CN102943319A - Method for preparing silicon carbide and precursor composite fibers - Google Patents
Method for preparing silicon carbide and precursor composite fibers Download PDFInfo
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Abstract
The invention relates to a method for preparing silicon carbide and precursor composite fibers. A silicon carbide precursor polymer is dissolved in at least one organic solvent to form uniform oil phase solution with the mass fraction of 10-70%; a water-soluble fiber-forming polymer is dissolved in water, surfactants are added, uniform water phase solution with the mass fraction of 1-50% is formed, and the quantity of the surfactants is 0.1-10% of the mass of the solution; the precursor solution and the water-soluble polymer solution are mixed according to the volume ratio of 1:10-1:1 to obtain stable oil-in-water (O/W) spinning solution; spinning precursor fibers with the spinning solution by a solution jet spinning method to obtain a precursor composite fiber with the diameter ranging from 50 nanometers to 50 micrometers; and the precursor fibers are not melted and calcined at high temperature to obtain silicon carbide fibers. The method has the advantages of high production efficiency, simple process, uniformity of fiber diameter distribution and the like, and is suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of carborundum precursor composite fibre.
Background technology
Carborundum is third generation semi-conducting material, is considered to the material of the excellence of microelectronic component of new generation and integrated circuit.It has the characteristics such as energy gap is large, operating temperature is high, thermal conductivity is high, the electronics saturation drift velocity is large, disruptive field intensity is high, intrinsic carrier concentration is low, Radiation hardness is strong, chemical stability is good, to make high temperature, high frequency, high pressure resistant, anti-irradiation, the ideal material of high-power electronic device.Silicon carbide fibre is the high-performance ceramic fiber that paid close attention to by material circle, not only density is little for it, specific strength is large, specific modulus is high, linear expansion coefficient is little, also having pyro-oxidation resistance, all have good compound phase capacitive with metal, pottery, polymer, is the desirable fortifying fibre of high-performance composite materials.Simultaneously, its conductance can be regulated at relative broad range, has wave and wave absorbtion according to the difference of creating conditions, and is up-and-coming Microwave Absorbing Materials.
The precursor conversion method is one of important method of preparation silicon carbide fibre, and it is take organic polymer as precursor, utilize its fusible characteristic moulding such as solvable after, through the high temperature thermal decomposition process, make it to change inorganic ceramic material into from organic compound.Utilizing the method to prepare in the process of silicon carbide fibre, the structure of precursor fiber and performance directly affect the performance of final silicon carbide fibre, so the preparation of precursor fiber is particularly important.Seishi Yajima of Japanese Tohoku university in 1975 etc. has synthesized first the Polycarbosilane of carborundum take dichlorodimethylsilane as raw material, and it is good then to use melt spinning method to prepare surface topography, the precursor fiber that diameter is evenly distributed; This fiber is carried out 2 hours calcination processing under 1000 ℃ vacuum condition, having obtained TENSILE STRENGTH is 350Kg/mm again
2, diameter be 10-20 μ m the silicon B-carbide fiber (Chem.Lett.[J], 1975,931-934).The increase of precursor molecular weight helps to improve the thermomechanical property of silicon carbide fibre, 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, adopting even molecular weight distribution, mean molecule quantity is that 10000 Polycarbosilane (HM-PCS) carries out dry spinning, has obtained the good and continuous polycarbosilane fiber of surface topography; Through do not melt process with high-temperature calcination after, final silicon carbide fibre oxygen content is low and resistance to elevated temperatures is splendid (Peng Shanyong, the standby low oxygen content silicon carbide fibre of dry spinning legal system, the National University of Defense technology, 2005).But the precursor fibre diameter that the method obtains is thick (15-50 μ m), directly causes the diameter of silicon carbide fibre thick, has limited the application in a lot of fields.In order to reduce the precursor fibre diameter; numerous research teams carried out the research that utilizes electrospinning process to prepare carborundum precursor nano/submicron fiber: the Ping Lu of Univ California-Davis USA etc. with preceramic polymer polyureas silane respectively with polymethyl methacrylate; polystyrene mixes; prepared the nascent composite fibre of precursor by electrostatic spinning again; its diameter is about 500nm: but this composite fibre is removed the polymer of thermal cracking through 1560 ℃ high-temperature calcination meeting under argon shield; obtained the SiC nano fiber that comes in every shape through the process of inorganicization and densification; the diameter of fiber be about 100nm (J.Mater. Chem.[J] 2011,21:1005-1012).The HarveyA.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 core-skin fibre; this fiber passes through 1600-1650 ℃ high-temperature calcination under argon shield; removed the cortex polystyrene of cleavable, obtained diameter and be 1.2nm the beta-type silicon carbide nanofiber (Mater.Lett.[J] 2009,63:2361-2364).This method can obtain the less nanofiber of diameter, but fiber yield is low and need more fibre-forming polymer to improve spinnability in the solution preparation process, there is more free carbon in fiber after can causing like this heat treatment, and this directly affects the performance of silicon carbide fibre.In order to reduce the free carbon content in the silicon carbide fibre, but the Kim of Korean Institute of Science and Technology etc. mix the fibre-forming polymer of non-polar solution, surfactant, polar solvent and a kind of high temperature thermal cracking of carborundum, prepare a kind of oil/water (O/W) emulsion, again this emulsion has been obtained the precursor composite fibre of embedding emulsion micella particle by electrostatic spinning; Finally through do not melt, high-temperature calcination processes and can obtain the monocrystalline silicon carbide nanofiber.But this method has been used the fibre-forming polymer of a small amount of high temperature thermal cracking, effectively reduces the free carbon content in the fiber.The fibre diameter that the method makes is 30nm-1 μ m, and draw ratio is greater than 10, and specific area is greater than 10m
2/ g (US Patent 20110274906A1).The major defect of the method is that the productive rate of fiber is lower.
Summary of the invention
For the deficiencies in the prior art; the technical problem that quasi-solution of the present invention is determined is; a kind of preparation method who utilizes solution jet spinning method to prepare carborundum precursor composite fibre is provided; this preparation method has the advantages such as production efficiency height, technique is simple, distribution of fiber diameters is even, is suitable for large-scale production.
A kind of preparation method of carborundum precursor composite fibre, this preparation method may further comprise the steps:
(1) preparation of oil-in-water type (O/W) spinning emulsion: a kind of carborundum preceramic polymer is dissolved at least a organic solvent, and making mass fraction is the homogeneous oil-phase solution of 10-70%; A kind of water-soluble fibre-forming polymer is dissolved in the water, adds surfactant, forming mass fraction is the homogeneous aqueous phase solution of 1-50%, and the consumption of surfactant is the 0.1-10% of solution quality; Again with described precursor solution and water-soluble polymer solution with volume ratio 1: 10-1: 1 mixes, and obtains stable oil-in-water type (O/W) spinning emulsion;
Described carborundum preceramic polymer is one or both and the above mixture in polyureas silane, Polycarbosilane, poly-carbon methyl-monosilane, polysilazane and the polymethyl silicane;
Described organic solvent is toluene, dimethylbenzene, benzene, cyclohexane, pentamethylene, chloroform, carbon tetrachloride or acetonitrile;
Described water-soluble fibre-forming polymer is one or more mixtures in polyvinyl acetate, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol oxide, polyacrylamide, poly, polyethylene glycol, the starch derivatives;
Described surfactant is linear alkylbenzene sulfonate (LAS), α alkenyl sulphonate, alkyl sulfate, polyethylene glycol oxide alkyl sulfate, sodium alkyl sulfate, alkylsurfuric acid calcium, alkyl benzene calcium sulfonate, dialkyl dimethyl ammonium salt, imidazole salts, alkyl dimethyl aniline salt, alkyl methyl ammonium bromide, fatty alcohol-polyoxyethylene ether, oxidation of alkyl Dimethyl Ammonium, fatty acid alkanol amides ester, APG, polyoxyethylene alkyl phenyl ether, alkyl betaine or alkyl sulfo betaines;
(2) solution jet spinning method prepares carborundum precursor composite fibre: the spinning emulsion is fed to a spray silk die head with the speed of 1-40mL/h/ spinneret orifice, the spinning emulsion is extruded from spinneret orifice, form spinning emulsion thread, utilize simultaneously at least one high velocity jet air-flow with spinning emulsion thread 0-30.The described spinning emulsion of jet angle drawing-off refinement thread, make it to form carborundum precursor composite fibre;
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;
The temperature of described high velocity jet air-flow is 20-140 ℃, and airflow rate is 1000-30000 times of spinning emulsion thread speed.
It is the method acquisition of carrying out jet spinning by the emulsion that preceramic polymer and fibre-forming polymer form under action of high-speed airflow that the present invention prepares carborundum precursor composite fibre, the fiber that makes is the nonwoven fabric form, fibre diameter is submicron order, generally at 100nm～50 μ m, representative value is 500nm～20 μ m, and technical process is simple, and energy consumption is low, with short production cycle, the productive rate advantages of higher.Prepared carborundum precursor composite fibre contains a small amount of fibre-forming polymer, and the silicon carbide fibre crystal habit that obtains after the process high-temperature calcination is processed 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, pressure controller; 6, vacuum chamber; 7, air exhauster.
Fig. 2 is the number picture figure of the carborundum precursor composite fibre of the embodiment of the invention 1.
Fig. 3 is the low multiple stereoscan photograph figure of the carborundum precursor composite fibre of the embodiment of the invention 1.
Fig. 4 is the high multiple stereoscan photograph figure of the carborundum precursor composite fibre of the embodiment of the invention 1.
Fig. 5 is the low multiple stereoscan photograph figure of the silicon carbide fibre of the embodiment of the invention 1.
Fig. 6 is the high multiple stereoscan photograph figure of the silicon carbide fibre of the embodiment of the invention 1.
Fig. 7 is the X-ray diffraction picture of the silicon carbide fibre of the embodiment of the invention 1.
The specific embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing.
The preparation facilities that all embodiment of the present invention use is seen Fig. 1: spinneret orifice 21 and spray silk air gap 22 are positioned on the spray silk die head 2, link to each other with spinning solution storage tank 1 by woven hose; Vacuum chamber 6 links to each other with air exhauster 7, the fiber of 3 li of hothouses is inhaled collected on the lace curtaining 4.
Embodiment 1.
(1) preparation of oil-in-water type (O/W) spinning emulsion: the 12g Polycarbosilane is dissolved in the 10mL toluene, makes mass fraction and be 60% homogeneous oil-phase solution; The 1.5g polyethylene glycol oxide is dissolved in the 10mL distilled water, adds the 0.07g lauryl sodium sulfate, the formation mass fraction is 13% homogeneous aqueous phase solution; Again described aqueous phase solution is dropwise joined in the oil-phase solution, obtain oil-in-water type (O/W) the spinning emulsion of stable and uniform after mixing;
(2) solution jet spinning method prepares the precursor fiber: the spinning emulsion is fed to a spray silk die head with the speed of 10mL/h/ spinneret orifice, the spinning emulsion is extruded from spinneret orifice, form the emulsion thread; Then utilize one high velocity jet air-flow (speed is 2000 times of spinning emulsion thread, and temperature is 25 ℃) with the described spinning emulsion of the jet angle drawing-off refinement thread of 0 ° of spinning emulsion thread, make it to form carborundum precursor composite fibre; The suction airstream of utilizing at last blower fan to produce is collected in described carborundum precursor composite fibre on the lace curtaining.Spray silk die head to the distance of lace curtaining is that receiving range is l00cm.
(3) melt processed and high-temperature calcination are not processed: above-mentioned carborundum precursor composite 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; Again with this fusion-free fibre under inert gas shielding, from room temperature, be warming up to 1100 ℃ with the speed of 0.5 ℃/min, and insulation 1.5 hours under this temperature, obtained silicon carbide fibre.
The number picture figure of the carborundum precursor composite fibre that obtains as shown in Figure 2, as can be seen from the figure, nascent composite fibre is the nonwoven fabric distributions, pattern is regular.
The low multiple scanning electron microscope (SEM) photograph sheet of the carborundum precursor composite fibre that obtains as shown in Figure 3, as can be seen from the figure, nascent composite fibre diameter distributes more even, average diameter is about 14.8 μ m.
The high multiple scanning electron microscope (SEM) photograph sheet of the carborundum precursor composite fibre that obtains as shown in Figure 4, as can be seen from the figure, nascent composite fibre is rough, contains a large amount of micelles, specific area is large.
The low multiple scanning electron microscope (SEM) photograph sheet of the silicon carbide fibre that obtains as shown in Figure 5, as can be seen from the figure, silicon carbide fibre fragility is larger, fibrous fracture is more, average diameter is about 9.2 μ m.
The high multiple scanning electron microscope (SEM) photograph sheet of the silicon carbide fibre that obtains as shown in Figure 6, as can be seen from the figure, the silicon carbide fibre surface is tending towards smooth, particle content tails off.
The X-ray diffraction picture of the silicon carbide fibre that obtains as shown in Figure 7, as can be seen from the figure, contain 2 θ=35.7 °, three diffraction maximums of 60.1 °, 70.9 ° in the fiber, correspond respectively to (111), (220) and (311) diffraction maximum of beta silicon carbide.
(1) preparation of oil-in-water type (O/W) spinning emulsion: 5g polyureas silane is dissolved in the 10mL dimethylbenzene, makes mass fraction and be 36.7% homogeneous oil-phase solution; The 1.2g polyvinylpyrrolidone is dissolved in the 10mL distilled water, adds the 0.06g neopelex, the formation mass fraction is 10.7% homogeneous aqueous phase solution; Again described aqueous phase solution is dropwise joined in the oil-phase solution, obtain oil-in-water type (O/W) the spinning emulsion of stable and uniform after mixing;
(2) solution jet spinning method prepares the precursor fiber: the spinning emulsion is fed to a spray silk die head with the speed of 15mL/h/ spinneret orifice, the spinning emulsion is extruded from spinneret orifice, form the emulsion thread; Then utilize one high velocity jet air-flow (speed is 4000 times of spinning emulsion thread, and temperature is 70 ℃) with the described spinning emulsion of the jet angle drawing-off refinement thread of 5 ° of spinning emulsion threads, make it to form carborundum precursor composite fibre; The suction airstream of utilizing at last blower fan to produce is collected in described carborundum precursor composite fibre on the lace curtaining.Spray silk die head to the distance of lace curtaining is that receiving range is 200cm.The carborundum precursor composite fibre average diameter that obtains is 5 μ m.
(3) melt processed and high-temperature calcination are not processed: above-mentioned carborundum precursor composite 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; Again with this fusion-free fibre under inert gas shielding, from room temperature, be warming up to 1000 ℃ with the speed of 0.5 ℃/min, and insulation 1.5 hours under this temperature, obtained silicon carbide fibre, average fibre diameter is about 3.8 μ in.
(1) preparation of oil-in-water type (O/W) spinning emulsion: the poly-carbon methyl-monosilane of 5g polysilazane and 5g is dissolved in the 10mL dimethylbenzene, makes mass fraction and be 53.7% homogeneous oil-phase solution; The 2.0g polyvinyl alcohol is dissolved in the 10mL distilled water, adds 0.10g alkyl methyl ammonium bromide, the formation mass fraction is 16.7% homogeneous aqueous phase solution; Again described aqueous phase solution is dropwise joined in the oil-phase solution, obtain oil-in-water type (O/W) the spinning emulsion of stable and uniform after mixing;
(2) solution jet spinning method prepares the precursor fiber: the spinning emulsion is fed to a spray silk die head with the speed of 5mL/h/ spinneret orifice, jet-stream wind speed is 6000 times of spinning emulsion thread, the jet-stream wind temperature is 60 ℃, and jet angle is 10 °, and the lace curtaining receiving range is 150cm.The precursor composite fibre average diameter that obtains is 1.4 μ m.
(3) melt processed and high-temperature calcination are not processed: above-mentioned carborundum precursor composite 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; Again with this fusion-free fibre under inert gas shielding, from room temperature, be warming up to 1000 ℃ with the speed of 0.5 ℃/min, and insulation 1.5 hours under this temperature, obtain silicon carbide fibre, average fibre diameter is 900nm.
Embodiment 4.
(1) preparation of oil-in-water type (O/W) spinning emulsion: the 8g Polycarbosilane is dissolved in (volume ratio of chloroform and carbon tetrachloride is 1: 1) in 10mL chloroform and the carbon tetrachloride mixed solution, makes mass fraction and be 48% homogeneous oil-phase solution; 2g polyethylene glycol oxide and 2g polyvinyl alcohol are dissolved in the 10mL distilled water, add the 0.05g polyoxyethylene alkyl phenyl ether, the formation mass fraction is 28.5% homogeneous aqueous phase solution; Again described aqueous phase solution is dropwise joined in the oil-phase solution, obtain oil-in-water type (O/W) the spinning emulsion of stable and uniform after mixing;
(2) solution jet spinning method prepares the precursor fiber: the spinning emulsion is fed to a spray silk die head with the speed of 20mL/h/ spinneret orifice, jet-impingement speed is 10000 times of spinning emulsion thread, the jet-stream wind temperature is 50 ℃, and jet angle is 15 °, and the lace curtaining receiving range is 50cm.The carborundum precursor composite fibre average diameter that obtains is 8 μ m.
(3) melt processed and high-temperature calcination are not processed: above-mentioned carborundum precursor composite 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; Again with this fusion-free fibre under inert gas shielding, from room temperature, be warming up to 1000 ℃ with the speed of 0.5 ℃/min, and insulation 1.5 hours under this temperature, obtain silicon carbide fibre, average fibre diameter is 7 μ m.
Embodiment 5.
(1) preparation of oil-in-water type (O/W) spinning emulsion: 10g Polycarbosilane and 5g polyureas silane are dissolved in (volume ratio of toluene and carbon tetrachloride is 1: 1) in 10mL toluene and the carbon tetrachloride mixed solution, make mass fraction and be 55% homogeneous oil-phase solution; 4g polyvinylpyrrolidone and 2g polyvinyl alcohol are dissolved in the 10mL distilled water, add the 0.02g alkyl betaine, the formation mass fraction is 37.5% homogeneous aqueous phase solution; Again described aqueous phase solution is dropwise joined in the oil-phase solution, obtain oil-in-water type (O/W) the spinning emulsion of stable and uniform after mixing;
(2) solution jet spinning method prepares the precursor fiber: the spinning emulsion is fed to a spray silk die head with the speed of 12mL/h/ spinneret orifice, jet-stream wind speed is 20000 times of spinning emulsion thread, the jet-stream wind temperature is 100 ℃, and jet angle is 20 °, and the lace curtaining receiving range is 120cm.The carborundum precursor composite fibre average diameter that obtains is 3 μ m.
(3) melt processed and high-temperature calcination are not processed: above-mentioned carborundum precursor composite 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; Again with this fusion-free fibre under inert gas shielding, from room temperature, be warming up to 1000 ℃ with the speed of 0.5 ℃/min, and insulation 1.5 hours under this temperature, obtain silicon carbide fibre, average fibre diameter is 2.1 μ m.
Claims (10)
1. the preparation method of a carborundum precursor composite fibre is characterized in that, may further comprise the steps:
1) preparation of oil-in-water type (O/W) spinning emulsion: a kind of carborundum preceramic polymer is dissolved at least a organic solvent, and making mass fraction is the homogeneous oil-phase solution of 10-70%; A kind of water-soluble fibre-forming polymer is dissolved in the water, adds surfactant, forming mass fraction is the homogeneous aqueous phase solution of 1-50%, and the consumption of surfactant is the 0.1-10% of solution quality; Again with described precursor solution and water-soluble polymer solution with volume ratio 1: 10-1: 1 mixes, and obtains stable oil-in-water type (O/W) spinning emulsion;
2) solution jet spinning method prepares carborundum precursor composite fibre: the spinning emulsion is fed to spinning head with the feed liquor speed of 1-40mL/h/ spinneret orifice, the spinning emulsion is extruded from spinning head, form the emulsion thread; Then utilize one high velocity jet air-flow at least with the described spinning emulsion of the jet angle drawing-off refinement thread of 0-30 ° of spinning emulsion thread, form gradually carborundum precursor composite fibre.
2. the preparation method of carborundum precursor composite fibre according to claim 1 is characterized in that, described carborundum precursor is one or more mixtures in Polycarbosilane, polysilazane, polyureas silane, polymethyl silicane, the poly-carbon methyl-monosilane.
3. the preparation method of carborundum precursor composite fibre according to claim 1 is characterized in that, described organic solvent is toluene, dimethylbenzene, benzene, cyclohexane, pentamethylene, chloroform, carbon tetrachloride or acetonitrile.
4. the preparation method of carborundum precursor composite fibre according to claim 1, it is characterized in that described water-soluble fibre-forming polymer is one or more mixtures in polyvinyl acetate, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol oxide, polyacrylamide, poly, polyethylene glycol, the starch derivatives.
5. the preparation method of carborundum precursor composite fibre according to claim 1 is characterized in that, described surfactant is anion active agent, cationic active agent, tween or amphoteric surfactant.
6. the preparation method of carborundum precursor composite fibre according to claim 5, it is characterized in that described anion active agent is linear alkylbenzene sulfonate (LAS), α alkenyl sulphonate, alkyl sulfate, polyethylene glycol oxide alkyl sulfate, sodium alkyl sulfate, alkylsurfuric acid calcium or alkyl benzene calcium sulfonate.
7. the preparation method of carborundum precursor composite fibre according to claim 5 is characterized in that, described cationic active agent is dialkyl dimethyl ammonium salt, imidazole salts, alkyl dimethyl aniline salt or alkyl methyl ammonium bromide.
8. the preparation method of carborundum precursor composite fibre according to claim 5, it is characterized in that described tween is fatty alcohol-polyoxyethylene ether, oxidation of alkyl Dimethyl Ammonium, fatty acid alkanol amides ester, APG or polyoxyethylene alkyl phenyl ether.
9. the preparation method of carborundum precursor composite fibre according to claim 5 is characterized in that, described amphoteric surfactant is alkyl betaine or alkyl sulfo betaines.
10. the preparation method of carborundum precursor composite fibre according to claim 1 is characterized in that, the temperature of described high velocity jet air-flow is 20-140 ℃, and speed is 1000-30000 times of spinning emulsion thread speed.
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