CN101519304A - Method for preparing dichroite-porzite complex phase material by in-situ reaction calcination - Google Patents
Method for preparing dichroite-porzite complex phase material by in-situ reaction calcination Download PDFInfo
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Abstract
The invention relates to a method for preparing a dichroite-porzite complex phase material by in-situ reaction calcinations, which belongs to the field of preparation of the complex phase ceramic materials. The method is characterized in that kaoline, talcum, manufactured alumina and a small amount of a little accessory ingredient (or without addition of a sintering aid) are used as raw materials to generate a composite material containing crystal phase of the dichroite and the porzite by an in-situ reaction calcinations method of temperature-gradient and heat preservation. In the composite material, crystals of the dichroite and the porzite have excellent growth and clear shape. The composite material has the characteristics of high flexure strength, excellent thermal shock resistance, and the like.
Description
Technical field
The present invention relates to the preparation method that a kind of reaction in of dichroite-mullite complex phase material burns till, belong to the diphase ceramic material preparation field.
Background technology
Trichroite (Cordierite) has advantages such as thermal expansivity is low, thermal shock resistance is good, be widely used in automobile exhaust gas purifying installation, refractory coating, support of the catalyst, heat exchanger material, foamed ceramics, electronic package material, printed circuit board (PCB) etc., and in the environment of some cold and hot cataclysms, such as ceramic heat exchanger, hotblast stove, pillar brick, casket body, refractory slab or the like.But because the trichroite physical strength is not high, load softening point is low, the synthesis temperature narrow range, if do not adopt the method that departs from the trichroite composition or add sintering aid with traditional method, difficulty obtains the pure phase trichroite, thereby has limited the performance of its premium properties.
Mullite (Mullite) is a kind of fine refractory materials, it is good to have high-temperature behavior, the load softening point height, the physical strength advantages of higher, but its thermal expansivity is relatively large, and because of it is mainly the covalent linkage compound, atom bulk diffusion speed at low temperatures is slower, the conventional sintering densification temperature is higher, generally all at 1550～1600 ℃.
As seen, the trichroite thermal expansivity is low, good thermal shock, but high-temperature behavior is general, and physical strength is not high, and the mullite high-temperature behavior is good, the physical strength height, but heat-shock resistance is bad.Therefore, be high-temperature behavior, physical strength and the thermal shock resistance of taking into account material, carrying out trichroite and mullite compound is the effective measure that improve material property.
Preparation dichroite-mullite mixture has multiple diverse ways.A kind of is to be raw material with liquid chemical reagent or colloidal sol, prepares dichroite-mullite powder [M.G.M.U.Ismail, J.Am.Ceram.Soc.73 (3) (1990) 537-543 by sol-gel method (wet-chemical reaction method); ].The advantage of this method is the product purity height, and particle is tiny and even, and the reactive behavior height can reduce sintering temperature greatly.But raw materials used great majority are organic compound, and some still is insalubrity, need be protected, and cost is too high, and complex disposal process, the time is longer.Another kind method is that in trichroite and the mullite one or both are mixed sintering then with raw mineral materials, industrial raw material etc., and [patent No. ZL 200610037794.4 thereby produce the dichroite-mullite mixture; Patent No. ZL 200510101941.5], this method needs synthetic trichroite or mullite, inevitably exists cost to improve problem, and contains other many crystalline phases toward contact in the synthetic dichroite-mullite mixture.
The present invention intends proposing the preparation method that a kind of dichroite-mullite complex phase material reaction in burns till.Method provided by the invention is fully based on mineral and industrial raw material, do not need to add trichroite or mullite grog, obtain the high purity dichroite-mullite complex phase material by common process such as mixing, burn till under lower firing temperature, trichroite wherein has good crystal habit mutually with mullite mutually.
Summary of the invention
The preparation method who the object of the present invention is to provide a kind of dichroite-mullite complex phase material original position to burn till, it is the dichroite-mullite complex phase material with cheap raw material, simple technology synthesis of high purity.
The technical solution used in the present invention:
(1) choosing kaolin, talcum and commercial alumina is main raw material, and their quality proportioning is: kaolin 45～60%, talcum 0.5～38%, commercial alumina 12～44%.The mass percent that adds the Vanadium Pentoxide in FLAKES auxiliary agent in above-mentioned compound is 0.5～6%, mixing.Select for use different proportioning raw materials can obtain trichroite, the different composite diphase material of mullite degree.
The quality percentage composition of mullite is 95%-5% in the dichroite-mullite complex phase material provided by the present invention, and surplus is a trichroite; As preferred forms is that the content of mullite in matrix material is 20wt%, 40wt%, 60wt%, 80wt%, and surplus is a trichroite.
Vanadium Pentoxide in FLAKES can reduce the synthesis temperature of mullite as mineralizer.In the present invention, the adding of Vanadium Pentoxide in FLAKES auxiliary agent not only can reduce the synthesis temperature of mullite, and can promote the growth of mullite crystal in the composite diphase material, helps the raising of composite diphase material mechanical property and heat-shock resistance.
(2) adding mass percent in the mixed batching of step (1) is 7～10% methocel solution (form that is 2% methocel solution adds) with mass percentage concentration, compression moulding behind the mixing, and the dry-pressing pressing pressure is 1～3MPa.
(3) the molding blank room temperature (18-25 ℃) that will be added with 0.5-6wt% Vanadium Pentoxide in FLAKES auxiliary agent is burnt to 950～1050 ℃, and temperature rise rate is 200～400 ℃/h, is incubated 0.5～1.5 hour, promotes the formation of nucleus; Temperature rise rate with 80～150 ℃/h is warming up to 1200～1300 ℃ again, is incubated 0.5～1.5 hour, promotes the formation of trichroite; Continuation is warming up to 1380～1460 ℃ with the speed of 50～150 ℃/h, is incubated 3～6 hours, promotes mullite, cordierite crystal growth, and insulation finishes the back with the stove naturally cooling.
The molding blank that does not add the Vanadium Pentoxide in FLAKES auxiliary agent is warming up to 1380～1460 ℃ by room temperature, temperature-rise period divides five sections to carry out, five sections temperature is respectively 1000 ℃, 1100 ℃, 1200 ℃, 1300 ℃ and last 1380-1460 ℃, this temperature rise rate of five sections is followed successively by 200～400 ℃/h, 100～200 ℃/h, 20～60 ℃/h, 60～150 ℃/h, 20～60 ℃/h, and in 1380～1460 ℃ of insulation 3～6h, naturally cooling.
Test analysis
Utilize X-ray diffraction analysis as can be known, the synthetic dichroite-mullite complex phase material is very pure under technology of the present invention, has only trichroite and mullite diffraction peak (seeing accompanying drawing 1～4) mutually in the XRD figure.
Utilize the analysis of SEM cross-section morphology as can be seen, crystal morphology is typical needle-like or bar styloid (mullite) and corynebacterium or granular crystal (trichroite).Add the composite diphase material of Vanadium Pentoxide in FLAKES sintering adjuvant in the raw material, crystal development is better relatively, form is clearly demarcated, interlaced intensive growth (seeing accompanying drawing 5～8).
Material open porosity, volume density adopt Archimedes's method to measure.Intensity adopts three-point bending resistance intensity to characterize.The heat-shock resistance test method: synthetic dichroite-mullite strip block placed in 1000 ℃ the body of heater, insulation 30min takes out rapidly and places water (room temperature) immediately, is thermal shock for the first time.Be reentered in 1000 ℃ the body of heater block taken out oven dry from water after, insulation 30min takes out and places water (room temperature) immediately, is thermal shock for the second time, and the like repeat said process, and the residual intensity of material after the test thermal shock.
The intensity height of institute of the present invention synthetic dichroite-mullite complex phase material, good thermal shock (seeing example 1～4), and technology is simple, and cost is low, is with a wide range of applications.Trichroite and mullite crystal physically well develop in matrix material, form is clearly demarcated.
Description of drawings
The XRD figure of Fig. 1: embodiment 2 gained dichroite-mullite complex phase materials;
The XRD figure of Fig. 2: embodiment 3 gained dichroite-mullite complex phase materials;
The XRD figure of Fig. 3: embodiment 2 (not adding the Vanadium Pentoxide in FLAKES auxiliary agent) gained dichroite-mullite complex phase material;
The XRD figure of Fig. 4: embodiment 3 (not adding the Vanadium Pentoxide in FLAKES auxiliary agent) gained dichroite-mullite complex phase material;
The cross-section morphology figure of Fig. 5: embodiment 2 gained dichroite-mullite complex phase materials;
The cross-section morphology figure of Fig. 6: embodiment 3 gained dichroite-mullite complex phase materials;
The cross-section morphology figure of Fig. 7: embodiment 2 (not adding the Vanadium Pentoxide in FLAKES auxiliary agent) gained dichroite-mullite complex phase material;
The cross-section morphology figure of Fig. 8: embodiment 3 (not adding the Vanadium Pentoxide in FLAKES auxiliary agent) gained dichroite-mullite complex phase material.
Embodiment
Example 1～4 (the mullite theoretical content is respectively 20%, 40%, 60%, 80%, and the trichroite theoretical content is respectively 80%, 60%, 40%, 20%).
Main raw material is chosen and composition analysis sees Table 1.
Table 1 raw material chemical composition analysis result (wt%)
Preparation raw material shown in the according to the form below 2.
Table 2 proportioning raw materials
Add mass percent and be 8% binding agent (form that with mass percentage concentration is 2% methocel solution adds) in mixed batching, machine is pressed into the strip base substrate under the 2MPa.Heat-up rate with 300 ℃/h rises to 1000 ℃ from room temperature, insulation 1h, and the heat-up rate with 100 ℃/h rises to 1250 ℃ again, insulation 1h continues to rise to 1400 ℃ with the heat-up rate of 100 ℃/h insulation 4h, the nature furnace cooling makes dichroite-mullite complex phase material.
If do not add Vanadium Pentoxide in FLAKES in the batching, only kaolin, commercial alumina, talcum are pressed mixed shown in the table 2, add mass percent and be 8% binding agent (form that with mass percentage concentration is 2% methocel solution adds) in mixed batching, machine is pressed into the strip base substrate under the 2MPa.Heat-up rate with 300 ℃/h rises to 1000 ℃ from room temperature, heat-up rate with 150 ℃/h rises to 1100 ℃ again, continuation rises to 1200 ℃ with the heat-up rate of 40 ℃/h, heat-up rate with 100 ℃/h rises to 1300 ℃, heat-up rate with 40 ℃/h rises to 1420 ℃, insulation 4h, natural furnace cooling can make dichroite-mullite complex phase material equally.
The XRD figure of embodiment 2 gained composite diphase materials, SEM figure are respectively accompanying drawing 1 and accompanying drawing 5.The XRD figure of embodiment 3 gained composite diphase materials, SEM figure are respectively accompanying drawing 2 and accompanying drawing 6.
Press the proportioning of embodiment 2, the XRD figure of adding assistant gained composite diphase material, SEM figure are not respectively accompanying drawing 3 and accompanying drawing 7.Press the proportioning of example 3, the XRD figure of adding assistant gained composite diphase material, SEM figure are not respectively accompanying drawing 4 and accompanying drawing 8.
Other performances of material see Table 3, table 4.
Table 3 material property
Table 4 material property (not adding the Vanadium Pentoxide in FLAKES auxiliary agent)
Claims (8)
1, a kind of reaction in of dichroite-mullite complex phase material burns till the preparation method, it is characterized in that being is raw material with kaolin, talcum and commercial alumina, press the oxide compound batching that mullite and trichroite are formed in the composite diphase material, adopt the original position process for calcining preparation of temperature-gradient method and insulation; Concrete preparation process adopts any in following two kinds of methods:
A.
(a) press the oxide compound batching that trichroite and mullite are formed in the dichroite-mullite complex phase material;
(b) add the Vanadium Pentoxide in FLAKES auxiliary agent in the batching of step a, adding mass percent is the 0.5-6% mixing;
(c) adding mass percent in the mixed material of step b is the methocel solution of 7-10%, dry-pressing compression moulding behind the mixing;
(d) adopt temperature-gradient method and insulation original position to burn till, specifically:
(1) temperature rise rate by 200-400 ℃/h is raised to 950-1050 ℃;
(2) temperature rise rate by 80-150 ℃/h is raised to 1200-1300 ℃;
(3) temperature rise rate by 50-150 ℃/h is raised to 1380-1460 ℃, and insulation 3-6h finishes the back with the stove naturally cooling;
B.
(a) press the oxide compound batching that trichroite and mullite are formed in the dichroite-mullite complex phase material;
(b) adding mass percent on the basis of step a batching mixing is the 7-10% methocel solution, dry-pressing compression moulding behind the mixing;
(c) adopt the original position of temperature-gradient method and insulation to burn till, specifically:
(1) the temperature rise rate room temperature with 200-400 ℃/h rises to 1000 ℃;
(2) temperature rise rate of following with 100-200 ℃/h rises to 1100 ℃;
(3) temperature rise rate of following with 20-60 ℃/h rises to 1200 ℃;
(4) rise to 1300 ℃ with the temperature rise rate of 60-150 ℃/h again;
(5) rise to 1380-1460 ℃ with the temperature rise rate room temperature of 20-60 ℃/h at last, insulation 3-6h, insulation finishes the back with the stove naturally cooling.
2, the reaction in by the described dichroite-mullite complex phase material of claim 1 burns till the preparation method, it is characterized in that each quality percentage composition of forming of described raw material is:
SiO
2 Al
2O
3 MgO P
2O
5 Fe
2O
3 CaO Na
2O K
2O TiO
2
1. kaolin 53.9 45.2-0.02 0.18 0.18-0.05 0.44;
Commercial alumina 0.10 99.7-0.01 0.03 0.04 0.11 0.01-;
3. talcum 64.1 0.66 33.0 0.23 0.82 0.73 0.06-0.03;
More than each total amount of forming be 100%.
3, the reaction in by the described dichroite-mullite complex phase material of claim 1 burns till the preparation method, and the quality percentage composition that it is characterized in that trichroite in the described composite diphase material is 95%-5%, and surplus is a mullite.
4, the reaction in by the described dichroite-mullite complex phase material of claim 3 burns till the preparation method, it is characterized in that trichroite quality percentage composition is 80%, 60%, 40% and 20% in the described composite diphase material, the quality percentage composition of mullite is 20%, 40%, 60% and 80%.
5, the reaction in by the described dichroite-mullite complex phase material of claim 4 burns till the preparation method, it is characterized in that described composite diphase material, and the raw material of use with the proportioning quality percentage composition that adds Vanadium Pentoxide in FLAKES is:
Kaolin industry aluminum oxide talcum Vanadium Pentoxide in FLAKES
80% trichroite-20% mullite 51.1 18.7 30.2 0.8;
60% trichroite-40% mullite 52.4 24.9 22.6 1.6;
40% trichroite-60% mullite 53.8 31.1 15.1 2.4;
20% trichroite-80% mullite 55.1 37.4 7.5 3.2.
6, the reaction in by the described dichroite-mullite complex phase material of claim 1 burns till the preparation method, it is characterized in that in the A method that the methocel solution described in the step b among the step c and B method is is that the form of 2% methocel solution adds with mass percentage concentration.
7, the reaction in by the described dichroite-mullite complex phase material of claim 1 burns till the preparation method, and the pressure that it is characterized in that dry-pressing compression moulding is 1-3Mpa.
8, the reaction in by the described dichroite-mullite complex phase material of claim 1 burns till the preparation method, it is characterized in that the time of (1) and (2) insulation in the steps d of method A is 0.5-1.5 hour.
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