the fiber of crossing through melt processed not places purity, is warming up to 1300 ℃ with the heat-up rate of 15 ℃/min, and under this temperature, is incubated 3h, promptly makes continuous carbofrax fibre.
Embodiment 6
10g Polycarbosilane, 0.5g trimethylammonium triethylene basic ring three silazane (D
3 NV) place Banbury mixer; Behind 220 ℃ of banburying 10min, take out, the presoma after the banburying placed melt spinning device, in purity be heated under 99.999% the nitrogen protection 260 ℃ carry out deaeration and handle after; At 240 ℃; 0.5MPa down, carry out melt-spinning, make the protofibril that diameter is 15 μ m with 100m/min speed; The precursor of gained places the electronics booster machinery, under the flowing nitrogen protection, carries out cross-linking radiation.During the following dosage of 2MGy, dose rate maintains 0.4kGy/s, and dose rate is increased to 0.8kGy/s afterwards, is 4MGy until total dose.It is the High Temperature Furnaces Heating Apparatus of 99.999% nitrogen protection that the fiber of crossing through melt processed not places purity, is warming up to 1300 ℃ with the heat-up rate of 15 ℃/min, and under this temperature, is incubated 3h, promptly makes continuous carbofrax fibre.
Embodiment 7
10g Polycarbosilane, 0.5g trimethylammonium triethylene basic ring three silazane (D
3 NV) and tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 V) mixture (mass ratio is 3: 1) place Banbury mixer; Behind 220 ℃ of banburying 10min, take out, the presoma after the banburying placed melt spinning device, in purity be heated under 99.999% the nitrogen protection 260 ℃ carry out deaeration and handle after; At 240 ℃; 0.5MPa down, carry out melt-spinning, make the protofibril that diameter is 15 μ m with 100m/min speed; The precursor of gained places the electronics booster machinery, under the flowing nitrogen protection, carries out cross-linking radiation.During the following dosage of 2MGy, dose rate maintains 0.4kGy/s, and dose rate is increased to 0.8kGy/s afterwards, is 4MGy until total dose.It is the High Temperature Furnaces Heating Apparatus of 99.999% nitrogen protection that the fiber of crossing through melt processed not places purity, is warming up to 1300 ℃ with the heat-up rate of 15 ℃/min, and under this temperature, is incubated 3h, promptly makes continuous carbofrax fibre.
Claims (3)
1. a method for preparing continuous carbofrax fibre is characterized in that, this method may further comprise the steps:
(1) Polycarbosilane, additive place Banbury mixer in the certain mass ratio, behind 190-260 ℃ of banburying 5-30min, take out;
The mass ratio of described Polycarbosilane and additive is 1: 0.01～0.6;
(2) presoma after the banburying is placed melt spinning device; In purity be heated under 99.999% the nitrogen protection 220-280 ℃ carry out deaeration and handle after, at 200-260 ℃, 0.2-1.2MPa; Carry out melt-spinning with 40-200m/min speed, make the precursor that diameter is 10-20 μ m;
(3) precursor with step (2) gained places the electronics booster machinery, under the flowing nitrogen protection, carries out cross-linking radiation and makes fusion-free fibre;
(4) it is the High Temperature Furnaces Heating Apparatus of 99.999% nitrogen protection that the fusion-free fibre that step (3) is made places purity, is warming up to 900-1600 ℃ with the heat-up rate of 10-20 ℃/min, and the insulation 0.5-3h that under this temperature, lives, and promptly makes silicon carbide fiber.
2. method according to claim 1 is characterized in that, the additive described in the step (1) is trimethylammonium trivinyl cyclotrisiloxane (D
3 V), tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4 V), pentamethyl-five vinyl D5 (D
5 V), trimethylammonium triethylene basic ring three silazane (D
3 NV) in a kind of or wherein any several kinds mixture.
3. method according to claim 1 is characterized in that, the cross-linking radiation condition described in the step (3) is: during the following dosage of 2MGy, dose rate maintains 0.3-0.5kGy/s, and dose rate is increased to 0.7-0.9kGy/s afterwards, is 3-12MGy until total dose.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105671688A (en) * | 2016-01-22 | 2016-06-15 | 中国人民解放军国防科学技术大学 | Method for preparing ultrahigh-temperature ceramic fibers by means of physically blending polycarbosilane and metal oxide |
| CN106116626A (en) * | 2016-06-27 | 2016-11-16 | 朗铂新材料科技（上海）有限公司 | A kind of preparation method of oxidation resistant carbon carbon composite heat-insulated material |
| CN106810262A (en) * | 2017-01-25 | 2017-06-09 | 厦门大学 | A kind of preparation method of continuous carbon SiClx ceramic fibre thermistor |
| CN106948031A (en) * | 2017-05-04 | 2017-07-14 | 中国人民解放军国防科学技术大学 | The preparation method of ultra-fine tow silicon carbide fibre |
| CN106987924A (en) * | 2017-05-15 | 2017-07-28 | 中国人民解放军国防科学技术大学 | The preparation method of Polycarbosilane fusion-free fibre |
| CN108085787A (en) * | 2018-01-03 | 2018-05-29 | 江西嘉捷信达新材料科技有限公司 | The preparation method of the silicon carbide fibre of hollow form containing basalt |
| CN108193322A (en) * | 2017-12-25 | 2018-06-22 | 晋江瑞碧科技有限公司 | A kind of preparation method of SiC nano fiber |
| CN110921670A (en) * | 2018-09-19 | 2020-03-27 | 比亚迪股份有限公司 | Silicon carbide and preparation method thereof |
| CN115787141A (en) * | 2021-09-10 | 2023-03-14 | 苏州赛力菲陶纤有限公司 | Method for improving temperature resistance of continuous silicon carbide fiber |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105671688A (en) * | 2016-01-22 | 2016-06-15 | 中国人民解放军国防科学技术大学 | Method for preparing ultrahigh-temperature ceramic fibers by means of physically blending polycarbosilane and metal oxide |
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| CN106810262A (en) * | 2017-01-25 | 2017-06-09 | 厦门大学 | A kind of preparation method of continuous carbon SiClx ceramic fibre thermistor |
| CN106948031A (en) * | 2017-05-04 | 2017-07-14 | 中国人民解放军国防科学技术大学 | The preparation method of ultra-fine tow silicon carbide fibre |
| CN106987924A (en) * | 2017-05-15 | 2017-07-28 | 中国人民解放军国防科学技术大学 | The preparation method of Polycarbosilane fusion-free fibre |
| CN108193322A (en) * | 2017-12-25 | 2018-06-22 | 晋江瑞碧科技有限公司 | A kind of preparation method of SiC nano fiber |
| CN108085787A (en) * | 2018-01-03 | 2018-05-29 | 江西嘉捷信达新材料科技有限公司 | The preparation method of the silicon carbide fibre of hollow form containing basalt |
| CN110921670A (en) * | 2018-09-19 | 2020-03-27 | 比亚迪股份有限公司 | Silicon carbide and preparation method thereof |
| CN115787141A (en) * | 2021-09-10 | 2023-03-14 | 苏州赛力菲陶纤有限公司 | Method for improving temperature resistance of continuous silicon carbide fiber |
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Application publication date: 20121205 |