CN102674845A - Preparation method of silicon carbide fibers with silicon nitride surface layer - Google Patents
Preparation method of silicon carbide fibers with silicon nitride surface layer Download PDFInfo
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Abstract
The invention relates to a preparation method of silicon carbide fibers with a silicon nitride surface layer. The preparation method comprises the following steps of: using polycarbosilane (PCS) which is prepared by using organic silicon polymers through high-temperature cracking as raw materials, conducting melt-spinning to obtain continuous PCS polymer fibers, placing the continuous PCS polymer fibers in the atmosphere of air or activated gas for non-melting treatment, placing the non-melting fibers in a high-temperature atmosphere furnace for high-temperature nitration and decarbonization under the atmosphere of ammonia with certain concentration, and further sintering for densification at high temperature to obtain the silicon carbide fibers with the silicon nitride surface layer. The preparation method of the silicon carbide fibers with the silicon nitride surface layer has the advantages that the process and the equipment are simple, the cost of the prepared silicon carbide fibers is low and the resistivity is adjustable.
Description
Technical field
The present invention relates to a kind of preparation method of silicon carbide fiber, especially relate to a kind of silicon nitride (Si that has
3N
4) silit (SiC) fiber preparation method on top layer.
Background technology
Silit (SiC) fiber is that important high-performance strengthens one of ceramic fiber, have excellent intensity, modulus, creep resistance, fire-resistant oxidation resistant property, with the consistency and the high band wave absorbtion of ceramic matrix.The SiC fiber is a kind of outstanding functional structure material, has a extensive future at numerous areas such as aerospace, nuclear power.Each developed country of the world gives very big concern to this, at present, Japan has realized the production of SiC fiber industry, and China's technical application is blocked.At home; The National University of Defense technology was through the exploratory development in surplus 30 years; Independent development goes out serial SiC fiber, comprises that KD-I SiC fiber, KD-II SiC fiber, KA-SA high-temperature resistant type SiC fiber and KD-X inhale ripple SiC fiber, and fibre quality index has reached or approaching external like product level.
Based on SiC fiber excellent mechanical property, high-temperature stability and microwave absorbing property, it becomes universally acknowledged one of the enhancing body of high performance structures Wave suction composite material that is suitable as most.Stealth material by the SiC fiber production has the dual nature of inhaling ripple and carrying.But the SiC fiber that utilizes present more sophisticated precursor method to prepare is a kind of n type, semiconductor material, and resistivity is 10
6About Ω cm.And wideband section stealth material requires the resistivity of SiC fiber can carry out regulation and control (10 in a big way
-2-10
7Ω cm).For this reason, developed the resistivity regulate and control method of multiple SiC fiber, mainly contained: chemical reaction method, physics blending method, controlling fiber interface shape method, controlling fiber oxygen level method and surface-coated method.As adjusting its electromagnetic parameter, at surface deposition B at fiber surface metal lining nickel, cobalt
4The C layer can change the fiber dielectric properties.Wherein, have cracking carbon (PyC) coating of conductivity and SP 1 (BN), silicon nitride (Si through coating with insulating property
3N
4), aluminum oxide (Al
2O
3) to wait inorganic coating be modal fiber electrical property regulate and control method.
Silicon nitride (Si
3N
4) pottery has good insulation performance property, also has compactness, stability simultaneously, characteristics such as HS, highly heatproof and shockproof stability, high temperature creep are little, wear-resisting, high antioxidant, and Si
3N
41400-1500 ℃ of high temperature pre-oxidation treatment, can on ceramic material surfaces, form Si
2N
2The O phase can significantly improve Si
3N
4The scale resistance and the hot strength of pottery, therefore, preparation has gradient silicon nitride (Si
3N
4) continuous SiC fiber of surface structure has important use and be worth.
CVD and PIP are the common coatings technology of ceramic based material.But for preparation silicon nitride (Si
3N
4) top layer, CVD technology not only needs special processing unit, and is controlling deposit thickness and guaranteeing that coating also has difficulties aspect evenly continuous; Possibly cause synnema internal fiber coating to coat problems such as incomplete; And the cracking at high temperature of PIP processing requirement possibly produce than macrolesion fiber, and is prone to form strong interface combination; Have tangible skin-core structure, these all might reduce the mechanical property and the wave-sucking performance of fiber.
Summary of the invention
The technical problem that the present invention will solve is, overcomes the deficiency of prior art, provides a kind of technology and equipment simple, low cost of manufacture, the regulatable preparation method with the silicon carbide fiber on silicon nitride top layer of resistivity.
The technical solution adopted for the present invention to solve the technical problems is that a kind of preparation method with the silicon carbide fiber on silicon nitride top layer may further comprise the steps:
(1) organosilicon polymer is placed reaction kettle, vacuumize for five times repeatedly, fill after purity is 99.999% high pure nitrogen or argon gas; Be heated to 400-500 ℃ of (preferred 430-480 ℃) cracking 1-6h (preferred 3-4 h); Crude product dissolves after-filtration through toluene, again filtrating is heated to 300-400 ℃ (preferred 350-380 ℃) and carries out underpressure distillation, removes and desolvates and lower-molecular substance; Cooling gets Polycarbosilane (PCS);
(2) step (1) gained Polycarbosilane is placed the molten tube of melt spinning device; Under 99.999% high pure nitrogen or argon gas inert atmosphere protection, be heated to 280-380 ℃; After treating that its fine melt becomes even melt, at 250-320 ℃, under the 0.1-0.8MPa (preferred 0.6-0.7 MPa); Carry out drawing-off with 200-600m/min (preferred 450-550 m/min) speed, get continuous P CS fiber;
(3) take one of following three kinds of methods to carry out not melt processed and produce the PCS fusion-free fibre: (a) step (2) gained continuous P CS fiber is placed not melt processed device; Vacuumize; Filling purity is 99.999% high pure nitrogen; Behind the triplicate, feed reactive atmosphere to 0.1MPa, (preferred 15-20 ℃/min) heat-up rate is heated to 300-450 ℃ (preferably 350-400 ℃) by 10-30 ℃/min; And after 1-6 hour (preferred 3-5 hour) handled in this temperature insulation, make fusion-free fibre; (b) step (2) gained continuous P CS fiber is placed not melt processed device; Heat-up rate by 10-20 ℃/hour (preferred 12-16 ℃/hour) in air atmosphere is heated to 150-250 ℃ (preferred 180-220 ℃); Insulation oxide treatment 2-4 hour makes fusion-free fibre; (c) step (2) gained continuous P CS fiber is placed electron beam irradiation, after irradiation dose reached 5-20MGy (preferred 12-16 MGy), anneal made fusion-free fibre;
(4) step (3) gained fusion-free fibre is placed high-temperature atmosphere furnace; At ammonia; Or ammonia and nitrogen or ammonia and argon gas etc. mix under the mixed atmosphere that forms; (preferred 130-160 ℃/h) speed is warming up to 600-1000 ℃ (preferred 700-900 ℃), and insulation was handled 1-2 hour under 1200-1400 ℃ of temperature, made to have Si by 100-200 ℃/h
3N
4Top layer SiC fiber.
In the step (1), said organosilicon polymer is the silane polymer that constitutes main chain with Si-Si key and Si-C key, and its structure is linearity or ring-type, preferred polysilane, polydimethyl silane, polymethyl silicane, polyphenylene silane or ring silicon-carbon alkane etc.
In the step (3), in the not melt processed of PCS fiber, said reactive atmosphere is ethene or acetylene.
In the step (4), said ammonia mixes with nitrogen, argon gas etc. in the mixed atmosphere that forms, volumetric concentration >=10% of preferred ammonia.
The present invention utilizes ammonia in infiltration of continuous fibre radial gas chemistry and original position decarburizing reaction, controls its diffusion depth and carries out the gradient nitrogenize, and preparation has silit (SiC) fiber on gradient silicon nitride top layer.Following positive effect is compared with prior art arranged: (1) the present invention places high-temperature atmosphere furnace under the ammonia atmosphere of proper concn, to carry out the high-temperature ammonolysis decarburization fusion-free fibre; Preparation gradient silicon nitride top layer; Can realize the regulation and control on a large scale of fabric resistor rate through the processing parameter of control nitrogenize decarburization; (2) the present invention directly adds reactive atmosphere adjusting electrical property and surface structure in firing process, compares with the PIP coating technology with the CVD technology, and technology is simple, and it is convenient to implement, and low cost of manufacture utilizes the production unit of SiC fiber just can implement, and is easy to industriallization; (3) silit with silicon nitride top layer (SiC) fiber of the present invention's preparation, with respect to general silicon carbide fiber, high temperature resistant and good in oxidation resistance.
Description of drawings
Fig. 1 is embodiment 1 obtained SEM microscopic appearance figure with the SiC fiber on silicon nitride top layer;
Fig. 2 is the EDX figure on embodiment 1 gained SiC fiber silicon nitride top layer.
Embodiment
Below in conjunction with specific embodiment the present invention is done further explain.
Embodiment 1
Present embodiment may further comprise the steps:
(1) polysilane is placed reaction kettle, vacuumizes for five times repeatedly, fill 99.999% high pure nitrogen after; Be heated to 400 ℃ of cracking 2h, crude product dissolves after-filtration through toluene, again filtrating is heated to 300 ℃ and carries out underpressure distillation; Remove and desolvate and lower-molecular substance, cooling gets Polycarbosilane (PCS);
(2) step (1) gained Polycarbosilane being placed the molten tube of melt spinning device, is to be heated to 300 ℃ under the protection of 99.999% high pure nitrogen in purity, treat that its fine melt becomes even melt after; At 280 ℃; 0.4MPa down, carry out drawing-off, get continuous P CS fiber with 300m/min speed;
(3) step (2) gained continuous P CS fiber is placed not melt processed device; Vacuumize, filling purity is 99.999% high pure nitrogen, behind the triplicate; Feed acetylene gas to 0.1MPa; Heat-up rate by 20 ℃/min is heated to 380 ℃, and after this temperature insulation is handled 3 hours, makes fusion-free fibre;
(4) step (3) gained fusion-free fibre is placed high-temperature atmosphere furnace, under ammonia atmosphere, be warming up to 1000 ℃ by 120 ℃/hour speed, insulation was handled 1 hour under 1400 ℃ of temperature, made to have gradient Si
3N
4Top layer SiC fiber.
Present embodiment is obtained, and to have a SEM microscopic appearance figure of SiC fiber on silicon nitride top layer as shown in Figure 1.
EDX is carried out on present embodiment gained SiC fiber silicon nitride top layer analyze (referring to Fig. 2): fiber surface is a silicon nitride structure, and Fibre diameter is 12.3
M, tensile strength is 2.2GPa, and Young's modulus is 270GPa, and the fiber oxygen level is 0.65wt%, and nitrogen content is 6.25wt%, resistivity is 2.6 * 10
8Ω cm.Handled 1 hour in 1400 ℃ of air, strength retention ratio is 65%.
Embodiment 2
Present embodiment may further comprise the steps:
Step (1) and (2) operation are with embodiment 1;
(3) step (2) gained continuous P CS fiber is placed not melt processed device, the heat-up rate by 15 ℃/hour in air atmosphere is heated to 220 ℃, and insulation oxide treatment 4 hours makes fusion-free fibre;
(4) step (3) gained fusion-free fibre is placed high-temperature atmosphere furnace, under the mixed atmosphere of ammonia and nitrogen (volume ratio 1:1) formation, be warming up to 1000 ℃ by 150 ℃/hour speed, insulation was handled 2 hours under 1200 ℃ of temperature, made to have Si
3N
4Top layer SiC fiber.
The continuous SiC fiber that present embodiment makes, top layer EDX analysis revealed, fiber surface are silicon nitride structure, Fibre diameter is 12
M, tensile strength is 2.1GPa, and Young's modulus is 260GPa, and the fiber oxygen level is 0.95wt%, and nitrogen content is 5.88wt%, resistivity is 3.5 * 10
7Ω cm.Handled 1 hour in 1400 ℃ of air, strength retention ratio is 68%.
Embodiment 3
Present embodiment may further comprise the steps:
Step (1) and (2) operation are with embodiment 1;
(3) step (2) gained continuous P CS fiber is placed the electron accelerator irradiation case, after irradiation dose reached 10MGy, anneal obtained the electron beam irradiation fusion-free fibre.
(4) step (3) gained electron beam irradiation fusion-free fibre is placed high-temperature atmosphere furnace, under ammonia and argon gas (volume ratio 1:1) mixed atmosphere, be warming up to 700 ℃ by 160 ℃/hour speed, 2h is handled in insulation under 1300 ℃ of temperature, obtains having Si
3N
4The continuous SiC fiber on top layer.
The continuous SiC fiber that present embodiment makes, top layer EDX analysis revealed fiber surface is a silicon nitride structure, Fibre diameter is 11
M, tensile strength is 2.6GPa, and Young's modulus is 285GPa, and the fiber oxygen level is 0.62wt%, and nitrogen content is 4.36wt%, resistivity is 2.6 * 10
6Ω cm.Handled 1 hour in 1400 ℃ of air, strength retention ratio is 66%.
Claims (5)
1. the preparation method with the silicon carbide fiber on silicon nitride top layer is characterized in that, may further comprise the steps:
(1) organosilicon polymer is placed reaction kettle, vacuumize for five times repeatedly, fill after purity is 99.999% high pure nitrogen or argon gas; Be heated to 400-500 ℃ of cracking 1-6h; Crude product dissolves after-filtration through toluene, again filtrating is heated to 300-400 ℃ and carries out underpressure distillation, removes and desolvates and lower-molecular substance; Cooling gets Polycarbosilane;
Said organosilicon polymer is the silane polymer that constitutes main chain with Si-Si key and Si-C key, and its structure is linearity or ring-type;
(2) step (1) gained Polycarbosilane is placed the molten tube of melt spinning device; Under 99.999% high pure nitrogen or argon gas inert atmosphere protection, be heated to 280-380 ℃; After treating that its fine melt becomes even melt, at 250-320 ℃, under the 0.1-0.8MPa; Carry out drawing-off with 200-600m/min speed, get continuous P CS fiber;
(3) take one of following three kinds of methods to carry out not melt processed and produce the PCS fusion-free fibre: (a) step (2) gained continuous P CS fiber is placed not melt processed device; Vacuumize, filling purity is 99.999% high pure nitrogen, behind the triplicate; Feed reactive atmosphere to 0.1MPa; Heat-up rate by 10-30 ℃/min is heated to 300-450 ℃, and after this temperature insulation is handled 1-6 hour, makes fusion-free fibre; (b) step (2) gained continuous P CS fiber is placed not melt processed device, the heat-up rate by 10-20 ℃/hour in air atmosphere is heated to 150-250 ℃, and insulation oxide treatment 2-4 hour makes fusion-free fibre; (c) step (2) gained continuous P CS fiber is placed electron beam irradiation, after irradiation dose reached 5-20MGy, anneal made fusion-free fibre;
(4) step (3) gained fusion-free fibre is placed high-temperature atmosphere furnace; At ammonia; Or ammonia mixes with argon gas under the mixed atmosphere that forms with nitrogen or ammonia; Speed by 100-200 ℃/h is warming up to 600-1000 ℃, and insulation was handled 1-2 hour under 1200-1400 ℃ of temperature, makes to have Si
3N
4The SiC fiber on top layer.
2. the preparation method with the silicon carbide fiber on silicon nitride top layer according to claim 1 is characterized in that, in the step (1), said organosilicon polymer is polysilane, polydimethyl silane, polymethyl silicane, polyphenylene silane or ring silicon-carbon alkane.
3. the preparation method with the silicon carbide fiber on silicon nitride top layer according to claim 1 and 2 is characterized in that, in the step (3), in the not melt processed of PCS fiber, said reactive atmosphere is ethene atmosphere or acetylene atmosphere.
4. the preparation method with the silicon carbide fiber on silicon nitride top layer according to claim 1 and 2 is characterized in that, in the step (4), and in the mixed atmosphere of said ammonia and nitrogen, ammonia and argon gas, the volumetric concentration of ammonia >=10%.
5. the preparation method with the silicon carbide fiber on silicon nitride top layer according to claim 1 is characterized in that, may further comprise the steps:
(1) organosilicon polymer is placed reaction kettle, vacuumize for five times repeatedly, fill after purity is 99.999% high pure nitrogen or argon gas; Be heated to 430-480 ℃ of cracking 3-4 h; Crude product dissolves after-filtration through toluene, again filtrating is heated to 350-380 ℃ and carries out underpressure distillation, removes and desolvates and lower-molecular substance; Cooling gets Polycarbosilane;
Said organosilicon polymer is polysilane, polydimethyl silane, polymethyl silicane, polyphenylene silane or ring silicon-carbon alkane;
(2) step (1) gained Polycarbosilane is placed the molten tube of melt spinning device; Under 99.999% high pure nitrogen or argon gas inert atmosphere protection, be heated to 280-380 ℃; After treating that its fine melt becomes even melt, at 250-320 ℃, under the 0.6-0.7 MPa; Carry out drawing-off with 450-550 m/min speed, get continuous P CS fiber;
(3) take one of following three kinds of methods to carry out not melt processed and produce the PCS fusion-free fibre: (a) step (2) gained continuous P CS fiber is placed not melt processed device; Vacuumize, filling purity is 99.999% high pure nitrogen, behind the triplicate; Feed reactive atmosphere to 0.1MPa; Heat-up rate by 15-20 ℃/min is heated to 350-400 ℃, and after this temperature insulation is handled 3-5 hour, makes fusion-free fibre; (b) step (2) gained continuous P CS fiber is placed not melt processed device, the heat-up rate by 12-16 ℃/hour in air atmosphere is heated to 180-220 ℃, and insulation oxide treatment 2-4 hour makes fusion-free fibre; (c) step (2) gained continuous P CS fiber is placed electron beam irradiation, after irradiation dose reached 12-16 MGy, anneal made fusion-free fibre;
Said reactive atmosphere is ethene atmosphere or acetylene atmosphere;
(4) step (3) gained fusion-free fibre is placed high-temperature atmosphere furnace; At ammonia, or under the mixed atmosphere of ammonia and nitrogen or ammonia and argon gas, be warming up to 700-900 ℃ by the speed of 130-160 ℃/h; Insulation was handled 1-2 hour under 1200-1400 ℃ of temperature, made to have Si
3N
4Top layer SiC fiber;
In the mixed atmosphere of said ammonia and nitrogen, ammonia and argon gas, the volumetric concentration of ammonia >=10%.
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| CN110105070A (en) * | 2019-05-24 | 2019-08-09 | 中国人民解放军国防科技大学 | Continuous silicon carbide fiber with controllable electrical property and wide range and preparation method thereof |
| CN112358621A (en) * | 2020-11-12 | 2021-02-12 | 江西信达航科新材料科技有限公司 | High-temperature-resistant silicon carbide fiber precursor polycarbosilane and preparation method thereof |
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