CN103966701A - Preparation method of porous silicon carbide nanofiber - Google Patents
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Abstract
The invention discloses a preparation method of a porous silicon carbide nanofiber. The preparation method comprises the following steps of: (1) preparing a carbon nanofiber precursor polymer spinning solution; (2) performing electrostatic spinning to prepare a polymer nanofiber; (3) carrying out pre-oxidization crosslinking on the polymer nanofiber; (4) carrying out high-temperature firing on the pre-oxidized polymer nanofiber to prepare a carbon nanofiber; and (5) carrying out carbon thermal reduction on the carbon nanofiber and silicon powder to obtain the porous silicon carbide nanofiber. According to the preparation method, the morphology, the diameter and the ordering of the obtained silicon carbide nanofiber can be effectively regulated and controlled through simple means; the production cycle is relatively short so that expanded production can be conveniently realized and the preparation process is simple so that the industrial production can be conveniently realized; the porous silicon carbide nanofiber has wide application prospect in the fields of high-temperature filtration, high-temperature catalysis, catalyst carriers, heat insulation and sound insulation, gas separation, chemical sensors and the like.
Description
Technical field
The present invention relates to a kind of preparation method of silicon carbide fibre, particularly relate to a kind of preparation method of porous silicon carbide nanofiber.
Background technology
Porous silicon carbide has the features such as specific area is large, 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 (as diesel oil and melted metal filtering), high-temperature catalytic, catalyst carrier, heat-and sound-insulating, gas.At present, different porous silicon carbide forms, as block, aeroge, nanotube, nano wire, foamed ceramics and nano whisker etc. all have report, the method of preparing porous silicon carbide also has a lot, as electrochemical etching, sol-gal process, carbothermic method, chemical vapor infiltration and nanometer casting etc.Prepare micron order high strength carbonizing silica fibre and mainly concentrate on melt spinning method for the research of silicon carbide 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 to rely on the high-pressure electrostatic of several thousand to several ten thousand volts to stretch to prepare the effective ways of nanofiber, except possess that equipment is simple, cost is low and the advantage such as applicability is wide, also have the following advantages: (1) can obtain the nanofiber that draw ratio is larger (length even can reach meter level); (2) reason such as rapid solvent evaporation during due to spinning, the nanofiber of preparation is generally porous, and its specific area is than high 1 ~ 2 order of magnitude of conventional film; (3), in preparing nanofiber, by design and the control of acceptor or electric field patterns, can control the morphosis of prepared superfine fibre.Adopt electrostatic methods to be also convenient to realize the large-scale production of nanofiber.Recently, the people such as Huilin Hou are taking polysilazane (polyureasilazane) and polyvinylpyrrolidone (polyvinylpyrrolidone) as raw material, adopt method of electrostatic spinning to prepare porous silicon carbide fibers, but its prepared silicon carbide fibre average diameter is 1.5 μ m, does not reach nanoscale.CN101876095A discloses a kind of preparation method of silicon carbide fibre; utilize precipitation fractionation principle; adopt method of electrostatic spinning can spin extremely rare Polycarbosilane turbid liquid; the Polycarbosilane precursor obtaining can be obtained to porous silicon carbide superfine fibre through not melting after crosslinking Treatment and high temperature burn till; fibre diameter is 0.5 ~ 2 μ m; but extremely dilute solution spinning fibre yield is low, be unsuitable for scale preparation.CN1033434225A discloses employing good solvent and non-solvent as mixed solvent, taking silicon carbide ceramics precursor silicon-containing polymer as raw material, obtains flexible porous silicon carbide fibers by method of electrostatic spinning.But same prepared silicon carbide fibre average diameter is 0.5 ~ 3 μ m, is difficult to realize the preparation of porous silicon carbide nanofiber; And CN101876095A and CN1033434225A are taking precursor silicon-containing polymer as raw material, and because the molecular weight of precursor silicon-containing polymer is generally lower, in electrostatic spinning process, spinnability is poor, and the fibre diameter obtaining is also inhomogeneous.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes the deficiencies in the prior art, and a kind of preparation method of porous silicon carbide nanofiber is provided, 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, taking carbon nano-fiber precursor polymer as raw material, a certain amount of precursor polymer is dissolved in solvent,, high temperature crosslinked through electrostatic spinning, pre-oxidation burns till and makes carbon nano-fiber, and then carbon nano-fiber and silica flour are carried out to the product that carbon thermal reduction makes under hot conditions.
Specifically comprise the following steps:
(1) preparation spinning solution: carbon nano-fiber precursor polymer is dissolved in solvent and is mixed with homogeneous phase spinning solution, and the concentration of described carbon nano-fiber precursor polymer in homogeneous phase spinning solution is 5wt% ~ 50wt%;
(2) electrostatic spinning: step (1) gained homogeneous phase spinning solution is carried out to electrostatic spinning, electrostatic spinning shower nozzle used is that internal diameter size is the metal needle of 0.5 ~ 1.5mm, spinning voltage 12 kV ~ 30kV, receiving range (needle point is to the vertical range of receiving screen) 15 ~ 25cm, feeding rate 5 ~ 30 μ 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 refinement gradually, solvent evaporates simultaneously, forms polymer nanofiber and is collected on receiver;
(3) pre-oxidation is crosslinked: the polymer nanofiber that step (2) is obtained is placed in oxidation furnace, with preferably 1 ~ 5 DEG C/min of 0.1 ~ 10 DEG C/min() heating rate be warming up to 200 ~ 300 DEG C, preferably 1 ~ 3h of insulation 0.5 ~ 5h(), carry out pre-oxidation crosslinked, do not melted nanofiber after being cooled to room temperature;
(4) high temperature burns till: what step (3) was obtained does not melt nanofiber under inert atmosphere protection, be 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 preferably 1 ~ 2h of 0.5 ~ 3h(), high temperature pyrolysis, obtains carbon nano-fiber;
(5) carbon thermal reduction: the carbon nano-fiber that step (4) is obtained is put into corundum crucible together with silica flour (described silica flour is greater than 1:1 with the mol ratio of carbon nano-fiber); be under the inert atmosphere protection of 0.1 ~ 1.0 L/min at flow; be heated 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 resins, pitch.
Further, in step (1), described solvent is dimethyl formamide (DMF) or dimethyl sulfoxide (DMSO) (DMSO).
Further, in step (2), described receiver is dull and stereotyped aluminium foil or parallel pole, adopts dull and stereotyped aluminium foil receiver, can obtain unordered porous silicon carbide nanofiber; Adopt parallel pole receiver, can obtain orderly porous silicon carbide nanofiber.
Further, in step (4) and step (5), described inert atmosphere is purity >=99.999%(v/v) high-purity argon gas or high pure nitrogen.
It is raw material that the present invention selects the good carbon nano-fiber precursor polymer of spinnability, first prepares carbon nano-fiber, and then by carbothermic reduction reaction, prepares porous silicon carbide nanofiber.The prepared carbide nano-fibril of the present invention is loose structure, and diameter is even, and diameter is 50 ~ 1000nm.Porous silicon carbide fibers or be unordered non-woven fibrofelt, or be the orderly fibrofelt of fiber height, specific area is large, and purity is high, and diameter and pattern are easily adjusted.
Compared with the prior art, the present invention has following advantage: raw materials wide material sources are easy to get, with low cost; Raw material good spinnability in electrostatic spinning process, has avoided adopting spinnability poor low-molecular-weight siliceous preceramic polymer and the shortcoming of the 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, is convenient to realize 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.
Brief description of the drawings
Fig. 1 is scanning electronic 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 photo of the ordered porous silicon carbide fibre of the different-diameter that obtains 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, and polyacrylonitrile powder and DMF mass ratio are 1: 10(is that the mass concentration of polyacrylonitrile is 9.1wt%), stir polyacrylonitrile is dissolved completely, obtain homogeneous phase spinning solution;
(2) electrostatic spinning: step (1) gained homogeneous phase spinning solution is carried out to electrostatic spinning, electrostatic spinning shower nozzle used is the metal needle of internal diameter 0.8mm, spinning voltage is 16kV, receiving range is 20cm, feeding rate is 10 μ l/min, 20 DEG C of spinning temperatures, relative air humidity 60RH%, adopt dull and stereotyped aluminium foil receiver, make nano polypropylene nitrile fibrillation;
(3) pre-oxidation is crosslinked: the polymer nanocomposite polyacrylonitrile fibrillation that step (2) is obtained is placed in oxidation furnace, heats up, and at 280 DEG C of insulation 1h with the speed of 5 DEG C/min, is not melted polyacrylonitrile fibre after being cooled to room temperature;
(4) high temperature burns till: the fusion-free fibre that step (3) is obtained is placed in the inert gas (high-purity N of purity>=99.999%
2) protection under high temperature furnace in, be warming up to 1000 DEG C with the speed of 5 DEG C/min, and be incubated 1h, high temperature pyrolysis, obtains carbon nano-fiber;
(5) carbon thermal reduction: the carbon nano-fiber that step (4) is obtained and silica flour (mol ratio of silica flour and carbon nano-fiber is 2:1) are placed in corundum crucible is the inert gas (high-purity N of purity>=99.999% of 0.15 L/min at flow
2) under protection, be warming up to 1300 DEG C with the speed of 5 DEG C/min, and be incubated 3h, obtain porous silicon carbide nanofiber.
The SEM photo of the prepared porous silicon carbide nanofiber of the present embodiment and XRD spectra are respectively as depicted in figs. 1 and 2.The average diameter that can find out nano silicon carbide silica fibre is 143nm, and diameter is even, and fiber is loose structure.Can be found out the diffraction maximum of nanofiber and cubic structure (3 by XRD spectra
c) carborundum meets completely, do not have the diffraction maximum of impurity to produce, its diffraction maximum that is 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, and polyacrylonitrile powder and DMF mass ratio are 1.2: 10(is that the mass concentration of polyacrylonitrile is 10.7wt%), stir polyacrylonitrile is dissolved completely, be mixed with homogeneous phase spinning solution;
(2) electrostatic spinning: step (1) gained homogeneous phase spinning solution is carried out to electrostatic spinning, electrostatic spinning shower nozzle used is the metal needle of internal diameter 0.8mm, spinning voltage is 16kV, receiving range is 20cm, feeding rate is 10 μ l/min, 20 DEG C of spinning temperatures, relative air humidity 60RH%, adopt parallel pole as receiver, make orderly nano polypropylene nitrile fibrillation;
(3) pre-oxidation is crosslinked: the polymer nanocomposite polyacrylonitrile fibrillation that step (2) is obtained is placed in oxidation furnace, heats up, and at 280 DEG C of insulation 1h, carry out pre-oxidation crosslinked with the speed of 5 DEG C/min; After being cooled to room temperature, obtain orderly infusible polyacrylonitrile fibre;
(4) high temperature burns till: the orderly fusion-free fibre that step (3) is obtained is placed in the inert gas (high-purity N of purity>=99.999%
2) protection under high temperature furnace in, be warming up to 1000 DEG C with the speed of 5 DEG C/min, and be incubated 1h, obtain carbon nano-fiber;
(5) carbon thermal reduction: the carbon nano-fiber that step (4) is obtained and silica flour (mol ratio of silica flour and carbon nano-fiber is 2:1) are placed in corundum crucible is the inert gas inert gas (high-purity N of purity>=99.999% of 0.15 L/min at flow
2) under protection, be warming up to 1300 DEG C with the speed of 5 DEG C/min, and be incubated 3h, obtain ordered porous SiC nano fiber.
The SEM photo of the prepared porous silicon carbide nanofiber of the present embodiment as shown in Figure 3.As seen from the figure, nanometer silicon carbide average fibre diameter is 200nm, and diameter is even, and fiber is loose structure, and fiber is arranged and formed ordered fiber along certain orientation.
Embodiment 3
The present embodiment comprises the following steps:
(1) preparation spinning solution: polyacrylonitrile powder is joined in DMF, and polyacrylonitrile powder and DMF mass ratio are 1.2: 10(is that the mass concentration of polyacrylonitrile is 10.7wt%), stir polyacrylonitrile is dissolved completely, be mixed with homogeneous phase spinning solution;
(2) electrostatic spinning: step (1) gained homogeneous phase spinning solution is carried out to electrostatic spinning, electrostatic spinning shower nozzle used is the metal needle of internal diameter 0.8mm, spinning voltage is 16kV, receiving range is 20cm, feeding rate is 15 μ l/min, 25 DEG C of spinning temperatures, relative air humidity 60RH%, adopt dull and stereotyped aluminium foil receiver, make nano polypropylene nitrile fibrillation;
(3) pre-oxidation is crosslinked: the polymer nanocomposite polyacrylonitrile fibrillation that step (2) is obtained is placed in oxidation furnace, heats up, and at 260 DEG C of insulation 1h with the speed of 3 DEG C/min, is not melted polyacrylonitrile fibre after being cooled to room temperature;
(4) high temperature burns till: the polyacrylonitrile fibre that do not melt that step (3) is obtained is placed in the high temperature furnace under inert gas (high-purity Ar of purity >=99.999%) protection, be warming up to 1000 DEG C with the speed of 5 DEG C/min, and be incubated 1h, obtain carbon nano-fiber;
(5) carbon thermal reduction: the carbon nano-fiber that step (4) is obtained and silica flour (silica flour and carbon nano-fiber mole for 3:1) are placed in corundum crucible; be under inert gas (high-purity Ar of the purity >=99.999%) protection of 0.2 L/min at flow; be warming up to 1500 DEG C with the speed of 5 DEG C/min; and be incubated 5h, obtain porous silicon carbide nanofiber.
The prepared porous silicon carbide nanofiber of the present embodiment average diameter is 206nm, and diameter is even, and fiber is loose structure.
Embodiment 4
The present embodiment comprises the following steps:
(1) preparation spinning solution: polyacrylonitrile powder is joined in DMF, and polyacrylonitrile powder and DMF mass ratio are 1.5: 10(is that the mass concentration of polyacrylonitrile is 13.0wt%), stir polyacrylonitrile is dissolved completely, be mixed with homogeneous phase spinning solution;
(2) electrostatic spinning: step (1) gained homogeneous phase spinning solution is carried out to electrostatic spinning, electrostatic spinning shower nozzle used is the metal needle that internal diameter size is 0.8mm, spinning voltage is 16kV, receiving range is 20cm, feeding rate is 10 μ l/min, 20 DEG C of spinning temperatures, relative air humidity 60RH%, adopt parallel pole as receiver, make orderly nano polypropylene nitrile fibrillation;
(3) pre-oxidation is crosslinked: the nano polypropylene nitrile fibrillation that step (2) is obtained is placed in oxidation furnace, heats up, and at 280 DEG C of insulation 1h with the speed of 5 DEG C/min, obtains orderly infusible polyacrylonitrile fibre after being cooled to room temperature;
(4) high temperature burns till: the fusion-free fibre that step (3) is obtained is placed in the high temperature furnace under inert gas inert gas (high-purity Ar of purity >=99.999%) protection, be warming up to 1400 DEG C with the speed of 3 DEG C/min, and be incubated 1h, obtain orderly carbon nano-fiber;
(5) carbon thermal reduction: the orderly carbon nano-fiber that step (4) is obtained and silica flour (mol ratio of silica flour and carbon fiber is 3:1) are placed in corundum crucible; be under inert gas (high-purity Ar of the purity >=99.999%) protection of 0.2 L/min at flow; be warming up to 1500 DEG C with the speed of 5 DEG C/min; and be incubated 6h, obtain ordered porous SiC nano fiber.
The prepared porous silicon carbide nanofiber of the present embodiment average diameter is 370nm, and diameter is evenly distributed, and fiber is loose structure, and fiber is arranged and formed ordered fiber along certain orientation.
Claims (10)
1. a preparation method for porous silicon carbide nanofiber, is characterized in that, comprises the following steps:
(1) preparation spinning solution: carbon nano-fiber precursor polymer is dissolved in solvent and is mixed with homogeneous phase spinning solution, and the concentration of described carbon nano-fiber precursor polymer in homogeneous phase spinning solution is 5wt% ~ 50wt%;
(2) electrostatic spinning: step (1) gained homogeneous phase spinning solution is carried out to electrostatic spinning, electrostatic spinning shower nozzle used is that internal diameter size is the metal needle of 0.5 ~ 1.5mm, spinning voltage 12 kV ~ 30kV, receiving range 15 ~ 25cm, feeding rate 5 ~ 30 μ 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 refinement gradually, solvent evaporates simultaneously, forms polymer nanofiber and is collected on receiver;
(3) pre-oxidation is crosslinked: the polymer nanofiber that step (2) is obtained is placed in oxidation furnace, is warming up to 200 ~ 300 DEG C with the heating rate of 0.1 ~ 10 DEG C/min, and insulation 0.5 ~ 5h, carries out pre-oxidation crosslinked, is not melted nanofiber after being cooled to room temperature;
(4) high temperature burns till: what step (3) was obtained does not melt nanofiber 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) is obtained is put into corundum crucible together with silica flour, be under the inert atmosphere protection of 0.1 ~ 1.0 L/min at flow, be heated 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 greater than 1:1.
2. the preparation method of porous silicon carbide nanofiber according to claim 1, is characterized in that, in step (1), described carbon nano-fiber precursor polymer is at least one in polyacrylonitrile, phenolic resins, pitch.
3. the preparation method of porous silicon carbide nanofiber according to claim 1 and 2, is characterized in that, in step (1), described solvent is dimethyl formamide or dimethyl sulfoxide (DMSO).
4. the preparation method of porous silicon carbide nanofiber according to claim 1 and 2, is characterized in that, in step (2), described receiver is dull and stereotyped aluminium foil or parallel pole.
5. the preparation method of porous silicon carbide nanofiber according to claim 1 and 2, is characterized 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, is characterized 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, is characterized in that, in step (4) and step (5), and the high-purity argon gas that described inert atmosphere is purity >=99.999% or high pure nitrogen.
8. the preparation method of porous silicon carbide nanofiber according to claim 1 and 2, is characterized in that, in step (4), will not melt nanofiber under inert atmosphere protection, is warmed up to 1000 ~ 1800 DEG C.
9. the preparation method of porous silicon carbide nanofiber according to claim 8, is characterized in that, in step (4), will not melt nanofiber under inert atmosphere protection, is warmed up to 1400 ~ 1600 DEG C.
10. the preparation method of porous silicon carbide nanofiber according to claim 1 and 2, is characterized in that, in step (4), temperature retention time is 1 ~ 2h.
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