CN103966701B - A kind of preparation method of porous silicon carbide nanofiber - Google Patents
A kind of preparation method of porous silicon carbide nanofiber Download PDFInfo
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Abstract
The preparation method of a kind of porous silicon carbide nanofiber, comprises the following steps: (1) preparation of nano carbon fiber precursor polymer spinning solution; (2) electrostatic spinning prepares polymer nanofiber; (3) polymer nanofiber is carried out pre-oxidation crosslinking; (4) high temperature of pre-oxidation polymer nanofiber burns till, and prepares carbon nano-fiber; (5) carbon nano-fiber and silica flour generation carbothermic reduction reaction obtain many empty SiC nano fibers. The pattern of gained SiC nano fiber of the present invention, diameter and order all can obtain Effective Regulation by simple means; Production cycle is shorter, it is simple to realizing extension and produce, its preparation process is simple, it is simple to realize commercial production; Porous silicon carbide nanofiber has a wide range of applications in fields such as high temperature filtration, high-temperature catalytic, catalyst carrier, heat-and sound-insulating, gas separation and chemical sensors.
Description
Technical field
The preparation method that the present invention relates to a kind of silicon carbide fibre, the preparation method particularly relating to a kind of porous silicon carbide nanofiber.
Background technology
Porous silicon carbide has the features such as specific surface area is big, density is low, high temperature resistant, corrosion-resistant, separates and the field such as chemical sensor has a wide range of applications at high temperature filtration (such as diesel oil and melted metal filtering), high-temperature catalytic, catalyst carrier, heat-and sound-insulating, gas. At present, different porous silicon carbide Silicon forms, all have been reported that such as block, aeroge, nanotube, nano wire, foamed ceramics and nano whisker etc., the method preparing porous silicon carbide also has a lot, such as electrochemical etching, sol-gal process, carbothermic method, chemical vapor infiltration and nanometer casting etc. And melt spinning method is concentrated mainly on for the research of silicon carbide fibre and prepares micron order high strength carbonizing silica fibre, the relevant report of porous silicon carbide fibers is less, and particularly nano level porous silicon carbide fibers have not been reported.
Electrostatic spinning is dependent on the high-pressure electrostatic of several thousand to several ten thousand volts and stretches the effective ways preparing nanofiber, except possessing that equipment is simple, cost is low and except the advantage such as the suitability is wide, also having the advantage that (1) can obtain the bigger nanofiber of draw ratio (length is even up to meter level); (2) reason such as rapid solvent evaporation time due to spinning, the nanofiber of preparation is generally porous, and its specific surface area is high 1 ~ 2 order of magnitude than conventional film; (3) while preparing nanofiber, by the design of acceptor or electric field patterns and control, it is possible to the morphosis of prepared superfine fibre is controlled. Electrostatic methods is adopted to also allow for realizing the large-scale production of nanofiber. Recently, HuilinHou et al. is with polysilazane (polyureasilazane) and polyvinylpyrrolidone (polyvinylpyrrolidone) for raw material, method of electrostatic spinning is adopted to prepare porous silicon carbide fibers, but its prepared silicon carbide fibre average diameter is 1.5 ��m, it does not have reach nanoscale.The preparation method that CN101876095A discloses a kind of silicon carbide fibre; utilize precipitation fractionation principle; adopt method of electrostatic spinning can spin extremely rare Polycarbosilane suspension; by the Polycarbosilane precursor obtained through do not melt crosslinking Treatment and high temperature burn till after can obtain porous silicon carbide superfine fibre; fibre diameter is 0.5 ~ 2 ��m; but extremely dilute solution spinning fibre yield is low, it is unsuitable for scale and prepares. CN1033434225A discloses the use of good solvent with non-solvent as mixed solvent, with silicon carbide ceramics precursor silicon-containing polymer for raw material, obtains flexible, porous silicon carbide fibre by method of electrostatic spinning. But same prepared silicon carbide fibre average diameter is 0.5 ~ 3 ��m, is difficulty with the preparation of porous silicon carbide nanofiber; And CN101876095A and CN1033434225A is with precursor silicon-containing polymer for raw material, and owing to the molecular weight of precursor silicon-containing polymer is generally relatively low, in electrostatic spinning process, spinnability is poor, and the fibre diameter obtained is also uneven.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes the deficiencies in the prior art, it is provided that the preparation method of a kind of porous silicon carbide nanofiber, and prepared porous silicon carbide fibers diameter reaches nanometer level.
The technical solution adopted for the present invention to solve the technical problems is, a kind of preparation method of porous silicon carbide nanofiber, it is with carbon nano-fiber precursor polymer for raw material, a certain amount of precursor polymer is dissolved in solvent, burn till make carbon nano-fiber through electrostatic spinning, pre-oxidation crosslinking, high temperature, and then carbon nano-fiber and silica flour are carried out the product that carbon thermal reduction prepares under the high temperature conditions.
Specifically include following steps:
(1) preparation spinning solution: being dissolved in solvent by carbon nano-fiber precursor polymer and be configured to homogeneous spinning solution, described carbon nano-fiber precursor polymer concentration in homogeneous spinning solution is 5wt% ~ 50wt%;
(2) electrostatic spinning: the homogeneous spinning solution of step (1) gained is carried out electrostatic spinning, shower nozzle used by electrostatic spinning is the metal needle that internal diameter is sized to 0.5 ~ 1.5mm, spinning voltage 12kV ~ 30kV, receiving range (needle point to the vertical dimension of receiving screen) 15 ~ 25cm, feeding rate 5 ~ 30 �� l/min, spinning temperature is 10 ~ 60 DEG C, and relative air humidity is 20RH% ~ 80RH%; Under electric field force effect, spinning solution drawing-off gradually refines, simultaneously solvent volatilization, forms polymer nanofiber and collects on the receiver;
(3) pre-oxidation crosslinking: the polymer nanofiber that step (2) obtains is placed in oxidation furnace, with 0.1 ~ 10 DEG C/min(preferably 1 ~ 5 DEG C/min) heating rate be warming up to 200 ~ 300 DEG C, insulation 0.5 ~ 5h(preferably 1 ~ 3h), carry out pre-oxidation crosslinking, after being cooled to room temperature, obtain non-fusible nanofiber;
(4) high temperature burns till: non-fusible nanofiber step (3) obtained is under inert atmosphere protection, it is warmed up to 600 ~ 2500 DEG C (preferably 1000 ~ 1800 DEG C with the heating rate of 1 ~ 10 DEG C/min, more preferably 1400 ~ 1600 DEG C), temperature retention time is 0.5 ~ 3h(preferably 1 ~ 2h), high temperature pyrolysis, obtains carbon nano-fiber;
(5) carbon thermal reduction: put in corundum crucible together with the carbon nano-fiber that step (4) is obtained and silica flour (mol ratio of described silica flour and carbon nano-fiber is more than 1:1); under the inert atmosphere protection that flow is 0.1 ~ 1.0L/min; heat to 1250 ~ 1600 DEG C with the heating rate of 3 ~ 10 DEG C/min; temperature retention time is 1 ~ 10h; carry out carbothermic reduction reaction, obtain porous silicon carbide nanofiber.
Further, in step (1), described carbon nano-fiber precursor polymer is at least one in polyacrylonitrile, phenolic resin, Colophonium.
Further, in step (1), described solvent is dimethylformamide (DMF) or dimethyl sulfoxide (DMSO).
Further, in step (2), described receptor is flat board aluminium foil or parallel pole, adopts flat board aluminium foil receptor, can obtain unordered porous silicon carbide nanofiber; Adopt parallel pole receptor, orderly porous silicon carbide nanofiber can be obtained.
Further, step (4) and in step (5), described inert atmosphere is purity >=99.999%(v/v) high-purity argon gas or high pure nitrogen.
The present invention selects the good carbon nano-fiber precursor polymer of spinnability to be raw material, first prepares carbon nano-fiber, and then by carbothermic reduction reaction, prepares porous silicon carbide nanofiber. Carbide nano-fibril prepared by the present invention is loose structure, uniform diameter, and diameter is 50 ~ 1000nm. Porous silicon carbide fibers or be unordered non-woven fibrofelt, or be the orderly fiber felt of fiber height, specific surface area is big, and purity is high, and diameter and pattern are easily adjusted.
Compared with the prior art, present invention have the advantage that raw materials wide material sources are easy to get, with low cost; In electrostatic spinning process raw material good spinnability, it is to avoid adopt the low-molecular-weight siliceous preceramic polymer of spinnability difference and the shortcoming of fibre diameter inhomogeneities that produces; Meanwhile, the pattern of the method gained nanofiber, diameter and order all can obtain Effective Regulation by simple means; Production cycle is shorter, it is simple to realizes extension and produces; Porous silicon carbide nanofiber has a wide range of applications in fields such as high temperature filtration, high-temperature catalytic, catalyst carrier, heat-and sound-insulating, gas separation and chemical sensors.
Accompanying drawing explanation
Fig. 1 is scanning electron microscope (SEM) photo of the unordered porous silicon carbide nanofiber of embodiment 1 gained;
Fig. 2 is X-ray diffraction (XRD) spectrogram of embodiment 1 gained porous silicon carbide nanofiber;
Fig. 3 is the SEM photograph of the ordered porous silicon carbide fibre of the different-diameter obtained in embodiment 2.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
The present embodiment comprises the following steps:
(1) preparation spinning solution: polyacrylonitrile powder is joined in DMF, polyacrylonitrile powder and DMF mass ratio be 1: 10(and the mass concentration of polyacrylonitrile be 9.1wt%), stirring makes polyacrylonitrile be completely dissolved, and obtains homogeneous spinning solution;
(2) electrostatic spinning: the homogeneous spinning solution of step (1) gained is carried out electrostatic spinning, shower nozzle used by electrostatic spinning is the metal needle of internal diameter 0.8mm, spinning voltage is 16kV, receiving range is 20cm, feeding rate is 10 �� l/min, spinning temperature 20 DEG C, relative air humidity 60RH%, adopt flat board aluminium foil receptor, prepare nano polypropylene nitrile fibril;
(3) pre-oxidation crosslinking: polymer nanocomposite polyacrylonitrile fibril step (2) obtained is placed in oxidation furnace, with the ramp of 5 DEG C/min, and is incubated 1h at 280 DEG C, obtains non-fusible polyacrylonitrile fibre after being cooled to room temperature;
(4) high temperature burns till: the fusion-free fibre that step (3) obtains is placed in the noble gas (high-purity N of purity >=99.999%2) protection under high temperature furnace in, with the ramp of 5 DEG C/min to 1000 DEG C, and be incubated 1h, high temperature pyrolysis, obtain carbon nano-fiber;
(5) carbon thermal reduction: carbon nano-fiber step (4) obtained is placed in corundum crucible with silica flour (mol ratio of silica flour and carbon nano-fiber is 2:1), in the noble gas (high-purity N of purity >=99.999% that flow is 0.15L/min2) under protection, with the ramp of 5 DEG C/min to 1300 DEG C, and be incubated 3h, obtain porous silicon carbide nanofiber.
The SEM photograph of the porous silicon carbide nanofiber obtained by the present embodiment and XRD spectra are respectively as depicted in figs. 1 and 2. Can be seen that the average diameter of nanometer silicon carbide fiber is 143nm, uniform diameter, fiber is loose structure. By XRD spectra it can be seen that the diffraction maximum of nanofiber and cubic structure (3C) carborundum complies fully with, it does not have the diffraction maximum of impurity produces, and its diffraction maximum being labeled as S.F. is that the stacking fault in crystal structure causes.
Embodiment 2
The present embodiment comprises the following steps:
(1) preparation spinning solution: polyacrylonitrile powder is joined in DMF, polyacrylonitrile powder and DMF mass ratio be 1.2: 10(and the mass concentration of polyacrylonitrile be 10.7wt%), stirring makes polyacrylonitrile be completely dissolved, and is configured to homogeneous spinning solution;
(2) electrostatic spinning: the homogeneous spinning solution of step (1) gained is carried out electrostatic spinning, shower nozzle used by electrostatic spinning is the metal needle of internal diameter 0.8mm, spinning voltage is 16kV, receiving range is 20cm, feeding rate is 10 �� l/min, spinning temperature 20 DEG C, relative air humidity 60RH%, adopt parallel pole as receptor, prepare orderly nano polypropylene nitrile fibril;
(3) pre-oxidation crosslinking: polymer nanocomposite polyacrylonitrile fibril step (2) obtained is placed in oxidation furnace, with the ramp of 5 DEG C/min, and is incubated 1h at 280 DEG C, carries out pre-oxidation crosslinking; Orderly infusible polyacrylonitrile fibre is obtained after being cooled to room temperature;
(4) high temperature burns till: the orderly fusion-free fibre that step (3) obtains is placed in the noble gas (high-purity N of purity >=99.999%2) protection under high temperature furnace in, with the ramp of 5 DEG C/min to 1000 DEG C, and be incubated 1h, obtain carbon nano-fiber;
(5) carbon thermal reduction: carbon nano-fiber step (4) obtained is placed in corundum crucible with silica flour (mol ratio of silica flour and carbon nano-fiber is 2:1), in the noble gas noble gas (high-purity N of purity >=99.999% that flow is 0.15L/min2) under protection, with the ramp of 5 DEG C/min to 1300 DEG C, and be incubated 3h, obtain ordered porous SiC nano fiber.
The SEM photograph of the porous silicon carbide nanofiber obtained by the present embodiment is as shown in Figure 3. As seen from the figure, nanometer silicon carbide fiber average diameter is 200nm, uniform diameter, and fiber is loose structure, and fiber forms ordered fiber along certain orientation arrangement.
Embodiment 3
The present embodiment comprises the following steps:
(1) preparation spinning solution: polyacrylonitrile powder is joined in DMF, polyacrylonitrile powder and DMF mass ratio be 1.2: 10(and the mass concentration of polyacrylonitrile be 10.7wt%), stirring makes polyacrylonitrile be completely dissolved, and is configured to homogeneous spinning solution;
(2) electrostatic spinning: the homogeneous spinning solution of step (1) gained is carried out electrostatic spinning, shower nozzle used by electrostatic spinning is the metal needle of internal diameter 0.8mm, spinning voltage is 16kV, receiving range is 20cm, feeding rate is 15 �� l/min, spinning temperature 25 DEG C, relative air humidity 60RH%, adopt flat board aluminium foil receptor, prepare nano polypropylene nitrile fibril;
(3) pre-oxidation crosslinking: polymer nanocomposite polyacrylonitrile fibril step (2) obtained is placed in oxidation furnace, with the ramp of 3 DEG C/min, and is incubated 1h at 260 DEG C, obtains non-fusible polyacrylonitrile fibre after being cooled to room temperature;
(4) high temperature burns till: be placed in by the non-fusible polyacrylonitrile fibre that step (3) obtains in the high temperature furnace under noble gas (high-purity Ar of purity >=99.999%) protection, with the ramp of 5 DEG C/min to 1000 DEG C, and it is incubated 1h, obtain carbon nano-fiber;
(5) carbon thermal reduction: carbon nano-fiber step (4) obtained and silica flour (silica flour and carbon nano-fiber mole for 3:1) are placed in corundum crucible; under noble gas (high-purity Ar of the purity >=99.999%) protection that flow is 0.2L/min; with the ramp of 5 DEG C/min to 1500 DEG C; and it is incubated 5h, obtain porous silicon carbide nanofiber.
Porous silicon carbide nanofiber average diameter obtained by the present embodiment is 206nm, uniform diameter, and fiber is loose structure.
Embodiment 4
The present embodiment comprises the following steps:
(1) preparation spinning solution: polyacrylonitrile powder is joined in DMF, polyacrylonitrile powder and DMF mass ratio be 1.5: 10(and the mass concentration of polyacrylonitrile be 13.0wt%), stirring makes polyacrylonitrile be completely dissolved, and is configured to homogeneous spinning solution;
(2) electrostatic spinning: the homogeneous spinning solution of step (1) gained is carried out electrostatic spinning, shower nozzle used by electrostatic spinning is the metal needle that internal diameter is sized to 0.8mm, spinning voltage is 16kV, receiving range is 20cm, feeding rate is 10 �� l/min, spinning temperature 20 DEG C, relative air humidity 60RH%, adopt parallel pole as receptor, prepare orderly nano polypropylene nitrile fibril;
(3) pre-oxidation crosslinking: nano polypropylene nitrile fibril step (2) obtained is placed in oxidation furnace, with the ramp of 5 DEG C/min, and is incubated 1h at 280 DEG C, obtains orderly infusible polyacrylonitrile fibre after being cooled to room temperature;
(4) high temperature burns till: be placed in by the fusion-free fibre that step (3) obtains in the high temperature furnace under noble gas noble gas (high-purity Ar of purity >=99.999%) protection, with the ramp of 3 DEG C/min to 1400 DEG C, and it is incubated 1h, obtain orderly carbon nano-fiber;
(5) carbon thermal reduction: orderly carbon nano-fiber step (4) obtained is placed in corundum crucible with silica flour (mol ratio of silica flour and carbon fiber is 3:1); under noble gas (high-purity Ar of the purity >=99.999%) protection that flow is 0.2L/min; with the ramp of 5 DEG C/min to 1500 DEG C; and it is incubated 6h, obtain ordered porous SiC nano fiber.
Porous silicon carbide nanofiber average diameter obtained by the present embodiment is 370nm, and diameter Distribution is uniform, and fiber is loose structure, and fiber forms ordered fiber along certain orientation arrangement.
Claims (10)
1. the preparation method of a porous silicon carbide nanofiber, it is characterised in that comprise the following steps:
(1) preparation spinning solution: being dissolved in solvent by carbon nano-fiber precursor polymer and be configured to homogeneous spinning solution, described carbon nano-fiber precursor polymer concentration in homogeneous spinning solution is 5wt% ~ 50wt%;
(2) electrostatic spinning: the homogeneous spinning solution of step (1) gained is carried out electrostatic spinning, shower nozzle used by electrostatic spinning is the metal needle that internal diameter is sized to 0.5 ~ 1.5mm, spinning voltage 12kV ~ 30kV, receiving range 15 ~ 25cm, feeding rate 5 ~ 30 �� l/min, spinning temperature is 10 ~ 60 DEG C, and relative air humidity is 20RH% ~ 80RH%;Under electric field force effect, spinning solution drawing-off gradually refines, simultaneously solvent volatilization, forms polymer nanofiber and collects on the receiver;
(3) pre-oxidation crosslinking: be placed in oxidation furnace by the polymer nanofiber that step (2) obtains, be warming up to 200 ~ 300 DEG C with the heating rate of 0.1 ~ 10 DEG C/min, is incubated 0.5 ~ 5h, carries out pre-oxidation crosslinking, obtain non-fusible nanofiber after being cooled to room temperature;
(4) high temperature burns till: non-fusible nanofiber step (3) obtained, under inert atmosphere protection, is warmed up to 600 ~ 2500 DEG C with the heating rate of 1 ~ 10 DEG C/min, and temperature retention time is 0.5 ~ 3h, and high temperature pyrolysis obtains carbon nano-fiber;
(5) carbon thermal reduction: the carbon nano-fiber that step (4) obtains is put in corundum crucible together with silica flour, under the inert atmosphere protection that flow is 0.1 ~ 1.0L/min, heat to 1250 ~ 1600 DEG C with the heating rate of 3 ~ 10 DEG C/min, temperature retention time is 1 ~ 10h, carry out carbothermic reduction reaction, obtain porous silicon carbide nanofiber;
The mol ratio of described silica flour and carbon nano-fiber is more than 1:1.
2. the preparation method of porous silicon carbide nanofiber according to claim 1, it is characterised in that in step (1), described carbon nano-fiber precursor polymer is at least one in polyacrylonitrile, phenolic resin, Colophonium.
3. the preparation method of porous silicon carbide nanofiber according to claim 1 and 2, it is characterised in that in step (1), described solvent is dimethylformamide or dimethyl sulfoxide.
4. the preparation method of porous silicon carbide nanofiber according to claim 1 and 2, it is characterised in that in step (2), described receptor is flat board aluminium foil or parallel pole.
5. the preparation method of porous silicon carbide nanofiber according to claim 1 and 2, it is characterised in that in step (3), heating rate is 1 ~ 5 DEG C/min.
6. the preparation method of porous silicon carbide nanofiber according to claim 1 and 2, it is characterised in that in step (3), temperature retention time is 1 ~ 3h.
7. the preparation method of porous silicon carbide nanofiber according to claim 1 and 2, it is characterised in that step (4) and in step (5), described inert atmosphere is high-purity argon gas or the high pure nitrogen of purity >=99.999%.
8. the preparation method of porous silicon carbide nanofiber according to claim 1 and 2, it is characterised in that in step (4), by non-fusible nanofiber under inert atmosphere protection, be warmed up to 1000 ~ 1800 DEG C.
9. the preparation method of porous silicon carbide nanofiber according to claim 8, it is characterised in that in step (4), by non-fusible nanofiber under inert atmosphere protection, be warmed up to 1400 ~ 1600 DEG C.
10. the preparation method of porous silicon carbide nanofiber according to claim 1 and 2, it is characterised in that in step (4), temperature retention time is 1 ~ 2h.
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| CN116143525A (en) * | 2023-01-09 | 2023-05-23 | 山东工业陶瓷研究设计院有限公司 | Method for preparing porous ceramic material based on BN precursor |
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| CN101177269B (en) * | 2007-12-13 | 2011-05-04 | 复旦大学 | Meso-porous structural high specific surface carborundum material and preparation method thereof |
| CN101876095B (en) * | 2010-07-28 | 2011-08-10 | 中国人民解放军国防科学技术大学 | Porous silicon carbide fibers and preparation method thereof |
| CN101876094B (en) * | 2010-08-11 | 2011-12-07 | 中国人民解放军国防科学技术大学 | Preparation method of superfine zirconia/silicon carbide composite fibers |
| CN102206883B (en) * | 2011-06-03 | 2012-07-11 | 中国人民解放军国防科学技术大学 | Method for preparing fluffy superfine fibers |
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