CN106119966A - The method of growth in situ mullite crystal whisker in rich aluminum fiber mat - Google Patents
The method of growth in situ mullite crystal whisker in rich aluminum fiber mat Download PDFInfo
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- CN106119966A CN106119966A CN201610446313.9A CN201610446313A CN106119966A CN 106119966 A CN106119966 A CN 106119966A CN 201610446313 A CN201610446313 A CN 201610446313A CN 106119966 A CN106119966 A CN 106119966A
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- fiber mat
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- ludox
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/34—Silicates
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/08—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by cooling of the solution
Abstract
The invention discloses a kind of method of growth in situ mullite crystal whisker in rich aluminum fiber mat, in Ludox, first add deionized water, prepared concentration is 0.033mol/L～0.667mol/L Ludox diluent, then richness aluminum fiber mat is immersed 0.5h under vacuum, with postlyophilization；It is immersed in concentration more under vacuum that configured is 0.5h in 0.100mol/L～2.000mol/L aluminum nitrate solution, with postlyophilization；It immerses concentration more under vacuum that configured is 0.5h in 0.400mol/L～8.000mol/L ammonium fluoride solution, with postlyophilization；Last heat treatment 1h～3h under conditions of 1200 DEG C, can grow equally distributed acicular mullite whisker in existing rich aluminum fiber mat.Present invention process is simple, energy consumption is relatively low, and solves the problem growing the controlled mullite crystal whisker of length in rich aluminum fiber mat, significantly improves comprcssive strength and the elastic modelling quantity of rich aluminum fiber mat.
Description
Technical field
The invention belongs to a kind of ceramic composition being characterized with composition, particularly to one original position in rich aluminum fiber mat
The method of growth mullite crystal whisker, the length of mullite crystal whisker can be controlled by the method.
Background technology
Rich aluminum fire-retardent fiber felt-rug have high temperature resistant, anti-thermal shock, unit weight are little, thermal conductivity is low, chemical stability is good, easy construction
Deng many advantages, have broad application prospects in the industry such as chemical industry, metallurgy, pottery, building.Mullite material has preferably
Resistance to elevated temperatures, Properties of High Temperature Creep, thermal shock resistance, and good mechanical performance, the most also there is higher change
Learn stability, relatively low true density and preferably dielectric properties.Mullite crystal whisker is the mullite crystal of a kind of specific form,
There is certain draw ratio, more rare at nature, owing to its diameter is the most tiny, it is difficult to accommodate lacking in conventional crystalline material
Falling into, inside its crystal structure, atomic arrangement high-sequential, its intensity is close with the theoretical strength of perfect cystal.This crystalline substance
The formation of body is the result of mullite different growth.Under given conditions, mullite crystal can be raw along the c-axis direction of lattice
Long, thus form mullite crystal whisker.Therefore, good except having the distinctive abrasion resistance properties of mullite crystal, heat resistance is excellent
Different (1750 DEG C), resistance to high temperature oxidation, thermal coefficient of expansion are less, and additionally the mechanical property under high temperature is extremely excellent (such as elevated temperature strength
Height, thermal shock resistance are good, high temperature spiral shell diminishes), and owing to the internal flaw of whisker is less, there is mechanical property excellent especially
Energy.Therefore, mullite crystal whisker is the composite strengthening and toughening material of a kind of excellence, and its exploitation application will promote composite wood
The research of material.Mullite can occur anisotropic growth in suitable condition, grows into acicular mullite crystal, i.e. mullite-
Whisker.But little about the research in terms of existing rich aluminum fiber mat growth in situ mullite crystal whisker at present, and growth in situ
Mullite crystal whisker length be difficult to control, how to simplify preparation flow, reduce process costs be a urgently to be resolved hurrily difficulties.
Lyophilization is the principle utilizing ice crystal to distil, in the environment of high vacuum, by frozen food material
Moisture without ice thawing directly from ice solid sublimation be steam, due to material be dried complete in the frozen state, with
Other drying meanss are compared, and physical arrangement and the molecule structure change of material are minimum, and its organizational structure and mode of appearance are by preferably
Ground preserves.During vacuum lyophilization, there is not Surface hardened layer problem in material.The shortcoming of the method is that dry rate is more general
Logical seasoning is relatively slow, costly.
Summary of the invention
The purpose of the present invention, is less for preparing mullite crystal whisker research in rich aluminum fiber mat, and is difficult to control
The deficiency of the length this respect of mullite crystal whisker.There is provided a kind of technique simple, with low cost and rich aluminum fiber can be significantly improved
The method of felt mechanical performance.
The present invention is achieved by following technical solution.
A kind of method of growth in situ mullite crystal whisker in rich aluminum fiber mat, has following steps:
(1) weigh Ludox, be added to deionized water and diluted, be uniformly mixing to obtain Ludox diluent, silicon
The concentration of colloidal sol diluent is 0.033mol/L～0.667mol/L；Again richness aluminum fiber mat is immersed Ludox diluent, very
Impregnating 0.5h under empty condition, then below 0 DEG C, it being refrigerated to impregnation liquid becomes solid, is placed in by the solid after freezing subsequently
Freeze dryer carries out lyophilization；
(2) weigh aluminum nitrate, prepare aluminum nitrate solution with deionized water for solvent, its concentration be 0.100mol/L～
2.000mol/L；The concentration of this aluminum nitrate solution is in step (1) 3 times of Ludox diluent concentration；Again by dry in step (1)
Dry good rich aluminum fiber mat immerses aluminum nitrate solution, impregnates 0.5h under vacuum, then it be refrigerated to below 0 DEG C leaching
Stain liquid is frozen into solid, is placed in freeze dryer by the solid after freezing subsequently and carries out lyophilization；
(3) weigh ammonium fluoride, with deionized water as solvent, prepare ammonium fluoride solution, its concentration be 0.400mol/L～
8.000mol/L；The concentration of this ammonium fluoride solution is in step (1) 12 times of Ludox diluent concentration；Again by step (2)
Dried rich aluminum fiber mat immerses ammonium fluoride solution, impregnates 0.5h under vacuum, then it is refrigerated to below 0 DEG C
Impregnation liquid is frozen into solid, is placed in freeze dryer by the solid after freezing subsequently and carries out lyophilization；
(4) rich aluminum fiber mat dried in step (3) is carried out heat treatment 1h～3h, Ji Ke under the conditions of 1200 DEG C
On the fiber of rich aluminum fiber mat, growth in situ goes out acicular mullite whisker.
The concentration of the Ludox diluent of described step (1) is 0.033mol/L.
The concentration of the aluminum nitrate solution of described step (2) is 0.100mol/L.
The concentration of the ammonium fluoride solution of described step (3) is 0.400mol/L.
The present invention is relative to the most conventional method preparing mullite crystal whisker, and its technological process is simple, and energy consumption is relatively low, energy
The length of enough effective mullite crystal whiskers controlling growth in situ, and serve the effect improving rich aluminum fiber mat mechanical performance.
Accompanying drawing explanation
Fig. 1 is 1000 times of SEM image of undressed rich aluminum fiber mat；
Fig. 2 is 1000 times of the mullite crystal whisker obtained after the rich aluminum fiber mat heat treatment that in embodiment 1, lyophilization is good
SEM image；
Fig. 3 is 1000 times of the mullite crystal whisker obtained after the rich aluminum fiber mat heat treatment that in embodiment 2, lyophilization is good
SEM image；
Fig. 4 is 1000 times of the mullite crystal whisker obtained after the rich aluminum fiber mat heat treatment that in embodiment 3, lyophilization is good
SEM image；
Fig. 5 is 1000 times of the mullite crystal whisker obtained after the rich aluminum fiber mat heat treatment that in embodiment 4, lyophilization is good
SEM image；
Fig. 6 be rich aluminum fiber mat after vacuum impregnation combines lyophilization growth in situ mullite crystal whisker, comprcssive strength
Test curve figure.
Detailed description of the invention
Ludox, ammonium fluoride and aluminum nitrate used by the present invention are Tianjin recovery fine chemistry industry institute and produce, for analyzing
Pure reagent.Rich aluminum fiber mat used by the present invention is that crystal fibre company limited of Zhejiang HTC produces.
The present invention is done the brightest below in conjunction with specific embodiment.
Embodiment 1
(1) weighing Ludox, be added to deionized water and diluted, being configured to concentration is 0.033mol/L Ludox
Diluent, immerses Ludox diluent by richness aluminum fiber mat, impregnates 0.5h under vacuum, then by its below 0 DEG C cold
Freeze and be frozen into solid to impregnation liquid, on freeze dryer, carry out lyophilization subsequently；
(2) weigh aluminum nitrate, be added thereto to deionized water and be configured to the aluminum nitrate solution that concentration is 0.1mol/L, will step
Suddenly dried in (1) rich aluminum fiber mat immerses aluminum nitrate solution, impregnates 0.5h under vacuum, then by its 0 DEG C with
Under be refrigerated to impregnation liquid and be frozen into solid, on freeze dryer, carry out lyophilization subsequently；
(3) weigh ammonium fluoride, be added thereto to deionized water and be configured to the ammonium fluoride solution that concentration is 0.4mol/L, will step
Suddenly dried in (2) rich aluminum fiber mat immerses ammonium fluoride solution, impregnates 0.5h under vacuum, then by its 0 DEG C with
Under be refrigerated to impregnation liquid and be frozen into solid, on freeze dryer, carry out lyophilization subsequently；
(4) rich aluminum fiber mat dried in step (3) is carried out heat treatment 2h under the conditions of 1200 DEG C, can be at rich aluminum
On fiber felt, growth in situ goes out acicular mullite whisker.
In embodiment 1, the SEM image of rich aluminum fiber mat is as shown in Figure 1.It is not difficult to find out from Fig. 1, undressed rich aluminum
The fiber of fiber felt is long fibre, and surface more brilliance.Fig. 2 is at the rich aluminum fiber mat heat that in embodiment 1, lyophilization is good
1000 times of SEM image of the mullite crystal whisker obtained after reason.After 1200 DEG C of heat treatments, the fluorination introduced by precipitation
Aluminum amount is less, and the degree of supersaturation of the rich fluorine gas atmosphere generating mullite crystal whisker is relatively low, finally gives the mullite crystal whisker that length is less.
Embodiment 2
(1) weighing Ludox, be added to deionized water and diluted, being configured to concentration is that 0.1mol/L Ludox is dilute
Release liquid, richness aluminum fiber mat is immersed Ludox diluent, impregnate 0.5h under vacuum, then by its freezing below 0 DEG C
It is frozen into solid to impregnation liquid, on freeze dryer, carries out lyophilization subsequently；
(2) weigh aluminum nitrate, be added thereto to deionized water and be configured to the aluminum nitrate solution that concentration is 0.3mol/L, will step
Suddenly dried in (1) mullite block immerses aluminum nitrate solution, impregnates 0.5h under vacuum, then by its 0 DEG C with
Under be refrigerated to impregnation liquid and be frozen into solid, on freeze dryer, carry out lyophilization subsequently；
(3) weigh ammonium fluoride, be added thereto to deionized water and be configured to the ammonium fluoride solution that concentration is 1.2mol/L, will step
Suddenly dried in (2) mullite block immerses ammonium fluoride solution, impregnates 0.5h under vacuum, then by its 0 DEG C with
Under be refrigerated to impregnation liquid and be frozen into solid, on freeze dryer, carry out lyophilization subsequently；
(4) mullite block dried in step (3) is carried out heat treatment 2h under the conditions of 1200 DEG C, can be at rich aluminum
On fiber felt, growth in situ goes out acicular mullite whisker.
In the impregnation liquid of embodiment 2, the content of Ludox, aluminum nitrate and ammonium fluoride relatively embodiment 1 increased.Can by Fig. 3
To find out, the length of whisker relatively embodiment 1 has increased, and whisker distribution is the finest and close.Through 1200 DEG C of heat treatments, immerse not come
There is the reaction of a series of gas phases in silicon dioxide and aluminium fluoride in stone body, under conditions of rich fluorine gas atmosphere, with rich aluminum fiber is
Growth substrate, by epitaxial growth, ultimately generates and is evenly distributed and mullite crystal whisker that relatively embodiment 1 is the finest and close, whisker
Draw ratio significantly increases.Fiber felt after growth whisker is carried out intensity test, finds that comprcssive strength is obviously improved.Thus
Visible, utilize Vacuum infusion techniques to combine introducing aluminium fluoride in lyophilization normal direction mullite block fibre agglomerates, can be in situ
Grow and be evenly distributed and intensive acicular mullite whisker.The comprcssive strength that mullite after growth whisker is block is carried out
Test can be seen that, the comprcssive strength of mullite block is significantly improved.
Embodiment 3
(1) weighing Ludox, be added to deionized water and diluted, being configured to concentration is 0.16mol/L Ludox
Diluent, immerses Ludox diluent by richness aluminum fiber mat, impregnates 0.5h under vacuum, then by its below 0 DEG C cold
Freeze and be frozen into solid to impregnation liquid, on freeze dryer, carry out lyophilization subsequently；
(2) weigh aluminum nitrate, be added thereto to deionized water and be configured to the aluminum nitrate solution that concentration is 0.5mol/L, will step
Suddenly dried in (1) mullite block immerses aluminum nitrate solution, impregnates 0.5h under vacuum, then by its 0 DEG C with
Under be refrigerated to impregnation liquid and be frozen into solid, on freeze dryer, carry out lyophilization subsequently；
(3) weigh ammonium fluoride, be added thereto to deionized water and be configured to the ammonium fluoride solution that concentration is 2.0mol/L, will step
Suddenly dried in (2) mullite block immerses ammonium fluoride solution, impregnates 0.5h under vacuum, then by its 0 DEG C with
Under be refrigerated to impregnation liquid and be frozen into solid, on freeze dryer, carry out lyophilization subsequently；
(4) mullite block dried in step (3) is carried out heat treatment 2h under the conditions of 1200 DEG C, can be at rich aluminum
On fiber felt, growth in situ goes out acicular mullite whisker.
Fig. 4 is 1000 times of the mullite crystal whisker obtained after the rich aluminum fiber mat heat treatment that in embodiment 3, lyophilization is good
SEM image.
The silicon dioxide immersed in the rich aluminum fiber mat obtained after 3 vacuum impregnations and lyophilization and aluminium fluoride sink
Shallow lake hybrid particles amount is more than embodiment 1 and embodiment 2；After Overheating Treatment, mullite crystal whisker draw ratio is more than embodiment 1 and reality
Execute example 2.This is that the fluorination aluminum amount owing to being introduced by precipitation is increased, and in heat treatment process, the rich fluorine gas atmosphere of formation is dense
Degree increases, and reaction gas phase promotes crystal continued growth along its length, and whisker draw ratio increases, and comprcssive strength promotes.
Embodiment 4
(1) weighing Ludox, be added to deionized water and diluted, being configured to concentration is 0.67mol/L Ludox
Diluent, immerses Ludox diluent by mullite block, impregnates 0.5h under vacuum, then by its below 0 DEG C cold
Freeze and be frozen into solid to impregnation liquid, on freeze dryer, carry out lyophilization subsequently；
(2) weigh aluminum nitrate, be added thereto to deionized water and be configured to the aluminum nitrate solution that concentration is 2.0mol/L, will step
Suddenly dried in (1) mullite block immerses aluminum nitrate solution, impregnates 0.5h under vacuum, then by its 0 DEG C with
Under be refrigerated to impregnation liquid and be frozen into solid, on freeze dryer, carry out lyophilization subsequently；
(3) weigh ammonium fluoride, be added thereto to deionized water and be configured to the ammonium fluoride solution that concentration is 8.0mol/L, will step
Suddenly dried in (2) mullite block immerses ammonium fluoride solution, impregnates 0.5h under vacuum, then by its 0 DEG C with
Under be refrigerated to impregnation liquid and be frozen into solid, on freeze dryer, carry out lyophilization subsequently；
(4) mullite block dried in step (3) is carried out heat treatment 3h under the conditions of 1200 DEG C, can be at rich aluminum
On fiber felt, growth in situ goes out acicular mullite whisker.
Fig. 5 is 1000 times of the mullite crystal whisker obtained after the rich aluminum fiber mat heat treatment that in embodiment 4, lyophilization is good
SEM image.
The silicon dioxide immersed in the rich aluminum fiber mat obtained after 3 vacuum impregnations and lyophilization and aluminium fluoride sink
Shallow lake hybrid particles amount is more than embodiment 1, embodiment 2, embodiment 3；After Overheating Treatment, mullite crystal whisker is bar-shaped, and whisker is long
Footpath is than the draw ratio less than embodiment 1 whisker.This is that the fluorination aluminum amount owing to being introduced by precipitation is too much, heat treated
The concentration of the rich fluorine gas atmosphere formed in journey is excessive, reactant excess, has exceeded the amount needed for whisker epitaxial growth, and residue gas phase promotees
Making crystal grow along other direction, cause crystal respectively to reduce to speed of growth difference, whisker draw ratio reduces, and whisker is roughened.This
Planting roughening also makes its comprcssive strength be obviously improved.(as shown in Figure 6) elastic modelling quantity in embodiment 4 is several apparently higher than other
Individual embodiment.
The method of growth in situ mullite crystal whisker in rich aluminum fiber mat of the present invention, it is adaptable to all siliceous fiber blocks
Body.
The above-mentioned description to embodiment is easy for those skilled in the art and is understood that and applies the present invention.Ripe
These embodiments are easily made various amendment by the personnel knowing art technology, and General Principle described herein is applied to
Without through performing creative labour in other embodiments.Therefore, the invention is not restricted to embodiment here, people in the art
Member should be within protection scope of the present invention according to the announcement of the present invention, the improvement made for the present invention and amendment.
Each raw material cited by the present invention can realize the present invention, and the bound value of raw material, interval value can be real
Show the present invention, then this is illustrated the most one by one.
Claims (4)
1. a method for growth in situ mullite crystal whisker in rich aluminum fiber mat, has following steps:
(1) weigh Ludox, be added to deionized water and diluted, be uniformly mixing to obtain Ludox diluent, Ludox
The concentration of diluent is 0.033mol/L～0.667mol/L；Again richness aluminum fiber mat is immersed Ludox diluent, at vacuum bar
Impregnating 0.5h under part, then below 0 DEG C, it being refrigerated to impregnation liquid becomes solid, subsequently the solid after freezing is placed in freezing
Exsiccator carries out lyophilization；
(2) weigh aluminum nitrate, prepare aluminum nitrate solution with deionized water for solvent, its concentration be 0.100mol/L～
2.000mol/L；The concentration of this aluminum nitrate solution is in step (1) 3 times of Ludox diluent concentration；Again by dry in step (1)
Dry good rich aluminum fiber mat immerses aluminum nitrate solution, impregnates 0.5h under vacuum, then it be refrigerated to below 0 DEG C leaching
Stain liquid is frozen into solid, is placed in freeze dryer by the solid after freezing subsequently and carries out lyophilization；
(3) weigh ammonium fluoride, with deionized water as solvent, prepare ammonium fluoride solution, its concentration be 0.400mol/L～
8.000mol/L；The concentration of this ammonium fluoride solution is in step (1) 12 times of Ludox diluent concentration；Again by step (2)
Dried rich aluminum fiber mat immerses ammonium fluoride solution, impregnates 0.5h under vacuum, then it is refrigerated to below 0 DEG C
Impregnation liquid is frozen into solid, is placed in freeze dryer by the solid after freezing subsequently and carries out lyophilization.
(4) rich aluminum fiber mat dried in step (3) is carried out heat treatment 1h～3h under the conditions of 1200 DEG C, can be at rich aluminum
On the fiber of fiber felt, growth in situ goes out acicular mullite whisker.
The method of growth in situ mullite crystal whisker in rich aluminum fiber mat the most according to claim 1, it is characterised in that institute
The concentration of the Ludox diluent stating step (1) is 0.033mol/L.
The method of growth in situ mullite crystal whisker in rich aluminum fiber mat the most according to claim 1, it is characterised in that institute
The concentration of the aluminum nitrate solution stating step (2) is 0.100mol/L.
The method of growth in situ mullite crystal whisker in rich aluminum fiber mat the most according to claim 1, it is characterised in that institute
The concentration of the ammonium fluoride solution stating step (3) is 0.400mol/L.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109320193A (en) * | 2017-07-31 | 2019-02-12 | 天津大学 | Mullite fiber/mullite crystal whisker/aerosil multilevel structure and its preparation method and application |
| CN110452008A (en) * | 2019-07-31 | 2019-11-15 | 辽宁科技大学 | A kind of preparation method of mullite crystal whisker enhancing carborundum porous ceramics |
| CN111302760A (en) * | 2018-12-11 | 2020-06-19 | 天津大学 | Mullite whisker/fiber synergistically enhanced silica aerogel multi-scale composite structure and preparation method and application thereof |
| CN112457037A (en) * | 2019-09-09 | 2021-03-09 | 天津大学 | Performance and application of mullite fiber whisker porous reinforcement reinforced silica aerogel composite material prepared based on liquid phase method |
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| CN109320193A (en) * | 2017-07-31 | 2019-02-12 | 天津大学 | Mullite fiber/mullite crystal whisker/aerosil multilevel structure and its preparation method and application |
| CN111302760A (en) * | 2018-12-11 | 2020-06-19 | 天津大学 | Mullite whisker/fiber synergistically enhanced silica aerogel multi-scale composite structure and preparation method and application thereof |
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| CN112457037B (en) * | 2019-09-09 | 2022-02-11 | 天津大学 | Performance and application of mullite fiber whisker porous reinforcement reinforced silica aerogel composite material prepared based on liquid phase method |
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Application publication date: 20161116 |