CN105603578A - Method for preparing high-specific-surface-area continuous SiO2 porous fiber through natural drying method - Google Patents
Method for preparing high-specific-surface-area continuous SiO2 porous fiber through natural drying method Download PDFInfo
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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Abstract
The invention relates to a method for preparing high-specific-surface-area continuous SiO2 porous fiber through a natural drying method. The method includes the steps of preparing a spinning solution from silicate or silanol sol, adding the spinning solution to an acid solution coagulating bath, conducting reaction and wet spinning to obtain orthosilicic acid/silicate fiber, winding the orthosilicic acid/silicate fiber, ageing the orthosilicic acid/silicate fiber at the normal temperature, washing the orthosilicic acid/silicate fiber with deionized water to be neutral, conducting solvent replacement through ethyl alcohol, and conducting natural drying. The method has the advantages that devices are simple, raw materials are low in price and easy to obtain, the reaction process is simple and spinnability is good, the problem that inorganic porous fiber can hardly be spun into fiber is solved, and meanwhile drying of the porous fiber is achieved through natural drying. The prepared SiO2 porous fiber has abundant pores, an ultrahigh specific surface area, high temperature resistance and chemical corrosion resistance, the specific surface area of the fiber can be adjusted, and the method can be used for the fields of catalyst carriers, adsorption filtration and the like.
Description
Technical field
The invention belongs to the preparation field of porous fibre, particularly a kind of natural seasoning is prepared the continuous SiO of high-specific surface area2ManyThe method of hole fiber.
Background technology
Porous material has high-specific surface area, and a large amount of reaction/interaction activated centres can be provided, and is particularly conducive to and interfaceAct on relevant process, for example absorption, catalysis and electrochemical action; Its duct can be used as multi-functional memory and monodispersed receivingRice reactor; The nano pore that it is special and the research that is shaped as cross discipline have brought and abundant space and place, for exampleDispersal behavior in nano pore of biomolecule, drug molecule, reactant molecule, with the contact performance in activated centre, reactActive grade all has close relationship with pore structure; And the skin effect that the network structure of its nanoscale is brought and quantum size effectShould, make some functional porous materials in sensor, lithium battery and nano-device, show excellent performance; Porous material justThe unique advantage of material on micro interface, makes them become one of the focus in investigation of materials field.
The performance of porous material, except relevant with its microscopic appearance, also has important relationship with composite porous macro morphology.For SiO2Porous material, nowadays existing a large amount of bibliographical information zero dimension powder, two-dimensional film, three-dimensional block, but to oneThe SiO of dimension2Porous fibre is but seldom reported. This is mainly the porous material because of other dimensions of comparing, fibrous porous materialThere is to more requirement the aspect such as raw materials, preparation condition. But fibrous porous material but has other dimension material instituteThe excellent properties not possessing. Analogy is similarly the porous active carbon fiber of inorganic porous fiber, and traditional active carbon is a kind of processThe porous charcoal of activation processing, is Powdered or graininess, and activated carbon fiber is fibrous, is covered with micropore on fiber, and it is rightOrganic gas adsorption capacity is higher several times to tens times in air than granular activated carbon, high 5～6 times in the aqueous solution, the rate of adsorptionFast 100～1000 times. The fibre diameter of activated carbon fiber is 5～20 μ m, and specific area is on average at 1000～1500m2/ g left and right,Average pore size is at 1.0～4.0nm, and micropore is uniformly distributed in fiber surface. Compared with active carbon, activated carbon fiber micropore size is littleAnd evenly, simple in structure, fast for the absorption small-molecule substance rate of adsorption, adsorption rate is high, easily desorption. Be adsorbedThe contact area of thing is large, and can even contact and absorption, and sorbing material is fully utilized. Efficiency is high, and have fiber,The various very thin statements such as felt, cloth and paper, the direct opening of hole is at fiber surface, and its adsorbate arrives the evolving path of adsorption potentialShort, and the external surface area of itself exceeds two orders of magnitude compared with internal surface area. Aspect air or water body purification, granular or powderyStructure, easily occurs stackingly, and its adsorption rate is slower, and separative efficiency is not high, and particularly its physical aspect has in the time of applicationMuch inconvenience, has limited range of application. Little and the narrowly distributing in NACF aperture, adsorption rate is fast, and adsorbance is large, easily againRaw. Compared with powdery (5nm～30nm) active carbon, the micro mist dirt that NACF in use produces is few, can be made into yarn,The goods of the variforms such as line, fabric, felt, more flexible when use. And block or membranaceous structure, make air orWater body by time can produce very large resistance, filter before with filter after pressure differ greatly. By SiO2Porous material is made fiber shapeState, will make its performance more excellent.
Bibliographical information is prepared SiO at present2The method of porous fibre has chemical synthesis, template, centrifugal spinning, but these sidesMethod all can not be prepared continuous single long fibre.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of natural seasoning and prepares the continuous SiO of high-specific surface area2Porous fibreMethod, the method has that equipment is simple, raw material is cheaply easy to get, course of reaction is simple, the feature of good spinnability; Prepared nothingMachine SiO2Fiber has the specific area of abundant hole, superelevation, high temperature resistant, resistance to chemical attack, and pulp freeness can simultaneouslyAdjust.
A kind of natural seasoning of the present invention is prepared the continuous SiO of high-specific surface area2The method of porous fibre, comprising:
(1) silicate or silanol colloidal sol are mixed with to spinning solution;
(2) in coagulating basin, add acid solution as coagulating bath;
(3) spinning solution in step (1) is joined in the coagulating bath in step (2), react wet spinning,To orthosilicic acid/silicate fiber; Spinning solution runs into coagulating bath acid the generation of strong acid weak acid reaction processed fast solid phase orthosilicic acid occurs,Realize the desired quick liquid-solid phase of wet spinning and change, form orthosilicic acid/silicate fiber, there is collosol and gel in this process simultaneouslyChange;
(4) orthosilicic acid in step (3)/silicate fiber is reeled, then immerses in ageing solution normal temperature ageing 2～10 days,Then with deionized water washing to neutral, carry out solvent exchange with ethanol, natural drying, obtain the continuous SiO of high-specific surface area2ManyHole fiber; Ageing makes orthosilicic acid/silicate fiber that collosol and gel further occur, and realizes by orthosilicic acid/silicate fiber to SiO2Fiber changes, and forms a large amount of holes simultaneously.
Described step (1) mesosilicic acid salt is sodium silicate, KP1 or nine water sodium metasilicate; Silanol colloidal sol be ethyl orthosilicate,MTES, MTMS or the phenyltrimethoxysila,e hydrolytic sol under diluted acid condition.
The specification of spinning solution in described step (1): the modulus of sodium silicate, KP1 is 2～3, and Baume degrees is 35～50,Nine water sodium metasilicate are directly heated into solution without solubilizer again, and the viscosity of silanol colloidal sol is 0.01～0.1PaS, and silicone content is greater than 10wt％。
Acid solution is that concentration is that dilution heat of sulfuric acid, the concentration of 0.2mol/L～0.4mol/L is 0.4 in described step (2)The dilute hydrochloric acid solution of mol/L～0.8mol/L or concentration are the acetic acid of 12mol/L～15mol/L.
In described step (3), the condition of reaction wet spinning is normal temperature and pressure.
The speed of reeling in described step (4) is 0.1～2m/s.
Ageing solution is low concentration acid solution in described step (4): dilution heat of sulfuric acid that concentration is 0.005mol/L～0.1mol/L,Concentration is the dilute hydrochloric acid solution of 0.01mol/L～0.2mol/L or the oxalic acid that concentration is 0.005mol/L～0.1mol/L.
The continuous SiO of high-specific surface area prepared by natural seasoning of the present invention2The hole of porous fibre is in nanoscale scope, and canTo regulate specific surface area size by changing preparation condition.
The present invention utilizes strong acid weak acid processed and collosol and gel principle, realizes continuous SiO by reaction spinning2The preparation of porous fibre.
This patent utilizes strong acid weak acid processed and collosol and gel principle, realizes continuous SiO by reaction spinning2The preparation of porous fibre,The method, without document patent report, has novelty. Prepared continuous SiO2Porous fibre is in catalysis, absorption, sensing etc.Series has more outstanding advantage in field, has very huge potential demand, has practicality. In addition, high-specific surface areaWhen porous silica material is dry, in order to keep hole pattern and high-specific surface area, often need to use freeze drying, overcriticalThe special drying mode such as dry, and this method only needs simple natural dryingly just can realize.
Continuous SiO in the present invention2The preparation method of porous fibre, is using cheap silicate and silanol colloidal sol as spinning solution,Using different acid solutions as coagulating bath, react and colloidal sol occurs with acid generation strong acid weak acid processed by silicate and silanol colloidal sol and coagulateGel, part generates the orthosilicic acid of solid phase, obtains orthosilicic acid/silicate fiber, by take up roll, fiber is carried out to rolling. Subsequently,Orthosilicic acid/the silicate fiber of rolling is immersed in low concentration acid solution and carries out ageing, make fiber further by ageing processCarry out collosol and gel, realize by orthosilicic acid/silicate fiber to SiO2Fiber changes, and forms a large amount of holes simultaneously. After ageing,Use deionized water to wash, then use ethanol to carry out solvent exchange, the last natural drying final SiO continuously that obtains2PorousFiber. Method used in the present invention has that equipment is simple, raw material is cheaply easy to get, course of reaction is simple, the feature of good spinnability,Solve the difficult problem that inorganic porous fiber is difficult to spin fibroblast, simultaneously with natural drying the dry of porous fibre of just realizing. ObtainedInorganic SiO2Porous fibre has the specific area of abundant hole, superelevation, high temperature resistant, resistance to chemical attack, simultaneously fiber ratioSurface area is adjustable, can be used for the fields such as catalyst carrier field and adsorption filtration.
Beneficial effect
(1) method of the present invention has that equipment is simple, raw material is cheaply easy to get, course of reaction is simple, the feature of good spinnability, solvesInorganic porous fiber be difficult to spin the difficult problem of fibroblast, simultaneously with natural drying the dry of porous fibre of just realizing;
(2) inorganic SiO of the present invention2Porous fibre have abundant hole, superelevation specific area, high temperature resistant, chemically-resistant is rottenErosion, pulp freeness is adjustable simultaneously, can be used for the fields such as catalyst carrier field and adsorption filtration.
Brief description of the drawings
Fig. 1 is SiO in embodiment 12The microscope figure of porous fibre pattern;
Fig. 2 is SiO in embodiment 22The scanning electron microscope (SEM) photograph of porous fibre pattern;
Fig. 3 is SiO in embodiment 32Porous fibre inner void pattern scanning electron microscope (SEM) photograph;
Fig. 4 is SiO in embodiment 42Porous fibre N2The attached isollaothermic chart of absorption desorption;
Fig. 5 is SiO in embodiment 52After porous fibre absorption methylene blue different time, methylene blue solution characteristic ultraviolet absorption peak becomesChange figure.
Detailed description of the invention
Below in conjunction with specific embodiment, further set forth the present invention. Should be understood that these embodiment are not only for the present invention is describedBe used for limiting the scope of the invention. In addition should be understood that those skilled in the art can after having read the content of the present invention's instructionSo that the present invention is made various changes or modifications, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
Sodium silicate taking modulus as 2,50 Baume degrees is for spinning solution, taking the dilution heat of sulfuric acid of 0.4mol/L as coagulating bath, entersRow reaction wet spinning. Orthosilicic acid/the silicate fiber forming in coagulating bath is reeled with the winding speed of 0.1m/s. VolumeAround after fiber immerse the dilute sulfuric acid of 0.005mol/L and within 10 days, carry out ageing, realize by orthosilicic acid/silicate fiber to SiO2FiberChange, form a large amount of holes simultaneously. After ageing, fiber is washed by deionized water, until neutral. The displacement of use absolute ethyl alcoholSolution in fiber, is drying to obtain SiO under field conditions (factors)2Porous fibre. Very smooth and easy in spinning process, not fracture of wire. MakeSiO2Porous fibre specific area is 449.1m2/ g, most probable aperture is 10nm, 5min can reach absorption methylene blue60% of maximal absorptive capacity. The SiO making2The microscope figure of porous fibre pattern as shown in Figure 1; The SiO making2Porous fibreThe scanning electron microscope (SEM) photograph of dimension pattern as shown in Figure 2; The SiO making2Porous fibre inner void pattern scanning electron microscope (SEM) photograph as shown in Figure 3;The SiO making2Porous fibre N2The attached isollaothermic chart of absorption desorption as shown in Figure 4; The SiO making2Porous fibre absorption methyleneAfter blue different time, methylene blue solution characteristic ultraviolet absorption peak variation diagram as shown in Figure 5.
Embodiment 2
KP1 taking modulus as 3,35 Baume degrees is for spinning solution, taking the dilution heat of sulfuric acid of 0.2mol/L as coagulating bath, entersRow reaction wet spinning. Orthosilicic acid/sodium metasilicate the fiber forming in coagulating bath is reeled with the winding speed of 0.5m/s. VolumeAround after fiber immerse the dilute sulfuric acid of 0.005mol/L and within 10 days, carry out ageing, realize by orthosilicic acid/silicate fiber to SiO2FiberChange, form a large amount of holes simultaneously. After ageing, fiber is washed by deionized water, until neutral. The displacement of use absolute ethyl alcoholSolution in fiber, is drying to obtain SiO under field conditions (factors)2Porous fibre. In spinning process, there is once in a while fracture of wire phenomenon. MakeSiO2Porous fibre specific area is 335.1m2/ g, most probable aperture is 12nm, 5min can reach absorption methylene blue48% of large adsorbance.
Embodiment 3
KP1 taking modulus as 3,35 Baume degrees is for spinning solution, taking the dilution heat of sulfuric acid of 0.4mol/L as coagulating bath, entersRow reaction wet spinning. Orthosilicic acid/potassium silicate the fiber forming in coagulating bath is reeled with the winding speed of 1m/s. ReelAfter fiber immerse the dilute sulfuric acid of 0.1mol/L and within 5 days, carry out ageing, realize by orthosilicic acid/silicate fiber to SiO2Fiber changes,Form a large amount of holes simultaneously. After ageing, fiber is washed by deionized water, until neutral. Use in absolute ethyl alcohol displacement fiberSolution, be drying to obtain under field conditions (factors) SiO2Porous fibre. In spinning process, there is once in a while fracture of wire phenomenon. The SiO making2Porous fibre specific area is 350.2m2/ g, most probable aperture is 11nm, 5min can reach the maximum suction of absorption methylene blue51% of attached amount.
Embodiment 4
Taking nine water sodium metasilicate directly heat solution as spinning solution, taking the dilute hydrochloric acid solution of 0.4mol/L as coagulating bath, carry out anti-Answer wet spinning. Orthosilicic acid/the silicate fiber forming in coagulating bath is reeled with the winding speed of 2m/s. After coilingThe watery hydrochloric acid that fiber immerses 0.01mol/L carries out ageing for 10 days, realizes by orthosilicic acid/sodium metasilicate fiber to SiO2Fiber changes,Form a large amount of holes simultaneously. After ageing, fiber is washed by deionized water, until neutral. Use in absolute ethyl alcohol displacement fiberSolution, be drying to obtain under field conditions (factors) SiO2Porous fibre. In spinning process, often there is fracture of wire phenomenon. The SiO making2Porous fibre specific area is 202.2m2/ g, most probable aperture is 16nm, 5min can reach the maximum suction of absorption methylene blue32% of attached amount.
Embodiment 5
Taking nine water sodium metasilicate directly heat solution as spinning solution, taking the dilute hydrochloric acid solution of 0.8mol/L as coagulating bath, carry out anti-Answer wet spinning. Orthosilicic acid/the silicate fiber forming in coagulating bath is reeled with the winding speed of 1m/s. After coilingThe watery hydrochloric acid that fiber immerses 0.2mol/L carries out ageing for 2 days, realizes by orthosilicic acid/sodium metasilicate fiber to SiO2Fiber changes, withTime form a large amount of holes. After ageing, fiber is washed by deionized water, until neutral. Use in absolute ethyl alcohol displacement fiberSolution, is drying to obtain SiO under field conditions (factors)2Porous fibre. In spinning process, there is once in a while fracture of wire phenomenon. The SiO making2Porous fibre specific area is 228.4m2/ g, most probable aperture is 18nm, 5min can reach the maximum suction of absorption methylene blue38% of attached amount.
Embodiment 6
Add colloidal sol that watery hydrochloric acid is hydrolyzed into viscosity 0.01PaS, silicon content 12wt% as spinning solution, with 12 taking ethyl orthosilicateThe acetum of mol/L is coagulating bath, reacts wet spinning. By the orthosilicic acid/silicate fiber forming in coagulating bath with 1The winding speed of m/s is reeled. The oxalic acid that fiber after coiling immerses 0.005mol/L carries out ageing for 10 days, realizes by former siliconAcid fiber is to SiO2Fiber changes, and forms a large amount of holes simultaneously. After ageing, fiber is washed by deionized water, until neutral.Use the solution in absolute ethyl alcohol displacement fiber, be drying to obtain under field conditions (factors) SiO2Porous fibre. In spinning process, send out once in a whileRaw fracture of wire phenomenon. The SiO making2Porous fibre specific area is 352.3m2/ g, most probable aperture is 8nm, 5minReach 51% of absorption methylene blue maximal absorptive capacity.
Embodiment 7
Add colloidal sol that watery hydrochloric acid is hydrolyzed into viscosity 0.05PaS, silicon content 18wt% as spinning solution taking MTES,Taking the acetum of 15mol/L as coagulating bath, react wet spinning. By the orthosilicic acid/silicate fiber forming in coagulating bathWinding speed with 1m/s is reeled. The oxalic acid that fiber after coiling immerses 0.1mol/L carries out ageing for 5 days, realizes by formerSilicate fiber is to SiO2Fiber changes, and forms a large amount of holes simultaneously. After ageing, fiber is washed by deionized water, until neutral.Use the solution in absolute ethyl alcohol displacement fiber, be drying to obtain under field conditions (factors) SiO2Porous fibre. In spinning process, do not occurFracture of wire phenomenon. The SiO making2Porous fibre specific area is 520.7m2/ g, most probable aperture is 5nm, 5min can reachTo 64% of absorption methylene blue maximal absorptive capacity.
Embodiment 8
Add colloidal sol that watery hydrochloric acid is hydrolyzed into viscosity 0.1PaS, silicon content 22wt% as spinning solution taking MTMS,Taking the glacial acetic acid solution of 15mol/L as coagulating bath, react wet spinning. By the orthosilicic acid/silicate fibre forming in coagulating bathDimension is reeled with the winding speed of 1m/s. The oxalic acid that fiber after coiling immerses 0.1mol/L carries out ageing for 5 days, realize byOrthosilicic acid fiber is to SiO2Fiber changes, and forms a large amount of holes simultaneously. After ageing, fiber is washed by deionized water, until inProperty. Use the solution in absolute ethyl alcohol displacement fiber, be drying to obtain under field conditions (factors) SiO2Porous fibre. In spinning process notThere is fracture of wire phenomenon. The SiO making2Porous fibre specific area is 535.2m2/ g, most probable aperture is 6nm, 5min isCan reach 64% of absorption methylene blue maximal absorptive capacity.
Embodiment 9
Add colloidal sol that watery hydrochloric acid is hydrolyzed into viscosity 0.08PaS, silicon content 20wt% as spinning solution taking phenyltrimethoxysila,e,Taking the glacial acetic acid solution of 15mol/L as coagulating bath, react wet spinning. By the orthosilicic acid/silicate fibre forming in coagulating bathDimension is reeled with the winding speed of 1m/s. The oxalic acid that fiber after coiling immerses 0.1mol/L carries out ageing for 5 days, realize byOrthosilicic acid fiber is to SiO2Fiber changes, and forms a large amount of holes simultaneously. After ageing, fiber is washed by deionized water, until inProperty. Use the solution in absolute ethyl alcohol displacement fiber, be drying to obtain under field conditions (factors) SiO2Porous fibre. In spinning process notThere is fracture of wire phenomenon. The SiO making2Porous fibre specific area is 491.5m2/ g, most probable aperture is 4nm, 5min isCan reach 61% of absorption methylene blue maximal absorptive capacity.
Claims (7)
1. a natural seasoning is prepared the continuous SiO of high-specific surface area2The method of porous fibre, comprising:
(1) silicate or silanol colloidal sol are mixed with to spinning solution;
(2) in coagulating basin, add acid solution as coagulating bath;
(3) spinning solution in step (1) is joined in the coagulating bath in step (2), react wet spinning, obtainOrthosilicic acid/silicate fiber;
(4) orthosilicic acid in step (3)/silicate fiber is reeled, then immerses in ageing solution normal temperature ageing 2～10 days,Then with deionized water washing to neutral, carry out solvent exchange with ethanol, natural drying, obtain the continuous SiO of high-specific surface area2ManyHole fiber.
2. a kind of natural seasoning according to claim 1 is prepared the continuous SiO of high-specific surface area2The method of porous fibre, its spyLevy and be, described step (1) mesosilicic acid salt is sodium silicate, KP1 or nine water sodium metasilicate; Silanol colloidal sol is positive silicic acid secondEster, MTES, MTMS or the phenyltrimethoxysila,e hydrolytic sol under diluted acid condition.
3. a kind of natural seasoning according to claim 1 is prepared the continuous SiO of high-specific surface area2The method of porous fibre, its spyLevy and be, the specification of spinning solution in described step (1): the modulus of sodium silicate, KP1 is 2～3, and Baume degrees is 35～50,Nine water sodium metasilicate are directly heated into solution without solubilizer again, and the viscosity of silanol colloidal sol is 0.01～0.1PaS, and silicone content is greater than 10wt％。
4. a kind of natural seasoning according to claim 1 is prepared the continuous SiO of high-specific surface area2The method of porous fibre, its spyLevy and be, acid solution is that concentration is that dilution heat of sulfuric acid, the concentration of 0.2mol/L～0.4mol/L is 0.4 in described step (2)The dilute hydrochloric acid solution of mol/L～0.8mol/L or concentration are the acetic acid of 12mol/L～15mol/L.
5. a kind of natural seasoning according to claim 1 is prepared the continuous SiO of high-specific surface area2The method of porous fibre, its spyLevy and be, in described step (3), the condition of reaction wet spinning is normal temperature and pressure.
6. a kind of natural seasoning according to claim 1 is prepared the continuous SiO of high-specific surface area2The method of porous fibre, its spyLevy and be, the speed of reeling in described step (4) is 0.1～2m/s.
7. a kind of natural seasoning according to claim 1 is prepared the continuous SiO of high-specific surface area2The method of porous fibre, its spyLevy and be, ageing solution is that concentration is that dilution heat of sulfuric acid, the concentration of 0.005mol/L～0.1mol/L is in described step (4)The dilute hydrochloric acid solution of 0.01mol/L～0.2mol/L or concentration are the oxalic acid of 0.005mol/L～0.1mol/L.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1236832A (en) * | 1998-05-22 | 1999-12-01 | 中国科学院山西煤炭化学研究所 | Process for preparing Al2O3-SiO2 compound fibre |
| JP2000247677A (en) * | 1999-02-24 | 2000-09-12 | Nitto Boseki Co Ltd | Corrosion resistant glass fiber composition |
| CN1511786A (en) * | 2002-12-30 | 2004-07-14 | 中国科学院化学研究所 | Process for continuously preparing meso visual ordered hybridization silicon dioxide fiber |
| CN1556033A (en) * | 2004-01-08 | 2004-12-22 | 上海交通大学 | Preparation method of mesohole silicon dioxide fiber |
| CN101717258A (en) * | 2009-12-01 | 2010-06-02 | 西安交通大学 | Technology of preparing aluminium oxide based continuous fibers by sol-gel process |
-
2015
- 2015-12-31 CN CN201511029848.8A patent/CN105603578B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1236832A (en) * | 1998-05-22 | 1999-12-01 | 中国科学院山西煤炭化学研究所 | Process for preparing Al2O3-SiO2 compound fibre |
| JP2000247677A (en) * | 1999-02-24 | 2000-09-12 | Nitto Boseki Co Ltd | Corrosion resistant glass fiber composition |
| CN1511786A (en) * | 2002-12-30 | 2004-07-14 | 中国科学院化学研究所 | Process for continuously preparing meso visual ordered hybridization silicon dioxide fiber |
| CN1556033A (en) * | 2004-01-08 | 2004-12-22 | 上海交通大学 | Preparation method of mesohole silicon dioxide fiber |
| CN101717258A (en) * | 2009-12-01 | 2010-06-02 | 西安交通大学 | Technology of preparing aluminium oxide based continuous fibers by sol-gel process |
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