CN102912476A - Preparation method of carbonized silicon (SiC) sub-micron fibers - Google Patents
Preparation method of carbonized silicon (SiC) sub-micron fibers Download PDFInfo
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Abstract
The invention relates to a preparation method of SiC sub-micron fibers. The method includes the steps that a precursor polymer is mixed with a fiber-forming polymer according to a mass ratio of (5:20)-(20:5) and dissolved in a solvent to produce an even and stable spinning solution; the spinning solution is supplied to a spinneret at a rate of 5-30mL/h for each spinneret orifice and extruded through the spinneret orifice to form solution trickles, and simultaneously, the spinning solution trickles are drafted and refined by high-speed injection airflow with an injection pressure of 0.1-1.5MPa to form precursor fibers with diameters of 50nm-10mum; the precursor fibers are subjected to oxidation treatment under an atmospheric condition of 160-250DEG C to obtain infusible fibers; and the infusible fibers are subjected to high-temperature calcinations under an inert gas atmosphere of 1000-1600DEG C to obtain the SiC sub-micron fibers with diameters of 10nm-5mum. The preparation method has the advantages of being high in production efficiency, simple in process, even in fiber diameter distribution, suitable for scale production and the like.
Description
Technical field
The present invention relates to a kind of preparation method of silicon carbide fibre, especially a kind of preparation method of carborundum sub-micron fibers.
Background technology
Carborundum (SiC) has antioxygenic property, decay resistance, mechanical property, the heat conductivility of high rigidity, excellence, and the advantages such as height resistance to wears, low thermal coefficient of expansion, low-friction coefficient.In addition, carborundum or a kind of semiconductor material with wide forbidden band, have the characteristics such as broad-band gap, high disruptive critical voltage, high heat conductance, high carrier mobility, be with a wide range of applications at high frequency, high-power, high temperature resistant, radiation-resistant semiconductor devices and the aspects such as ultraviolet detector and short-wave LED.Silicon carbide fibre is as a kind of new ceramics fiber, compare with oxide fibre with carbon fiber, in tensile strength, creep-resistant property, high temperature resistant, non-oxidizability and the performance that shows a series of excellences aspect the ceramic matrix excellent compatibility, it is with a wide range of applications in high-tech sectors such as military affairs, Aeronautics and Astronautics, automobile, electronics and nuclear industry.
The topmost method of preparation silicon carbide fibre is the precursor conversion method at present, Seishi Yajima such as Japanese Tohoku university adopts the precursor conversion method take dichlorodimethylsilane as raw material, the precursor of elder generation's synthesizing silicon carbide, then carry out 2 hours heat treatment under 1000 ℃ vacuum condition, having obtained TENSILE STRENGTH is 350Kg/mm
2, diameter is 10-20 μ m, and the silicon carbide fibre of beta crystal (Chem.Lett.[J], 1975,931-934).The silicon carbide fibre diameter of the method preparation is thick, process is comparatively loaded down with trivial details, cost is higher.The Peng Shanyong of China's national defense University of Science and Technology etc. are pressed into by height and have obtained the Polycarbosilane of mean molecule quantity in 4000～12000 scopes, adopt High Molecular Weight Polycarbosilane (HM-PCS) dry spinning method, prepared that oxygen content is lower, resistance to elevated temperatures silicon carbide fibre preferably, have low oxygen content and higher resistance to elevated temperatures (Peng Shanyong, the standby low oxygen content silicon carbide fibre of dry spinning legal system, the National University of Defense technology, 2005), the SiC fibre diameter that the method obtains is thicker, and its diameter is between the 15-50 micron.For reducing fibre diameter; numerous research teams have carried out the research that utilizes electrospinning process to prepare the carborundum sub-micron fibers: the Ping Lu of Univ California-Davis USA etc. mixes preceramic polymer polyureas silane respectively with polymethyl methacrylate, polystyrene; prepare nascent composite fibre by electrostatic spinning; again under argon shield through 1560 ℃ high-temperature calcination; prepared the SiC nano fiber that comes in every shape; the diameter of fiber be about 100nm (J.Mater.Chem.[J] 2011,21:1005-1012).The Harvey A.Liu of U.S. Texas university etc. use coaxial electrostatic spinning technology; take polystyrene solution as cortex; Polycarbosilane solution is sandwich layer; prepare polystyrene/Polycarbosilane composite fibre; again with this fiber under argon shield through 1600-1650 ℃ high-temperature heat treatment 6 hours; obtained diameter and be 1-2nm the beta-type silicon carbide nanofiber (Mater.Lett.[J] 2009,63:2361-2364).The people such as Yang Daxiang utilize the xylene solution of Polycarbosilane to carry out electrostatic spinning, obtained ganoid carborundum sub-micron fibers (Chinese Surface Engineering [J], 2010,23:39-44).Although utilize electrostatic spinning technique can obtain the less nanofiber of diameter, there are the shortcomings such as fiber yield is low, fibre diameter is inhomogeneous in the party's rule at present.
Summary of the invention
For the deficiencies in the prior art; the technical problem that quasi-solution of the present invention is determined is; provide a kind of solution jet spinning method of utilizing to prepare carborundum precursor fiber; again through the method that makes the carborundum sub-micron fibers is not processed in melt processed, high-temperature calcination; this preparation method has the advantages such as production efficiency is high, technique is simple, distribution of fiber diameters is even, is suitable for large-scale production.
A kind of preparation method of carborundum sub-micron fibers, this preparation method may further comprise the steps:
(1) preparation of spinning solution: preceramic polymer and fiber-forming polymer were mixed in 5: 20 in mass ratio～20: 5, it is dissolved in the solvent, make uniform and stable spinning solution;
The concentration mass fraction of described spinning solution is 5～20%;
Described preceramic polymer is one or both and the above mixture in polyureas silane, Polycarbosilane, poly-carbon methyl-monosilane, polysilazane and the polymethyl silicane;
Described fibre-forming polymer is one or both and the above mixture in polystyrene, polystyrene copolymer, polymethyl methacrylate, PMA, acrylate copolymer and the PLA;
Described spinning solution is prepared one or both and the above mixture that employed solvent is dimethylbenzene, toluene, oxolane, cyclohexane, carbon tetrachloride, chloroform, acetonitrile, acetone;
(2) solution jet spinning method prepares the precursor fiber: spinning solution is fed to a spray silk die head with the speed of 5-30mL/h/ spinneret orifice, spinning solution is extruded from spinneret orifice, form the solution thread, simultaneously utilization at least one expulsion pressure is the described spinning solution thread of high velocity jet air drawing refinement of 0.1～1.5MPa, makes it to form the precursor fiber of diameter 50nm～10 μ m;
Described solution jet spinning method is to utilize high velocity air that spinning solution is extruded thread to carry out ultra-fine stretching and promote solvent evaporates and obtain the spinning process of ultra-fine even nanofiber, the processing step of this spinning process is " a kind of preparation method of polymeric nano-micro fiber non-woven fabric " who announces among the Chinese invention patent ZL201110041792.3, the basic principle of the method is to utilize high velocity air that solution is extruded thread to jet, impel the division of solution thread to produce jet, in the volatilization of fluidic operation Solvent, be solidified into fiber.
(3) melt processed not: described precursor fiber speed according to 5～30 ℃/min in air atmosphere is warming up to 160～250 ℃, and under this temperature insulation oxidation processes 0.5～8 hour, obtain fusion-free fibre behind the cool to room temperature;
(4) high-temperature calcination is processed: described fusion-free fibre in nitrogen atmosphere, be warming up to 1000～1600 ℃ with the speed of 0.5～50 ℃/min, and insulation was processed 0.5～5.0 hour under this temperature, obtained the carborundum sub-micron fibers.
Described carborundum sub-micron fibers diameter is 10nm～5 μ m, and representative value is 100nm～1 μ m.
The precursor fiber that the present invention prepares the carborundum sub-micron fibers is the method acquisition of carrying out jet spinning by preceramic polymer and fibre-forming polymer under action of high-speed airflow, and the fiber that makes is the nonwoven fabric form.The carborundum sub-micron fibers of the present invention's preparation is to carry out not melt processed, high-temperature calcination by the precursor fiber that the solution jet spinning is made to process and make, traditional melt spinning, dry spinning and electrostatic spinning have been replaced, fibre diameter is submicron order, generally at 10nm～5 μ m, representative value is 100nm～1 μ m, and technical process is simple, and energy consumption is low, with short production cycle, the productive rate advantages of higher.Prepared carborundum sub-micron fibers have fibre diameter thin, be evenly distributed, crystal habit is good, thermal stability is excellent, can be widely used in the fields such as military affairs, Aeronautics and Astronautics, automobile, electronics and nuclear industry.
Description of drawings
Fig. 1 is the preparation facilities schematic diagram of the embodiment of the invention.
Among the figure: 1, spinning solution storage tank; 2, spray silk die head; 21, spinneret orifice; 22, spray silk air gap; 3, hothouse; 4, collect lace curtaining; 5, temperature controller; 6, vacuum chamber; 7, air exhauster.
Fig. 2 is the ESEM picture of the carborundum sub-micron fibers of the embodiment of the invention 1.
Fig. 3 is the XRD picture of the carborundum sub-micron fibers of the embodiment of the invention 1.
The specific embodiment
The invention will be further described below in conjunction with embodiment.
(1) preparation of spinning solution: polyureas silane and polymethyl methacrylate are mixed in mass ratio at 10: 5, it is dissolved in the oxolane, make polyureas silane/polymethyl methacrylate spinning solution; The concentration that described polyureas silane accounts for total solution is 10%;
(2) solution jet spinning method prepares the precursor fiber: spinning solution is fed to a spray silk die head with the speed of 15mL/h/ spinneret orifice, spinning solution is extruded from spinneret orifice, form the solution thread; Then utilize one high velocity jet air-flow (pressure is 0.50MPa, and temperature is 25 ℃) described spinning solution thread of drawing-off refinement, and make it to enter hothouse; The spinning solution thread forms the precursor fiber gradually under the effect of high velocity jet air-flow and hothouse; Utilize at last suction airstream that blower fan produces with described precursor fiber collecting on lace curtaining.Spray silk die head to the distance of lace curtaining is that receiving range is 100cm.
(3) melt processed not: above-mentioned as-spun fibre speed according to 2 ℃/min in air atmosphere is heated up, and 190 ℃ of insulations 2 hours, obtain fusion-free fibre behind the cool to room temperature.
(4) high-temperature calcination is processed: above-mentioned fusion-free fibre under inert gas shielding, from room temperature, is warming up to 1100 ℃ with the speed of 0.5 ℃/min, and insulation 1.5 hours under this temperature, obtain the carborundum sub-micron fibers.
The ESEM picture of the carborundum sub-micron fibers that obtains as shown in Figure 2, fiber is disorganized form and distributes, pattern is smooth, average diameter is about 550nm.
X-ray diffraction (XRD) result of the carborundum sub-micron fibers that obtains as shown in Figure 3, as can be seen from the figure sample in 2 θ=35.7 °, 60.1 °, 70.9 ° diffraction maximum appears, correspond respectively to (111), (220) and (311) diffraction of silicon B-carbide, product is silicon carbide fibre.
(1) preparation of spinning solution: will gather carbon methyl-monosilane and PLA/polystyrene (mass ratio 1: 1) and mix at 10: 10 in mass ratio, it is dissolved in toluene and the oxolane mixed solvent, the solvent volume ratio is 1: 1, makes spinning solution; The concentration that described poly-carbon methyl-monosilane accounts for total solution is 20%;
(2) solution jet spinning method prepares the precursor fiber: spinning solution is fed to spinning head with the speed of 20mL/h/ spinneret orifice, spinning solution is extruded from spinning head, form the solution thread; Then utilize one high velocity jet air-flow (pressure is 1.0MPa, and temperature is 45 ℃) described spinning solution thread of drawing-off refinement, and make it to enter hothouse; The spinning solution thread forms as-spun fibre gradually under the effect of high velocity jet air-flow and spinning manifold; The suction airstream of utilizing at last blower fan to produce is collected in described as-spun fibre on the lace curtaining.Spinning head to the distance of lace curtaining is that receiving range is 150cm.
(3) melt processed not: above-mentioned as-spun fibre speed according to 4 ℃/min in air atmosphere is heated up, and 185 ℃ of insulations 3 hours, obtain fusion-free fibre behind the cool to room temperature.
(4) high-temperature calcination is processed: above-mentioned fusion-free fibre under inert gas shielding, from room temperature, is warming up to 1600 ℃ with the speed of 0.8 ℃/min, and insulation 1 hour under this temperature, obtaining average diameter is 420nm carborundum sub-micron fibers.
(1) preparation of spinning solution: will gather carbon methyl-monosilane/polyureas silane (mass ratio is 1: 1) and polystyrene and mix at 10: 10 in mass ratio, it is dissolved in toluene and the oxolane mixed solvent, the solvent volume ratio is 3: 1, makes spinning solution; The concentration that described poly-carbon methyl-monosilane/polyureas silane accounts for total solution is 30%;
(2) solution jet spinning method prepares the precursor fiber: spinning solution is fed to a spray silk die head with the speed of 5mL/h/ spinneret orifice, and jet-impingement pressure is 0.60MPa, and the jet-stream wind temperature is 60 ℃, and the lace curtaining receiving range is 200cm.
(3) melt processed not: above-mentioned as-spun fibre speed according to 3 ℃/min in air atmosphere is heated up, and 200 ℃ of insulations 1 hour, obtain fusion-free fibre behind the cool to room temperature.
(4) high-temperature calcination is processed: above-mentioned fusion-free fibre under inert gas shielding, from room temperature, is warming up to 1200 ℃ with the speed of 2.0 ℃/min, and insulation 2 hours under this temperature, obtaining average diameter is 480nm carborundum sub-micron fibers.
Embodiment 4.
(1) preparation of spinning solution: Polycarbosilane and polystyrene are mixed in mass ratio at 5: 10, it is dissolved in the dimethylbenzene, make Polycarbosilane/polystyrene spinning solution; The concentration that described Polycarbosilane accounts for total solution is 5%;
(2) solution jet spinning method prepares the precursor fiber: spinning solution is fed to a spray silk die head with the speed of 10mL/h/ spinneret orifice, and jet-impingement pressure is 0.40MPa, and the jet-stream wind temperature is 50 ℃, and the lace curtaining receiving range is 50cm.
(3) melt processed not: above-mentioned as-spun fibre speed according to 1 ℃/min in air atmosphere is heated up, and 180 ℃ of insulations 4 hours, obtain fusion-free fibre behind the cool to room temperature.
(4) high-temperature calcination is processed: above-mentioned fusion-free fibre under inert gas shielding, from room temperature, is warming up to 1000 ℃ with the speed of 1 ℃/min, and insulation 5 hours under this temperature, obtaining average diameter is the carborundum sub-micron fibers of 580nm.
Claims (7)
1. the preparation method of a carborundum sub-micron fibers is characterized in that, may further comprise the steps:
(1) preparation of spinning solution: preceramic polymer and fiber-forming polymer were mixed in 5: 20 in mass ratio～20: 5, it is dissolved in the solvent, make uniform and stable spinning solution;
(2) solution jet spinning method prepares the precursor fiber: spinning solution is fed to a spray silk die head with the speed of 5-30mL/h/ spinneret orifice, spinning solution is extruded from spinneret orifice, form the solution thread, simultaneously utilization at least one expulsion pressure is the described spinning solution thread of high velocity jet air drawing refinement of 0.1～1.5MPa, makes it to form the precursor fiber of diameter 50nm～10 μ m;
(3) melt processed not: described precursor fiber speed according to 5～30 ℃/min in air atmosphere is warming up to 160～250 ℃, and under this temperature insulation oxidation processes 0.5～8 hour, obtain fusion-free fibre behind the cool to room temperature;
(4) high-temperature calcination is processed: described fusion-free fibre in nitrogen atmosphere, be warming up to 1000～1600 ℃ with the speed of 0.5～50 ℃/min, and insulation was processed 0.5～5.0 hour under this temperature, obtained the carborundum sub-micron fibers.
2. the preparation method of carborundum sub-micron fibers according to claim 1, it is characterized in that, described preceramic polymer is one or both and the above mixture in polyureas silane, Polycarbosilane, poly-carbon methyl-monosilane, polysilazane and the polymethyl silicane.
3. the preparation method of carborundum sub-micron fibers according to claim 1, it is characterized in that, described fibre-forming polymer is one or both and the above mixture in polystyrene, polystyrene copolymer, polymethyl methacrylate, PMA, acrylate copolymer and the PLA.
4. the preparation method of carborundum sub-micron fibers according to claim 1 is characterized in that, described solvent is one or both and the above mixture in dimethylbenzene, toluene, oxolane, cyclohexane, carbon tetrachloride, chloroform, acetonitrile, the acetone.
5. the preparation method of carborundum sub-micron fibers according to claim 1 is characterized in that, the concentration mass fraction of described spinning solution is 5～20%.
6. the preparation method of carborundum sub-micron fibers according to claim 1 is characterized in that, the temperature of described high velocity jet air-flow is 20～110 ℃.
7. the preparation method of carborundum sub-micron fibers according to claim 1 is characterized in that, the diameter of described carborundum sub-micron fibers is 10nm～5 μ m, and representative value is 100nm～1 μ m.
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Cited By (9)
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| CN105155041A (en) * | 2015-10-20 | 2015-12-16 | 中国人民解放军国防科学技术大学 | Preparation method for continuous SiC fibers capable of adjusting resistivity in large range |
| CN105256407A (en) * | 2015-11-03 | 2016-01-20 | 西北工业大学 | Core-shell structured carbon-silicon carbide composite nano-fibers based on coaxial electrostatic spinning process and preparation method thereof |
| CN105734720A (en) * | 2016-03-01 | 2016-07-06 | 江苏赛菲新材料有限公司 | Preparation method for improving strength and modulus of SiC fibers |
| CN106337211A (en) * | 2016-08-29 | 2017-01-18 | 浙江惠侬丝针织内衣有限公司 | Processing method of ceramic health-care yarn |
| CN109650895A (en) * | 2019-01-07 | 2019-04-19 | 中国人民解放军国防科技大学 | Preparation method of high-crystallinity SiC fibers |
| CN109705730A (en) * | 2018-12-28 | 2019-05-03 | 东南大学苏州医疗器械研究院 | Durable type super-amphiphobic coating and preparation method thereof |
| CN110079896A (en) * | 2019-04-17 | 2019-08-02 | 中国人民解放军国防科技大学 | Silicon carbide nanofiber bundle and preparation method thereof |
| CN112779631A (en) * | 2021-01-13 | 2021-05-11 | 清华大学 | Flexible silicon carbide fiber and preparation method thereof |
| CN114829686A (en) * | 2020-11-17 | 2022-07-29 | Aa博奇瓦尔无机材料高新技术研究股份公司 | Method for producing coreless beta silicon carbide fibers |
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| CN110079896A (en) * | 2019-04-17 | 2019-08-02 | 中国人民解放军国防科技大学 | Silicon carbide nanofiber bundle and preparation method thereof |
| CN110079896B (en) * | 2019-04-17 | 2021-04-30 | 中国人民解放军国防科技大学 | Silicon carbide nanofiber bundle and preparation method thereof |
| CN114829686A (en) * | 2020-11-17 | 2022-07-29 | Aa博奇瓦尔无机材料高新技术研究股份公司 | Method for producing coreless beta silicon carbide fibers |
| CN114829686B (en) * | 2020-11-17 | 2023-11-17 | Aa博奇瓦尔无机材料高新技术研究股份公司 | Method for producing coreless beta silicon carbide fibers |
| CN112779631A (en) * | 2021-01-13 | 2021-05-11 | 清华大学 | Flexible silicon carbide fiber and preparation method thereof |
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