CN106350899A - Preparation method for hollow aluminum oxide fiber - Google Patents
Preparation method for hollow aluminum oxide fiber Download PDFInfo
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- CN106350899A CN106350899A CN201610721538.0A CN201610721538A CN106350899A CN 106350899 A CN106350899 A CN 106350899A CN 201610721538 A CN201610721538 A CN 201610721538A CN 106350899 A CN106350899 A CN 106350899A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
- C04B35/62236—Fibres based on aluminium oxide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention discloses a preparation method for a hollow aluminum oxide fiber. A hollow kapok fiber is used as a carrier, the kapok fiber is soaked into a water-soluble aluminum salt solution or zirconium oxychloride-containing water-soluble aluminum salt solution, and the kapok fiber is taken out and then is sintered in oxygen atmosphere, so that the hollow aluminum oxide fiber is obtained. The aluminum oxide fiber prepared according to the method disclosed by the invention is hollow and has the characteristics of low density, high hollow degree, excellent heat-insulating performance, and the like. After the hollow aluminum oxide fibers are stacked together, air can be divided into smaller spaces; and in a heat transfer process, air flow in the hollow fiber is more difficult than in a solid fiber, so that the heat-insulating performance of the material can be greatly increased, and thus the hollow aluminum oxide fiber can be applied to the field of fire-proof materials.
Description
Technical field
The invention belongs to fire-resistant heat insulating material field, be related to a kind of preparation method of hollow aluminum fiber and in particular to
A kind of method preparing hollow aluminum heat insulation fiber using bombax cotton.
Background technology
Alumina fibre remove there are the high intensity of general ceramic fibre, high-moduluss, thermal conductivity is little, thermal coefficient of expansion is low, anti-
Outside the advantages of chemical erosion ability, extraordinary thermostability, high-temperature oxidation, also have that cost of material is relatively low, production technology is simple
Single the features such as, there is higher cost performance and commercial value, be widely used in industry, military affairs, civilian field of compound material.Control
The different process process that alumina fibre produces, can get heterogeneity and the high-performance fiber product being applied to different application.
Because zirconium oxide can occur martensitic phase transformation, doped zirconia can play certain toughness reinforcing work to alumina fibre
With (Yan Hong etc., the transformation toughening mechanism of zirconia ceramic and application, ceramic journal [m] .2000,1 (1): 46-50).At present
The alumina fibre using is mostly solid fibers, such as the alumina fibre of solution spurt method preparation, and solid construction is unfavorable for
Hinder the conduction of heat, (Li Lei etc., novel solutions spurt method prepares alumina fibre to the heat-proof quality of impact fiber and performance is ground
Study carefully, functional material [m] 2014 (13)).Li Meng etc. is equally solid fiber with aluminium oxide prepared by sol-gal process, fiber stack
Really have more outstanding heat-proof quality after long-pending, but comparatively, solid construction is unfavorable for raising (Lee of heat-proof quality
Sprout, sol-gal process prepares the research [j] of alumina fibre. Rare Metals Materials and engineering, 2012 (s3)).
Bombax cotton is hollow tubular structure, and length is 8～32mm, and average diameter is 10～30 μm, and cell wall thickness is about
0.5～2 μm, fiber hollow rate is 80%～90%, and density is 0.29g/cm3, it is that hollow rate most high-density is minimum so far
Natural fiber.
Content of the invention
For the deficiencies in the prior art, the invention provides a kind of system of simple, stable, practical hollow aluminum fiber
Preparation Method, the bombax cotton using hollow is carrier, is impregnated in acquisition presoma in aluminum salt solution, is obtained after high-temperature calcination
Hollow aluminum fiber, the fiber of the method preparation has the features such as density is low, and degree of hollowness is high, heat-insulating property is good.
Technical scheme is as follows:
A kind of preparation method of hollow aluminum fiber, comprises the following steps:
Mass ratio by water-soluble aluminum salt and water is that 1～15:100 prepares aqueous aluminum salt solution, molten in water-soluble aluminum salt
Add zirconium oxychloride in liquid, bombax cotton is immersed in aqueous aluminum salt solution, under vacuum condition, soaks more than 1h, take out and dry
Sinter to 600～1800 DEG C with the heating rate of 1～10 DEG C/min in having oxygen atmosphere afterwards, prepared hollow aluminum fiber.
Described water-soluble aluminum salt is aluminum chloride, aluminum nitrate etc..
Preferably, under vacuum condition, described soak time is 6h.
The described oxygen atmosphere that has is air or pure oxygen atmosphere.
Preferably, described heating rate is 3 DEG C/min, and described sintering temperature is 1000 DEG C, described sintering process
In temperature retention time be 0～10h, more preferably 1h.
Preferably, described zirconium oxychloride and the mass ratio of aluminium salt are 0～8.3:100.
The bombax cotton that the present invention uses has the characteristics that oil suction water repellent, needs its dipping of guarantee under vacuum conditions
Effect.After the blended solution soaking of bombax cotton, aluminium salt, toughener enter in bombax cotton tube wall.Drying and sintering
In temperature-rise period, aluminium salt is changed into aluminium oxide, and zirconium-containing compound is transformed into zirconium oxide, is present in bombax cotton tube wall.Higher
During temperature, bombax cotton decomposes ablation, leaves aluminium oxide, the final alumina fibre obtaining hollow, and toughener can be certain
The toughness of alumina fibre is improved on degree.
Compared with prior art, the present invention has a following remarkable advantage:
It is carrier that the present invention utilizes bombax cotton, and the alumina fibre of preparation is in hollow form, the alumina fibre heap of hollow
Amass together, air can be divided into more tiny space, therefore in diabatic process, the flowing of air is than in solid fibers
In more difficult, the thermal conductivity of the alumina fibre of hollow is lower, and its heat-proof quality significantly improves.
Brief description
Fig. 1 is the x-ray diffraction collection of illustrative plates of the hollow aluminum fiber being obtained in embodiment 1.
Fig. 2 is the high magnification micro-structure diagram of the hollow aluminum fiber being obtained in embodiment 1.
Fig. 3 is the low range micro-structure diagram of the hollow aluminum fiber being obtained in embodiment 1.
Fig. 4 is the x-ray diffraction collection of illustrative plates of the hollow aluminum fiber being obtained in embodiment 2.
Fig. 5 is the high magnification micro-structure diagram of the hollow aluminum fiber being obtained in embodiment 2
Fig. 6 is the low range micro-structure diagram of the hollow aluminum fiber being obtained in embodiment 2.
Specific embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail.
Embodiment 1
The Aluminum Chloride Hexahydrate taking 0.922g dissolves in 50ml deionized water, prepares aluminum chloride dipping solution.By bombax cotton
Immerse in above-mentioned solution, insert in vacuum tank and be evacuated to -0.1mpa with vacuum pump, after soaking 6h, take out and dry.After drying
Bombax cotton rise to 600 DEG C with the heating rate of 1 DEG C/min in atmosphere, prepared hollow aluminum fiber.
Understand that the hollow aluminum fiber being obtained is γ-al from the x-ray diffraction collection of illustrative plates of Fig. 12o3.Fig. 2 is prepared hollow
Alumina fibre scanning electron microscope high magnification photo is it is seen that fiber is in hollow form.Fig. 3 is that alumina fibre scanning electron microscope low range is shone
Piece is it is seen that fiber has certain seriality.
Embodiment 2
The Aluminum Chloride Hexahydrate taking 4.98g dissolves in 50ml deionized water, adds 0.41g zirconium oxychloride as toughener, joins
Aluminum chloride dipping solution processed.Bombax cotton is immersed in above-mentioned solution, insert in vacuum tank be evacuated to vacuum pump-
0.1mpa, after soaking 1h, takes out and dries.Bombax cotton after drying is risen to the heating rate of 3 DEG C/min in atmosphere
1000 DEG C, after insulation 1h, prepared hollow aluminum fiber.
Understand that this hollow aluminum fiber is γ-al from the x-ray diffraction collection of illustrative plates of Fig. 42o3And t-zro2.Fig. 5 show
The scanning electron microscope high magnification photo of prepared hollow aluminum fiber is it is seen that fiber is in hollow form.Fig. 6 show hollow aluminum
The scanning electron microscope low range photo of fiber is it is seen that fiber seriality is preferable.
Embodiment 3
The aluminum chloride taking 18.66g dissolves in 50ml deionized water, prepares liquor alumini chloridi.Bombax cotton is immersed above-mentioned
In solution, insert in vacuum tank and be evacuated to -0.1mpa with vacuum pump, after soaking 6h, take out and dry.Will be fine for the kapok after drying
Dimension rises to 1800 DEG C with the heating rate of 10 DEG C/min in atmosphere, after insulation 10h, prepared hollow aluminum fiber.
Claims (8)
1. a kind of preparation method of hollow aluminum fiber is it is characterised in that comprise the following steps:
Mass ratio by water-soluble aluminum salt and water is that 1～15:100 prepares aqueous aluminum salt solution, in aqueous aluminum salt solution
Add zirconium oxychloride, by bombax cotton immerse aqueous aluminum salt solution in, under vacuum condition soak more than 1h, take out dry after
Have in oxygen atmosphere and sinter to 600～1800 DEG C with the heating rate of 1～10 DEG C/min, prepared hollow aluminum fiber.
2. hollow aluminum fiber according to claim 1 preparation method it is characterised in that described zirconium oxychloride with
The mass ratio of aluminium salt is 0～8.3:100.
3. the preparation method of hollow aluminum fiber according to claim 1 and 2 is it is characterised in that described water solublity
Aluminium salt is aluminum chloride or aluminum nitrate.
4. the preparation method of hollow aluminum fiber according to claim 1 and 2 is it is characterised in that under vacuum condition, institute
The soak time stated is 6h.
5. the preparation method of hollow aluminum fiber according to claim 1 and 2 is it is characterised in that described has oxygen
Atmosphere is air or pure oxygen atmosphere.
6. the preparation method of hollow aluminum fiber according to claim 1 and 2 is it is characterised in that described intensification is fast
Rate is 3 DEG C/min, and described sintering temperature is 1000 DEG C.
7. the preparation method of hollow aluminum fiber according to claim 1 and 2 is it is characterised in that described is sintered
Temperature retention time in journey is 0～10h.
8. the preparation method of hollow aluminum fiber according to claim 1 and 2 is it is characterised in that described is sintered
Temperature retention time in journey is 1h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610721538.0A CN106350899B (en) | 2016-08-24 | 2016-08-24 | A kind of preparation method of hollow aluminum fiber |
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| CN201610721538.0A CN106350899B (en) | 2016-08-24 | 2016-08-24 | A kind of preparation method of hollow aluminum fiber |
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| CN106350899A true CN106350899A (en) | 2017-01-25 |
| CN106350899B CN106350899B (en) | 2019-01-11 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6427644B1 (en) * | 2017-09-20 | 2018-11-21 | 太平洋セメント株式会社 | Method for producing alumina hollow fiber |
| CN109879666A (en) * | 2019-04-17 | 2019-06-14 | 南京理工大学 | The method for obtaining hollow yttrium-aluminium-garnet heat insulation fiber using bombax cotton |
| CN110156447A (en) * | 2019-05-30 | 2019-08-23 | 南京理工大学 | The preparation method of hollow mullite heat insulation fiber |
| CN112174690A (en) * | 2020-10-12 | 2021-01-05 | 南京理工大学 | Method for preparing hollow aluminum titanate fiber by using kapok fiber |
| CN113737315A (en) * | 2021-08-16 | 2021-12-03 | 南京理工大学 | Method for preparing hollow alumina-based ceramic fiber by using reed as template |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1035479A (en) * | 1987-03-13 | 1989-09-13 | 中国科学院山西煤炭化学研究所 | The preparation method of compound aluminium oxide fibre |
| CN103508475A (en) * | 2012-06-19 | 2014-01-15 | 同济大学 | Preparation methods of alumina hollow microspheres |
| CN104005115A (en) * | 2014-06-17 | 2014-08-27 | 山东大学 | Method for preparing aluminum oxide ceramic fibers |
-
2016
- 2016-08-24 CN CN201610721538.0A patent/CN106350899B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1035479A (en) * | 1987-03-13 | 1989-09-13 | 中国科学院山西煤炭化学研究所 | The preparation method of compound aluminium oxide fibre |
| CN103508475A (en) * | 2012-06-19 | 2014-01-15 | 同济大学 | Preparation methods of alumina hollow microspheres |
| CN104005115A (en) * | 2014-06-17 | 2014-08-27 | 山东大学 | Method for preparing aluminum oxide ceramic fibers |
Non-Patent Citations (2)
| Title |
|---|
| KYUNG-JUN HWANG AT AL: ""Synthesis and characterization of hollow metal oxide micro-tubes using a biomaterial template"", 《BIOMASS AND BIOENERGY》 * |
| 高俊国等: ""模板浸渍法制备Al2O3-ZrO2 -Y2O3复合陶瓷纤维及其烧结工艺"", 《材料热处理学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6427644B1 (en) * | 2017-09-20 | 2018-11-21 | 太平洋セメント株式会社 | Method for producing alumina hollow fiber |
| CN109879666A (en) * | 2019-04-17 | 2019-06-14 | 南京理工大学 | The method for obtaining hollow yttrium-aluminium-garnet heat insulation fiber using bombax cotton |
| CN110156447A (en) * | 2019-05-30 | 2019-08-23 | 南京理工大学 | The preparation method of hollow mullite heat insulation fiber |
| CN112174690A (en) * | 2020-10-12 | 2021-01-05 | 南京理工大学 | Method for preparing hollow aluminum titanate fiber by using kapok fiber |
| CN113737315A (en) * | 2021-08-16 | 2021-12-03 | 南京理工大学 | Method for preparing hollow alumina-based ceramic fiber by using reed as template |
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