CN103614808A - Mullite fiber with villous whisker and preparation method thereof - Google Patents
Mullite fiber with villous whisker and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a mullite fiber with villous whisker and a preparation method thereof. The mullite fiber is characterized in that the surface of the fiber is distributed with radial whiskers, which grow, with central axis as origin, towards the outside of the fiber. The whiskers on the fiber surface are mullite monocrystal. The invention first employs a sol-gel method to prepare mullite fiber with good continuity; then the gel fibers, nano aluminum oxide powder, nano silicon oxide powder and a catalyst are sintered together in a closed container to 1150-1350 DEG C, so that the fibers are crystallized, and monocrystal mullite whiskers grow in a radial pattern on the surface. The invention has the advantages of simple preparation process, and the obtained fiber has unique structure and excellent performance, and is suitable for usage as a structure function integrated material.
Description
Technical field
The present invention relates to a kind of polycrystalline mullite fibre structure and preparation technology that composite strengthens the bigger serface of toughness reinforcing, skeleton or carrier material that can be used for.
Background technology
At SiO
2～Al
2o
3in binary system, mullite is the crystalline compound of unique stable existence.Mullite has the physical and chemical performance of many excellences.For example mullite has stronger thermal shock resistance.The mullite composite that the people such as Kaya strengthen with mullite fiber carries out after 300 cold cycling between 1150 ℃ and room temperature, and sample does not have obvious crackle, and its intensity is that the intensity of 201MPa(room temperature is 235MPa).Mullite also has higher elevated temperature strength, lower creep.The people such as Osendi study and find that mullite is 240MPa the bending strength of 1400 ℃, higher than its 230MPa when the room temperature.Its Young's modulus starts to have a small amount of reduction after 800 ℃, at 1400 ℃, is about 130GPa.Mullite also has lower thermal conductivity, and along with temperature increases, its thermal conductivity declines.Mullite is oxide ceramics, so it can be used as high-temperature structural ceramics and high-temperature refractory under aerobic conditions.Nearest research finds that high-purity mullite still has good heat endurance under aerobic conditions and without crystal transfer, be heated to 1800 ℃ just has micro-liquid phase to generate above.Mullite also has the ability of anti-sodium metal salt corrosion under hot conditions, at 1000 ℃ of oxidation environments, uses Na
2sO
4corrosion 100h, there is not any change in the performance of material.
Whisker refers to have certain draw ratio (being generally greater than 10) and sectional area are less than 5.2 * 10
-4cm
2mono-crystlling fibre material.Because the crystal structure of whisker is more complete, internal flaw is less, so the strength and modulus of whisker all approaches the theoretical value of its perfect crystal material, is the advanced composite material (ACM) strengthening and toughening agent that a kind of mechanical property is very excellent.And mullite fiber, due to its constituent (Al
2o
3, SiO
2, B
2o
3, Na
2o, ZrO
2, MgO etc.) excellent properties, and the wettability of it and all kinds of matrixes is good, interfacial reaction is less, therefore as the composite toughening fortifying fibre of pottery, metal and resin etc., in fields such as space flight and aviation, military project weapon, machine-building, stationery sports goodss, there are extremely considerable application prospect and huge commercial value.At present, there are the Nextel series long fiber of Minnesota Mining and Manufacturing Company, the FP of E.I.Du Pont Company and PRD-166 series long fiber in the company of preparing mullite fiber of open report; The Altex series of Japan Sumitomo company and the continuous fibers of Sumica series and the Saffil of Britain ICI company series staple fibre.
Document [Journal of the Ceramic Society of Japan, 1995,103 (2): 199-201.] has been studied the mechanical property of alumina whisker/mullite composite ceramic.The mullite ceramic that contains respectively volume fraction 10,20,30% α-Al2O3 whisker is to make under 1500-1800 ℃ of condition by hot pressed sintering.At 1700 ℃, just obtained composite very fine and close, that Whisker Content reaches 30vol.%.The highest room temperature bending strength reaches 380MPa.Elevated temperature strength and Whisker Content have substantial connection.The increase of Whisker Content has improved the consistency and elasticity modulus of material.Fracture toughness during Whisker Content 30vol.% is 1.5 times of single mullite.But the intensity of compound rear material does not have clear superiority with single matrix phase ratio.
Document [Chemical Physics Letters, 2001,347 (4-6): 337-343] utilizes high temperature service, and aluminium oxide and Co catalyst are carried out to high-temperature process under certain atmosphere, obtains having the alumina nano fiber of herring-bone form structure.By transmission electron microscope observing, find, the trunk of vertical limb structure can grow secondary trunk, has again the vertical secondary trunk grow of less dendritic crystal, successively repeatedly, has the feature of fractal structure.
About mullite crystal whisker, strengthen research toughness reinforcing and mullite fiber at present all more common in new ceramic material field.But the research about whisker mainly concentrates on the toughness reinforcing block materials of enhancing; And the ceramic fibre as structural material occurring at present, equal smooth surface, specific area is little, simple in structure; Also cannot be applied to the fields such as biology, chemical industry as skeleton or carrier material.Have the dendritic fiber of special construction that waits and only appear at nanoscale, as functional material, use, Application Areas is relatively limited to.Whisker growth, to the surface of fiber, is obtained having the mullite fiber of special construction, as the correlative study of structure function integral material, still relatively lack at present.
Summary of the invention
The object of this invention is to provide a kind of structure of the mullite fiber with villous shape whisker and the technique of preparing this structure mullite fiber.
For reaching above object, the present invention takes following technical scheme to be achieved:
A kind of mullite fiber with villous shape whisker, it is characterized in that, described fiber surface be take the fibrillar center axis radial whisker that distributes as initial point towards fiber external diameter direction, this radial whisker is mullite single crystal, diameter 100～550nm, length 1.5～7 μ m, the principal crystalline phase of described fiber is mullite, or contain a small amount of corundum, accounting is 0～18wt%, described in comprise that the diameter of the fiber of radial whisker is 4.1～56 μ m.
The preparation method of the above-mentioned mullite fiber with villous shape whisker, is characterized in that, comprises following step:
(1) by Aqueous Basic Aluminum Chloride and acidic silicasol according to volume ratio 1:0.18～0.45 mixed at room temperature, obtain mixed sols;
(2) in the mixed sols of step (1), slowly drip the poly-vinyl alcohol solution of 5wt%, stir the precursor sol obtaining at least 2 hours under room temperature, wherein, the addition of poly-vinyl alcohol solution is 21～42% of mixed sols volume;
(3) precursor sol of step (2) is concentrated, obtain spinnable colloidal sols; Spinnable colloidal sols is adopted to dry spinning, obtain primary gelatinous fibre;
(4) the primary gelatinous fibre of step (3) and nano alumina powder, nano oxidized silica flour and aluminum fouoride mix are evenly obtained to mixture, wherein, nano aluminium oxide, nano silicon oxide and aluminum fouoride three's mass ratio is 3.4～5.5:1.5～2.4:1;
(5) the uniform mixture of step (4) mix is put into closed container, in air atmosphere, in 1150～1350 ℃ of sintering, be incubated 0.5～2 hour, obtain the mullite fiber with villous shape whisker.
In said method, the described Aqueous Basic Aluminum Chloride of step (1), mass concentration >=20% of aluminium oxide wherein, total basicity 60～95, pH value < 6; Described acidic silicasol is molten, siliconoxide mass concentration >=20% wherein, sol particle granularity < 30nm, pH value < 7.
The described polyvinyl alcohol degree of polymerization of step (2) is 1700～2400, and alcoholysis degree is 88～99%.
Described the concentrating of step (3) is to complete for 24～120 hours under 20～60 ℃ of water bath condition.
The described nano alumina powder grain graininess of step (4) is 1～45nm; Nano oxidized silica flour specific surface 85～425m
2/ g.
Step (5) described in air atmosphere sintering, at 870～970 ℃, increase an insulation platform, temperature retention time 0.5～5 hour; Heating rate is 1～10 ℃/min.
The present invention adopts traditional handicraft, first applies sol-gel process and prepares the good Study on Mullite Gel fiber of continuity, then by gelatinous fibre and powder sintering together with catalyst, make the radial monocrystalline mullite crystal whisker that grows in surface of fiber.Gained fibre structure is unique, function admirable.
The invention has the advantages that:
1, the preparation of primary gelatinous fibre adopts sol-gel technology, effectively reduces fiber firing temperature; Colloid adopts water-soluble system, and cost is lower; Adopt dry spinning, winder is reeled, and technique is simple, is easy to large-scale industrialization development.
2, the direct sintering together with powder and catalyst of primary gelatinous fibre, the growth of mullite crystal whisker and the crystallization of fiber are carried out simultaneously, and sintering schedule is simple.
3, gained fibre structure is unique, and surface distributed is radial, the whisker of three-dimensional growth.This structure has increased the specific area of fiber, both can when as composite reinforcing toughening material, " inlaying " in matrix inside, be combined tightr with matrix; More can be used as the materials such as skeleton, carrier, at chemical industry, biological fields such as support, catalysis, absorption, filtrations, be more widely used.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Fig. 1 is the mullite fiber structural representation of band villous shape whisker of the present invention.
Fig. 2 is the fiber low power SEM photo that the embodiment of the present invention 3 single surfaces of gained have fine hair shape whisker.
Fig. 3 is the magnification at high multiple SEM photo of Fig. 1.
The specific embodiment
Referring to Fig. 1, the mullite fiber of band villous shape whisker of the present invention, the radial whisker of surface distributed, the fibrillar center axial line of take is grown outside as initial point to fiber.Fiber surface whisker is mullite single crystal, diameter 100～550nm, length 1.5～7 μ m.The principal phase of fiber is mullite phase, or contains a small amount of corundum phase, and the ratio of corundum phase is 0～18wt.%.Mullite fiber diameter (comprising surperficial whisker part) is 4.1～56 μ m.The natural length of fiber is greater than 3mm.As can be seen from Figure 1, the tiny whisker of fiber surface is three-dimensional dense distribution, is the nano whisker of radial distribution, has greatly increased the specific area of fiber.
A method of preparing the mullite fiber that is accompanied with fine hair shape whisker, comprises the following step:
(1) Aqueous Basic Aluminum Chloride and acidic silicasol are mixed according to the listed different volumes ratio of table 1, room temperature lower magnetic force stirs 1 hour, obtains mixed sols, and wherein in Aqueous Basic Aluminum Chloride, the mass concentration of aluminium oxide is 20～25%; Ludox pH value 1.5～5.5(table 1).
(2) in mixed sols, slowly drip 5wt% poly-vinyl alcohol solution, addition is in Table 1, and room temperature lower magnetic force stirs and obtains evenly micro-white precursor sol in 3 hours, and wherein, the polyvinyl alcohol degree of polymerization is 1700～2400, and alcoholysis degree is 88～99%(table 1).
(3) by precursor sol in 20～60 ℃ of water-baths concentrated 24～120 hours, reach 0.9～150Pas to viscosity, obtain spinnable colloidal sols; Spinnable colloidal sols is adopted to laboratory vertical dry-process spinning machine spinning, and winder is reeled to collect and is obtained primary gelatinous fibre.Protofibre average length is greater than 3m, protofibre diameter 5～65 μ m(tables 2).
(4) by protofibre and nano alumina powder, nano oxidized silica flour and the even mix of aluminum fouoride.Wherein, nano aluminium oxide, nano silicon oxide and aluminum fouoride three's mass ratio is referring to table 2.Nano alumina powder grain graininess is 1～45nm; Nano oxidized silica flour specific surface 85～425m
2/ g(table 2).
(5) powder that is mixed with gelatinous fibre is put into closed container, 1150～1350 ℃ of sintering in batch-type furnace, target temperature insulation 0.5～2 hour; Be preferably in 870～970 ℃ and increase an insulation platform, temperature retention time 0.5～5 hour; Heating rate is 1～10 ℃/min.(technological parameter is referring to table 2).
Aqueous Basic Aluminum Chloride molecular formula in the present invention: [Al(OH) nC
16-nxH
2o] m(m≤10, N=1～5)), quality of alumina concentration>=20%, total basicity 60～95, pH value < 6; Ludox siliconoxide mass concentration>=20%, sol particle granularity < 30nm, pH value < 7; Nano alumina powder, grain graininess is 1～45nm; Nano oxidized silica flour, specific surface 85～425m
2/ g.
The mullite fiber of the subsidiary fine hair shape structure that the present invention finally obtains, the design parameter after sintering is in Table 3.
The primary gelatinous fibre preparation technology parameter of table 1 the present invention
This whisker growth of table 2 and firing process parameter
The properity parameter of fiber after table 3 sintering
| Embodiment numbering | Diameter of whiskers (nm) | Fibre diameter (μ m) | Whisker density (root/μ m 2） | The ratio of corundum phase (wt.%) |
| 1 | 120 | 29.4 | 9.05 | 18 |
| 2 | 190 | 17.1 | 7.37 | 18 |
| 3 | 150 | 9.6 | 8.71 | 0 |
| 4 | 290 | 11.2 | 5.70 | 0 |
| 5 | 360 | 10.9 | 3.69 | 2 |
| 6 | 320 | 9.2 | 4.36 | 2 |
| 7 | 180 | 8.0 | 7.38 | 18 |
| 8 | 150 | 3.8 | 8.05 | 18 |
By SEM, measure fiber, diameter of whiskers, by XRD analysis, measure crystal structure.Gained fiber surface has fine hair shape whisker, and burning till rear main component is mullite phase and corundum phase.Referring to Fig. 2～3.From the high power photo of Fig. 3, can find, the cross section of whisker is rectangle, and whole whisker is rhombic prism body, shows as typical orthorhombic system crystal formation, binding constituents analysis, and whisker is mullite single crystal.Mullite single crystal excellent performance, the mullite fiber with this spline structure is suitable as structure function integral material and is applied to field widely.
Claims (8)
1. the mullite fiber with villous shape whisker, it is characterized in that, described fiber surface be take the fibrillar center axis radial whisker that distributes as initial point towards fiber external diameter direction, this radial whisker is mullite single crystal, diameter 100～550nm, length 1.5～7 μ m, the principal crystalline phase of described fiber is mullite, or contain a small amount of corundum, accounting is 0～18wt%, described in comprise that the diameter of the fiber of radial whisker is 4.1～56 μ m.
Described in claim 1 with a preparation method for the mullite fiber of villous shape whisker, it is characterized in that, comprise following step:
(1) by Aqueous Basic Aluminum Chloride and acidic silicasol according to volume ratio 1:0.18～0.45 mixed at room temperature, obtain mixed sols;
(2) in the mixed sols of step (1), slowly drip the poly-vinyl alcohol solution of 5wt%, under room temperature, stir and within least 2 hours, obtain precursor sol, wherein, the addition of poly-vinyl alcohol solution is 21～42% of mixed sols volume;
(3) precursor sol of step (2) is concentrated, obtain spinnable colloidal sols; Spinnable colloidal sols is adopted to dry spinning, obtain primary gelatinous fibre;
(4) the primary gelatinous fibre of step (3) and nano alumina powder, nano oxidized silica flour and aluminum fouoride mix are evenly obtained to mixture, wherein, nano aluminium oxide, nano silicon oxide and aluminum fouoride three's mass ratio is 3.4～5.5:1.5～2.4:1;
(5) the uniform mixture of step (4) mix is put into closed container, in air atmosphere, in 1150～1350 ℃ of sintering, be incubated 0.5～2 hour, obtain the mullite fiber with villous shape whisker.
3. as claimed in claim 2 with the preparation method of the mullite fiber of villous shape whisker, it is characterized in that the described Aqueous Basic Aluminum Chloride of step (1), mass concentration >=20% of aluminium oxide wherein, total basicity 60～95, pH value < 6.
As described in kind of claim 2 with the preparation method of the mullite fiber of villous shape whisker, it is characterized in that, described acidic silicasol is molten, wherein siliconoxide mass concentration >=20%, sol particle granularity < 30nm, pH value < 7.
As described in kind of claim 2 with the preparation method of the mullite fiber of villous shape whisker, it is characterized in that, the described polyvinyl alcohol degree of polymerization of step (2) is 1700～2400, alcoholysis degree is 88～99%.
As described in kind of claim 2 with the preparation method of the mullite fiber of villous shape whisker, it is characterized in that, step (3) described concentrated be to complete for 24～120 hours under 20～60 ℃ of water bath condition.
As described in kind of claim 2 with the preparation method of the mullite fiber of villous shape whisker, it is characterized in that, the described nano alumina powder grain graininess of step (4) is 1～45nm; Nano oxidized silica flour specific surface 85～425m
2/ g.
As described in kind of claim 2 with the preparation method of the mullite fiber of villous shape whisker, it is characterized in that, step (5) described in air atmosphere sintering, at 870～970 ℃, increase an insulation platform, temperature retention time 0.5～5 hour; Heating rate is 1～10 ℃/min.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086200A (en) * | 2014-07-22 | 2014-10-08 | 南京理工大学 | Preparation method of mullite fiber |
| CN104446578A (en) * | 2014-11-11 | 2015-03-25 | 天津大学 | Method for preparing mullite fiber or mullilte whisker high-temperature structural material |
| CN109939664A (en) * | 2019-04-16 | 2019-06-28 | 天津工业大学 | A kind of multiple dimensioned preparation method for receiving micrometer alumina fiber photocatalyst carrier |
| CN109987929A (en) * | 2019-04-16 | 2019-07-09 | 天津工业大学 | A kind of preparation method of the multiple dimensioned alumina fibre of needle prick shape of fluorine induced growth |
| CN110004519A (en) * | 2019-04-16 | 2019-07-12 | 天津工业大学 | One kind can produce the electrostatic spinning liquid of the multiple dimensioned alumina fibre of " caterpillar " shape |
| CN113677837A (en) * | 2019-03-29 | 2021-11-19 | 绵天科技有限公司 | Hollow fiber group with ultrahigh forward and compact arrangement |
| CN114717705A (en) * | 2022-03-25 | 2022-07-08 | 吴江市康佳纺织有限公司 | Warm-keeping fiber with velvet, fabric and preparation process of warm-keeping fiber |
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| CN104086200A (en) * | 2014-07-22 | 2014-10-08 | 南京理工大学 | Preparation method of mullite fiber |
| CN104446578A (en) * | 2014-11-11 | 2015-03-25 | 天津大学 | Method for preparing mullite fiber or mullilte whisker high-temperature structural material |
| CN113677837A (en) * | 2019-03-29 | 2021-11-19 | 绵天科技有限公司 | Hollow fiber group with ultrahigh forward and compact arrangement |
| CN113677837B (en) * | 2019-03-29 | 2023-12-29 | 绵天科技有限公司 | Hollow fiber group with ultrahigh forward direction and tight arrangement |
| CN109939664A (en) * | 2019-04-16 | 2019-06-28 | 天津工业大学 | A kind of multiple dimensioned preparation method for receiving micrometer alumina fiber photocatalyst carrier |
| CN109987929A (en) * | 2019-04-16 | 2019-07-09 | 天津工业大学 | A kind of preparation method of the multiple dimensioned alumina fibre of needle prick shape of fluorine induced growth |
| CN110004519A (en) * | 2019-04-16 | 2019-07-12 | 天津工业大学 | One kind can produce the electrostatic spinning liquid of the multiple dimensioned alumina fibre of " caterpillar " shape |
| CN109987929B (en) * | 2019-04-16 | 2021-07-27 | 天津工业大学 | Preparation method of fluorine-induced-growth needle-punched multi-scale alumina fiber |
| CN114717705A (en) * | 2022-03-25 | 2022-07-08 | 吴江市康佳纺织有限公司 | Warm-keeping fiber with velvet, fabric and preparation process of warm-keeping fiber |
| CN114717705B (en) * | 2022-03-25 | 2023-12-08 | 吴江市康佳纺织有限公司 | Thermal fiber with velvet and fabric and preparation process thereof |
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