CN101195938A - Core-skin structure micropore silicon carbide fiber and method for producing the same - Google Patents
Core-skin structure micropore silicon carbide fiber and method for producing the same Download PDFInfo
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Abstract
The invention relates to skin-core structure micro-pore silicon carbide fiber and the preparation method, the fiber is characterized in that both the skin layer and the core part contain the micro-pore with pore diameter less than 2 nm, and the micro-pore volume content of the skin is higher than the core part; the ratio between the skin layer thickness and the radius is 0.1 to 0.9; according to the differences of the skin thickness, the specific surface area of the fiber is 400m<2>/g to 1400m<2>/g, and the average pore diameter is 1.30 to 1.60 nm; the C content of the skin layer is more than 90 wt percent, the residual is Si, or Si and O; the C content of the core part is 27 to 35 wt percent, the O content is 10 to 20 wt percent, and the residual is Si. The preparation method is characterized in that the Si element of the skin layer is etched through the KOH activation method and the skin-core structure is formed, simultaneously, the micro-pore with higher proportion is formed, the specific surface area and the conducting property of the fiber can be adjusted through the method. The skin-core structure micro-pore silicon carbide fiber of the invention can be used in the physico chemical adsorption field, catalyst carrier field, and wave-absorbed stealth field.
Description
Technical field
The present invention relates to a kind of silicon carbide fibre and preparation method thereof, particularly relate to a kind of micro-pore silicon carbide fiber and preparation method thereof with skin-core structure.
Background technology
Carborundum (SiC) fiber has advantages such as high strength, high temperature resistant, anti-oxidant, resistance to chemical attack and high temperature creep-resisting.Continuous SiC fiber plays the purpose that improves intensity and toughness mainly as the enhancing body of refractory ceramics based composites (CMC), is the crucial raw material in fields such as Aero-Space, national defence weapon equipment and ceramic engine.In addition, because characteristics such as outstanding chemical inertness and semiconductors, continuous SiC fiber has outstanding application prospect in fields such as nuclear radiation parts, chemical device, radar invisible structures.
In addition, if introduce the porous SiC fiber that hole forms, then more wide application prospect is arranged in fields such as catalyst carrier, adsorption energy-storing, vehicle exhaust filtration, metal melt filtering, lightweight Radar Stealth Materials at the SiC fiber; If the SiC fiber is made skin-core structure, regulate the composition of core-skin, will give the SiC fiber more wide purposes again.
The method for preparing at present the SiC fiber comprises chemical vapor deposition (CVD) method (US Patent 3433725), powder sintering (US Patent 4908340,1990), precursor conversion method (Chemical Letters, 1975:931), chemical gas-phase reaction method (CVR) (JP Patent 58/91823,1983; JP Patent55/085472,1980) etc., wherein the fiber that makes of CVD method is to be that core, SiC are the core-skin composite fiber of skin with C fiber or W silk, and mechanical property is better, and diameter is thicker, the compact structure imporosity; The SiC fiber porosity of powder sintering preparation is higher, be in mesoporous scope (～10-100nm), mechanical property is relatively poor; The SiC fibrous mechanical property of Stainless Steel via Precursor Pyrolysis is good, fibre diameter is thin, stitchability good, and (Journal of Material Science, 1990:2118), but these micropores are closed pores, the very low (＜1m of fiber specific surface area a spot of micropore
2/ g), mainly be external surface area, and do not have skin-core structure; Chemical gas-phase reaction method is had and the similar pore character of active C fiber, but is not had skin-core structure by active C fiber Siization.
Disclosing for Chinese patent ZL02140433.X number a kind of is that C, core are the fiber with skin-core structure of SiC by bi-component spinning method preserved skin floor, but this method purpose is final oxidation and removes the SiC fiber that top layer C obtains continuous sintering, with powder sintering (US Patent 4908340,1990) similar, can not obtain microporous fibre.
In addition, utilize chlorine that the Si element etching of SiC fiber surface is removed, can form cortex and be micropore (＜2nm) C, core are SiC fiber (Nature Material, the 1994:628 with skin-core structure of fine and close SiC; Ceramic Engineering and Science Proceedings, 1998:87), but this method efficient is very low, be difficult to obtain thicker cortex, and only to be fit to surface is the fiber of pure SiC, and is inapplicable for the SiC fiber of top layer richness C.
Summary of the invention
The purpose of this invention is to provide the rich C of a kind of cortex, core and be SiC and cortex and core and all be rich in core-skin structure micropore silicon carbide fiber of micropore and preparation method thereof.
The cortex of the present invention's core-skin structure micropore silicon carbide fiber and core all contain the micropore of aperture＜2nm, and cortex micro pore volume content is higher than core; Skin thickness is 0.1-0.9 with the ratio of radius; Fiber specific surface area according to the difference of skin thickness, is 400m
2/ g-1400m
2/ g, average pore size is 1.30-1.60nm; Cortex C content＞90wt%, surplus is Si, perhaps Si and O; Core C content is 27-35wt%, and O content is 10-20wt%, and surplus is Si.
The preparation method of the present invention's core-skin structure micropore type silicon carbide fibre may further comprise the steps:
(1) polycarbosilane precusor is placed melt spinning device, be heated under the protection of the high pure nitrogen of purity 〉=99% after 230-340 ℃ (preferred 260-300 ℃) carry out deaeration and handle, at 200-300 ℃ (preferred 250-270 ℃), (0.2-1.2MPa preferred 0.4-0.6MPa), carry out melt spinning with 40-200m/min (preferred 80-150m/min) speed, make the fibrillation that diameter is 10-20 μ m;
(2) described fibrillation is placed oxidation furnace, the programming rate by 10-30 ℃/h in air is heated to 160-230 ℃ (preferred 190-210 ℃), and insulation oxidation processes 1-10 hour obtains fusion-free fibre;
(3) described fusion-free fibre is placed the high temperature furnace of the nitrogen protection of purity 〉=99%, programming rate with 10-20 ℃/min is warming up to 400-1200 ℃, 50-70 minute (preferred 60 minutes) are handled in the insulation cracking under this temperature, and making diameter is the cracking fiber of 9-18 μ m;
(4) described cracking fiber is placed KOH saturated solution soaking at room temperature 3-20h (preferred 10-15h), oven dry is placed on N
2In the high temperature furnace of protection, be warming up to 700-1100 ℃ (preferred 800-900 ℃, more excellent is 850 ℃) with the programming rate of 10-20 ℃/min, and after activation processing 0.2-15 under this temperature hour, make the activation silicon carbide fibre;
(5) described activation silicon carbide fibre is soaked 1-5h with watery hydrochloric acid, water flushing then is neutral up to pH, and oven dry promptly gets core-skin structure micropore type silicon carbide fibre.
All there are micropore in the cortex and the core of the present invention's core-skin structure micropore type silicon carbide fibre, and average pore size is 1.30-1.60nm, can be widely used in fields such as physical and chemical adsorption, catalyst carrier and wave-absorbing and camouflage.
The present invention's preparation method can realize the adjusting of skin thickness and micro pore volume reserves and specific area, has organic coating, SiO for the surface
2The continuous SiC fiber of coating, C coating all can obtain skin-core structure, is much better than the chlorine removal method; And the inventive method can be regulated the specific area and the conductive characteristic of continuous SiC fiber according to application need.
Description of drawings
Fig. 1 is the core-skin microscopic appearance figure of the silicon carbide fibre of embodiment 1 preparation;
Fig. 2 is the core-skin microscopic appearance figure of the silicon carbide fibre of embodiment 2 preparations.
The specific embodiment
Below in conjunction with embodiment the present invention is further described, but these embodiment must not be interpreted as limiting the scope of the invention.
Below the preparation method of the used raw material Polycarbosilane (PCS) of each embodiment referring to Chinese patent ZL200410023185.4.
The silicon carbide fibre microscopic appearance of present embodiment as shown in Figure 1, specific area is 1100m
2/ g, average pore size is 1.42nm, skin thickness is 4.8 μ m, with the ratio of radius be 0.80, the content that energy spectrum analysis obtains cortex C, Si, O is respectively 94wt%, 1wt%, 5wt%, the content of core C, Si, O is respectively 30wt%, 55wt%, 15wt%.The resistivity of fiber is 3 * 10
-2Ω cm.
Preparation: (1) is got 10g PCS and is placed melt spinning device, be heated under the protection of the high pure nitrogen of purity 〉=99% 290 ℃ and carry out deaeration and handle after, at 260 ℃, under the 0.5MPa pressure, carry out melt spinning with 120m/min speed, making diameter is 15 μ m precursor; (2) precursor is placed oxidation furnace, be heated to 200 ℃ with 15 ℃/h programming rate in air atmosphere, insulation was handled 2 hours, obtained the fusion-free fibre that oxygen content is 16wt%; (3) fusion-free fibre being placed high temperature furnace, is under the protection of 〉=99% high pure nitrogen in purity, is warming up to 800 ℃ with the programming rate of 10 ℃/min, and insulation was handled 60 minutes, and making diameter is 12 μ m cracking fibers; (4) the cracking fiber is soaked 10h with the KOH saturated solution, oven dry places high temperature furnace, is warming up to 850 ℃ with the programming rate of 10 ℃/min, after 9 hours, makes the activation silicon carbide fibre in activation processing under this temperature; (5) will activate silicon carbide fibre and soak 3h with watery hydrochloric acid, water flushing then is neutral up to pH, oven dry.
Embodiment 2
The silicon carbide fibre microscopic appearance of present embodiment as shown in Figure 2, specific area is 510m
2/ g, average pore size is 1.35nm, skin thickness is 0.6 μ m, with the ratio of radius be 0.10, the content that energy spectrum analysis obtains cortex C, Si, O is respectively 92wt%, 3wt%, 5wt%, the content of core C, Si, O is respectively 30wt%, 55wt%, 15wt%.The resistivity of fiber is 10 Ω cm.
Preparation: (4) the activation processing time in step of present embodiment is 0.5h, and all the other are with embodiment 1.
Embodiment 3
The silicon carbide fibre specific area of present embodiment is 1400m
2/ g, average pore size is 1.55nm, and skin thickness is about 5.4 μ m, with the ratio of radius be 0.90, the content that energy spectrum analysis obtains cortex C, Si, O is respectively 96wt%, 0wt%, 4wt%, and the content of core C, Si, O is respectively 31wt%, 54wt%, 15wt%.The resistivity of fiber is 5 * 10
-3Ω cm.
Preparation: in (4) step of present embodiment, the activation processing time is 15h, and all the other are with embodiment 1.
Embodiment 4
The silicon carbide fibre specific area of present embodiment is 1200m
2/ g, average pore size is 1.40nm, and skin thickness is about 5.5 μ m, is about 0.90 with the ratio of radius, the content that energy spectrum analysis obtains cortex C, Si, O is respectively 95wt%, 1wt%, 4wt%, and the content of core C, Si, O is respectively 35wt%, 50wt%, 15wt%.The resistivity of fiber is 6 * 10
-3Ω cm.
Preparation: in (3) step of present embodiment, the cracking temperature of fusion-free fibre is 400 ℃, and all the other are with embodiment 1.
Embodiment 5
The silicon carbide fibre specific area of present embodiment is 1010m
2/ g, average pore size is 1.41nm, and skin thickness is about 4.5 μ m, is about 0.75 with the ratio of radius, the content that energy spectrum analysis obtains cortex C, Si, O is respectively 94wt%, 1wt%, 5wt%, and the content of core C, Si, O is respectively 30wt%, 56wt%, 14wt%.The resistivity of fiber is 9 * 10
-2Ω cm.
Preparation: in (3) step of present embodiment, the cracking temperature of fusion-free fibre is 1200 ℃, and all the other are with embodiment 1.
Embodiment 6
The silicon carbide fibre specific area of present embodiment is 1150m
2/ g, average pore size is 1.45nm, skin thickness is 4.8 μ m, with the ratio of radius be 0.80, the content that energy spectrum analysis obtains cortex C, Si, O is respectively 98wt%, 2wt%, 0wt%, the content of core C, Si, O is respectively 32wt%, 55wt%, 13wt%.The resistivity of fiber is 1 * 10
-2Ω cm.
Preparation: in (2) step of present embodiment, precursor is heated to 190 ℃ with 10 ℃/h programming rate in air atmosphere, and insulation was handled 5 hours, obtained the fusion-free fibre that oxygen content is 12wt%, and all the other are with embodiment 1.
Embodiment 7
The silicon carbide fibre specific area of present embodiment is 1020m
2/ g, average pore size is 1.44nm, skin thickness is 4.8 μ m, with the ratio of radius be 0.82, the content that energy spectrum analysis obtains cortex C, Si, O is respectively 92wt%, 1wt%, 6wt%, the content of core C, Si, O is respectively 30wt%, 52wt%, 18wt%.The resistivity of fiber is 6 * 10
-2Ω cm.
Preparation: in (2) step of present embodiment, precursor is heated to 210 ℃ with 10 ℃/h programming rate in air atmosphere, and insulation was handled 8 hours, obtained the fusion-free fibre that oxygen content is 19wt%, and all the other are with embodiment 1.
Embodiment 8
The silicon carbide fibre specific area of present embodiment is 1160m
2/ g, average pore size is 1.46nm, skin thickness is 4.8 μ m, with the ratio of radius be 0.60, the content that energy spectrum analysis obtains cortex C, Si, O is respectively 94wt%, 1wt%, 5wt%, the content of core C, Si, O is respectively 30wt%, 55wt%, 15wt%.The resistivity of fiber is 3 * 10
-2Ω cm.
Preparation: (1) step of present embodiment, at 250 ℃, under the 0.6MPa pressure, carry out melt spinning with 80m/min speed, making diameter is 20 μ m precursor, all the other are with embodiment 1.
Reference examples 1
Get 10g PCS and place melt spinning device, purity be heated under for the protection of 〉=99% high pure nitrogen 290 ℃ and carry out deaeration and handle after, at 260 ℃, under the 0.5MPa, carry out melt spinning with 120m/min speed, diameter be 15 μ m precursor; Precursor is placed oxidation furnace, be heated to 200 ℃ with 15 ℃/h in air atmosphere, insulation was handled 2 hours, and oxygen content is 16wt%; Fusion-free fibre is placed high temperature furnace, and the programming rate with 10 ℃/min under the high pure nitrogen protection of purity 〉=99% is warming up to 800 ℃, and insulation was handled 1 hour, and making diameter is 12 μ m cracking fibers.
The silicon carbide fibre specific area of this reference examples is 0.28m
2/ g, no skin-core structure, the content that energy spectrum analysis obtains C, Si, O is respectively 27wt%, 57wt%, 16wt%.The resistivity of fiber is 8 * 10
2Ω cm.
Claims (7)
1. a core-skin structure micropore silicon carbide fiber is characterized in that, cortex and core all contain the micropore of aperture＜2nm, and cortex micro pore volume content is higher than core; Skin thickness is 0.1-0.9 with the ratio of radius; Fiber specific surface area according to the difference of skin thickness, is 400m
2/ g-1400m
2/ g, average pore size is 1.30-1.60nm; Cortex C content＞90wt%, surplus is Si, perhaps Si and O; Core C content is 27-35wt%, and O content is 10-20wt%, and surplus is Si.
2. the preparation method of core-skin structure micropore type silicon carbide fibre according to claim 1 is characterized in that, may further comprise the steps:
(1) polycarbosilane precusor is placed melt spinning device, be heated under the protection of the high pure nitrogen of purity 〉=99% 230-340 ℃ carry out deaeration and handle after, at 200-300 ℃, 0.2-1.2MPa, carry out melt spinning with 40-200m/min speed, make the fibrillation that diameter is 10-20 μ m;
(2) described fibrillation is placed oxidation furnace, the programming rate by 10-30 ℃/h in air is heated to 160-230 ℃, and insulation oxidation processes 1-10 hour obtains fusion-free fibre;
(3) described fusion-free fibre is placed the high temperature furnace of the high pure nitrogen protection of purity 〉=99%, be warming up to 400-1200 ℃ with the programming rate of 10-20 ℃/min, the insulation cracking was handled 50-70 minute under this temperature, and making diameter is the cracking fiber of 9-18 μ m.
(4) described cracking fiber is placed KOH saturated solution soaking at room temperature 3-20h, oven dry is placed in the high temperature furnace of N2 protection, programming rate with 10-20 ℃/min is warming up to 700-1100 ℃, and makes the activation silicon carbide fibre after activation processing 0.2-15 under this temperature hour;
(5) described activation silicon carbide fibre is soaked 1-5h with watery hydrochloric acid, water flushing then is neutral up to pH, oven dry.
3. as the preparation method of core-skin structure micropore type silicon carbide fibre as described in the claim 2; it is characterized in that; described (1) step; under the nitrogen protection of purity 〉=99%, be heated to 260-300 ℃ and carry out the deaeration processing; at 250-270 ℃; 0.4-0.6MPa, carry out melt spinning with 80-150m/min speed.
4. as the preparation method of core-skin structure micropore type silicon carbide fibre as described in claim 2 or 3, it is characterized in that in described (2) step, described fibrillation insulation oxidation temperature is 190-210 ℃.
5. as the preparation method of core-skin structure micropore type silicon carbide fibre as described in claim 2 or 3, it is characterized in that in described (3) step, the insulation cracking processing time is 60 minutes.
6. as the preparation method of core-skin structure micropore type silicon carbide fibre as described in claim 2 or 3, it is characterized in that in described (4) step, cracking fiber soaking at room temperature time in the KOH saturated solution is 10-15h, activating treatment temperature is 800-900 ℃.
7. as the preparation method of core-skin structure micropore type silicon carbide fibre as described in the claim 6, it is characterized in that described activating treatment temperature is 850 ℃.
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| CN102392326B (en) * | 2011-10-10 | 2013-07-31 | 中国人民解放军国防科学技术大学 | Axial gradient silicon carbide fibers and preparation method and device thereof |
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| CN103575754B (en) * | 2012-07-20 | 2017-12-29 | 中国科学院宁波材料技术与工程研究所 | A kind of assay method of carbon fiber oxidization fiber skin-core structure |
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| CN108218435A (en) * | 2018-01-16 | 2018-06-29 | 贵州师范大学 | A kind of preparation method of skin-core structure silicon carbide ceramic fiber |
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| US11951729B2 (en) | 2018-08-23 | 2024-04-09 | Nitto Denko Corporation | Laminated sheet |
| CN109851363A (en) * | 2019-01-31 | 2019-06-07 | 中南大学 | A kind of fiber of SiC containing heterogeneous element with graded interface layer and preparation method thereof and equipment |
| CN109851363B (en) * | 2019-01-31 | 2021-08-27 | 中南大学 | Heterogeneous element-containing SiC fiber with gradient interface layer and preparation method and equipment thereof |
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