A kind of micro-closed pore of lightweight is containing magnesium corundum fireproof aggregate and preparation method thereof
Technical field
The invention belongs to corundum fireproof aggregate technical field.It is specifically related to a kind of micro-closed pore of lightweight containing magnesium corundum fireproof aggregate and preparation method thereof.
Background technology
Along with the development of the development of New Metallurgical Technique, particularly external refining and continuous casting technology, ladle carries the most important metallurgical task, and lining material in the ladle also proposes more strict requirements.To the major demands of lining material in the ladle it is at present: (1) light weight energy-saving, it is possible to effectively reducing ladle heat and scatter and disappear, the control for steel quality is significant;(2) long service life, it is bigger that inner lining material Spalling resistance energy and slag resistance need lifting further, the particularly otherness of the difference smelting condition lower liner material slag resistances such as slag system, steel grade badly.Therefore, the lightweight of working lining refractory material is the important research direction solving the problems referred to above.
Refractory aggregate lightweight is to realize the light-weighted main path of working lining refractory material.The light weight aggregate preparation method of report mainly has at present: the inorganic matter decomposition methods such as organic matter decomposition method, foam in place hole creating technology and hydroxide.O.
Lyckfeldt et al. use starch as bonding agent and foaming agent (O. Lyckfeldt, J. M. F. Ferreira,
Processing of porous ceramics by starch consolidation, J. Eur. Ceram. Soc. 18
(2) (1998) 131 140.), being prepared for Woelm Alumina, though prepared aggregate volume density substantially reduces, but apparent porosity and aperture are bigger;S. J. Li et al. use kaolinite as foaming agent (S. J. Li,
N. Li, Effects of composition and temperature on porosity and pore size
distribution of porous ceramics prepared from Al(OH)3 and
Kaolinite gangue, Ceram. Int. 33 (4) (2007) 551-556.), it is prepared for porous corundum-mullite aggregate, prepared aggregate average pore size is less, but apparent porosity is up to 40%;R. Salomãoa
Et al. utilize hydrotalcite decomposition in situ (R. Salom oa, M.V. B asa, V.C. Pandolfellia,
Porous alumina-spinel ceramics for high temperature applications, Ceram. Int.
37 (4) (2011) 1393-1399.), it is prepared for porous corundum-spinel aggregate, prepared aggregate is also unable to reach production requirement in terms of apparent porosity and aperture.
In sum, all there is the defect that apparent porosity is high, average pore size is big in the most prepared light weight refractory aggregate, when for lining material in the ladle, material slag resistance will be a greater impact, it is difficult to reaches the requirement of actual industrial production.Micro-the closing of pore of light weight aggregate is effectively to solve the important channel of the problems referred to above.
Summary of the invention
It is contemplated that overcome prior art defect, it is therefore an objective to provide that a kind of apparent porosity is low, closed porosity is high, bulk density is less, average pore size is little, thermal conductivity is relatively low, resistance to erosion and the strong micro-closed pore of lightweight of slag-resistant erosiveness be containing magnesium corundum fireproof aggregate and preparation method thereof.
For realizing above-mentioned task, the technical solution adopted in the present invention is: with the γ-Al of 80 ~ 95wt%2O3The fine magnesium oxide micro-powder of fine powder, the nano alumina powder of 1 ~ 10wt% and 1 ~ 10wt% is raw material, the water of additional described raw material 40 ~ 70wt%, mixing, with planetary ball mill wet-milling 0.5 ~ 3 hour, obtains slip;Again described slip is placed in mould, places 12 ~ 24 hours under room temperature condition, the demoulding;Then the base substrate after the demoulding is dried 12 ~ 36 hours under the conditions of 110 ~ 200 DEG C, under the conditions of 1750 ~ 1900 DEG C, is incubated 1 ~ 8 hour, obtains lightweight micro-closed pore corundum fireproof aggregate in magnesium.
Described γ-Al2O3The Al of fine powder2O3Content > 99wt%, particle diameter is 0.045 ~ 0.088mm.
The Al of described nano alumina powder2O3Content > 99wt%, average grain diameter is 20 ~ 50nm.
The content of MgO of described fine magnesium oxide micro-powder > 99wt%, particle diameter D50It is 2 ~ 7 μm.
The mill ball of described planetary ball mill is corundum ball.
Owing to using technique scheme, the present invention compared with prior art has a following good effect:
The nano alumina powder that present invention introduces at high temperature can show superplasticity, under conditions of stress exists, this characteristic can make crystal boundary quickly move, the migration rate of crystal boundary is more than hole migration rate, in sintering process, crystal boundary can be closed before hole is excluded, thus forms a large amount of closed pore.Owing to superplasticity needs competence exertion effect under the promotion of stress, the fine magnesium oxide micro-powder that present invention introduces can react in-situ preparation spinelle with aluminum oxide, along with certain volumetric expansion in course of reaction, thus produces corresponding force in situ.The existence of this original position corresponding force can effectively promote the superplastic performance of nano aluminium oxide, thus form a large amount of closed pore, meanwhile, along with the movement of crystal boundary, macroscopic void is divided into Minute pores, thus reaches the purpose forming the micro-closed pore of lightweight containing magnesium corundum fireproof aggregate.Additionally, the In-suit spinel that the fine magnesium oxide micro-powder introduced is internally formed at aggregate, when with slag contacts, it is possible to the components such as effectively Fe, Mn in solid solution slag, promote aggregate slag resistance.
The micro-closed pore of lightweight prepared by the present invention contains magnesium corundum fireproof aggregate after testing: bulk density is 2.8 ~ 3.15g/cm3, apparent porosity is 2 ~ 10%, and average pore size is 0.3 ~ 1 μm.
Therefore, the lightweight micro-closed pore corundum fireproof aggregate in magnesium prepared by the present invention have that apparent porosity is low, closed porosity is high, bulk density is less, average pore size is little, thermal conductivity is relatively low, resistance to erosion and the strong feature of slag-resistant erosiveness.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the invention will be further described, not limiting of its scope:
For avoiding repeating, first by as follows to the raw material involved by this detailed description of the invention and technological parameter Unify legislation, embodiment repeats no more:
Described γ-Al2O3The Al of fine powder2O3Content > 99wt%, particle diameter is 0.045 ~ 0.088mm.
The Al of described nano alumina powder2O3Content > 99wt%, average grain diameter is 20 ~ 50nm.
The content of MgO of described fine magnesium oxide micro-powder > 99wt%, particle diameter D50It is 2 ~ 7 μm.
The mill ball of described planetary ball mill is corundum ball.
Embodiment
1
A kind of micro-closed pore of lightweight is containing magnesium corundum fireproof aggregate and preparation method thereof.γ-Al with 92 ~ 95wt%2O3The fine magnesium oxide micro-powder of fine powder, the nano alumina powder of 1 ~ 4wt% and 1 ~ 4wt% is raw material, the water of additional described raw material 40 ~ 60wt%, mixing, with planetary ball mill wet-milling 1.5 ~ 3 hours, obtains slip;Again described slip is placed in mould, places 12 ~ 24 hours under room temperature condition, the demoulding;Then the base substrate after the demoulding is dried 24 ~ 36 hours under the conditions of 110 ~ 160 DEG C, under the conditions of 1750 ~ 1850 DEG C, is incubated 5 ~ 8 hours, obtains lightweight micro-closed pore corundum fireproof aggregate in magnesium.
The micro-closed pore of lightweight prepared by the present embodiment contains magnesium corundum fireproof aggregate after testing: bulk density is 3.05 ~ 3.15g/cm3;Apparent porosity is 5 ~ 9%;Average pore size is 0.6 ~ 1 μm.
Embodiment
2
A kind of micro-closed pore of lightweight is containing magnesium corundum fireproof aggregate and preparation method thereof.γ-Al with 92 ~ 95wt%2O3The fine magnesium oxide micro-powder of fine powder, the nano alumina powder of 1 ~ 4wt% and 1 ~ 4wt% is raw material, the water of additional described raw material 50 ~ 70wt%, mixing, with planetary ball mill wet-milling 0.5 ~ 1.5 hour, obtains slip;Again described slip is placed in mould, places 12 ~ 24 hours under room temperature condition, the demoulding;Then the base substrate after the demoulding is dried 12 ~ 24 hours under the conditions of 150 ~ 200 DEG C, under the conditions of 1800 ~ 1900 DEG C, is incubated 1 ~ 5 hour, obtains lightweight micro-closed pore corundum fireproof aggregate in magnesium.
The micro-closed pore of lightweight prepared by the present embodiment contains magnesium corundum fireproof aggregate after testing: bulk density is 3.0 ~ 3.1g/cm3;Apparent porosity is 6 ~ 10%;Average pore size is 0.5 ~ 1 μm.
Embodiment
3
A kind of micro-closed pore of lightweight is containing magnesium corundum fireproof aggregate and preparation method thereof.γ-Al with 88 ~ 92wt%2O3The fine magnesium oxide micro-powder of fine powder, the nano alumina powder of 3 ~ 6wt% and 3 ~ 6wt% is raw material, the water of additional described raw material 40 ~ 60wt%, mixing, with planetary ball mill wet-milling 1.5 ~ 3 hours, obtains slip;Again described slip is placed in mould, places 12 ~ 24 hours under room temperature condition, the demoulding;Then the base substrate after the demoulding is dried 24 ~ 36 hours under the conditions of 110 ~ 160 DEG C, under the conditions of 1750 ~ 1850 DEG C, is incubated 5 ~ 8 hours, obtains lightweight micro-closed pore corundum fireproof aggregate in magnesium.
The micro-closed pore of lightweight prepared by the present embodiment contains magnesium corundum fireproof aggregate after testing: bulk density is 2.9 ~ 3.1g/cm3;Apparent porosity is 5 ~ 7%;Average pore size is 0.6 ~ 0.8 μm.
Embodiment
4
A kind of micro-closed pore of lightweight is containing magnesium corundum fireproof aggregate and preparation method thereof.γ-Al with 88 ~ 92wt%2O3The fine magnesium oxide micro-powder of fine powder, the nano alumina powder of 3 ~ 6wt% and 3 ~ 6wt% is raw material, the water of additional described raw material 50 ~ 70wt%, mixing, with planetary ball mill wet-milling 0.5 ~ 1.5 hour, obtains slip;Again described slip is placed in mould, places 12 ~ 24 hours under room temperature condition, the demoulding;Then the base substrate after the demoulding is dried 12 ~ 24 hours under the conditions of 150 ~ 200 DEG C, under the conditions of 1800 ~ 1900 DEG C, is incubated 1 ~ 5 hour, obtains lightweight micro-closed pore corundum fireproof aggregate in magnesium.
The micro-closed pore of lightweight prepared by the present embodiment contains magnesium corundum fireproof aggregate after testing: bulk density is 2.9 ~ 3.0g/cm3;Apparent porosity is 6 ~ 8%;Average pore size is 0.5 ~ 1 μm.
Embodiment
5
A kind of micro-closed pore of lightweight is containing magnesium corundum fireproof aggregate and preparation method thereof.γ-Al with 84 ~ 88wt%2O3The fine magnesium oxide micro-powder of fine powder, the nano alumina powder of 6 ~ 8wt% and 6 ~ 8wt% is raw material, the water of additional described raw material 40 ~ 60wt%, mixing, with planetary ball mill wet-milling 1.5 ~ 3 hours, obtains slip;Again described slip is placed in mould, places 12 ~ 24 hours under room temperature condition, the demoulding;Then the base substrate after the demoulding is dried 24 ~ 36 hours under the conditions of 110 ~ 160 DEG C, under the conditions of 1750 ~ 1850 DEG C, is incubated 5 ~ 8 hours, obtains lightweight micro-closed pore corundum fireproof aggregate in magnesium.
The micro-closed pore of lightweight prepared by the present embodiment contains magnesium corundum fireproof aggregate after testing: bulk density is 2.9 ~ 3.0g/cm3;Apparent porosity is 4 ~ 6%;Average pore size is 0.4 ~ 0.6 μm.
Embodiment
6
A kind of micro-closed pore of lightweight is containing magnesium corundum fireproof aggregate and preparation method thereof.γ-Al with 84 ~ 88wt%2O3The fine magnesium oxide micro-powder of fine powder, the nano alumina powder of 6 ~ 8wt% and 6 ~ 8wt% is raw material, the water of additional described raw material 50 ~ 70wt%, mixing, with planetary ball mill wet-milling 0.5 ~ 1.5 hour, obtains slip;Again described slip is placed in mould, places 12 ~ 24 hours under room temperature condition, the demoulding;Then the base substrate after the demoulding is dried 12 ~ 24 hours under the conditions of 150 ~ 200 DEG C, under the conditions of 1800 ~ 1900 DEG C, is incubated 1 ~ 5 hour, obtains lightweight micro-closed pore corundum fireproof aggregate in magnesium.
The micro-closed pore of lightweight prepared by the present embodiment contains magnesium corundum fireproof aggregate after testing: bulk density is 2.85 ~ 2.95g/cm3;Apparent porosity is 5 ~ 7%;Average pore size is 0.5 ~ 0.7 μm.
Embodiment
7
A kind of micro-closed pore of lightweight is containing magnesium corundum fireproof aggregate and preparation method thereof.γ-Al with 80 ~ 84wt%2O3The fine magnesium oxide micro-powder of fine powder, the nano alumina powder of 7 ~ 10wt% and 7 ~ 10wt% is raw material, the water of additional described raw material 40 ~ 60wt%, mixing, with planetary ball mill wet-milling 1.5 ~ 3 hours, obtains slip;Again described slip is placed in mould, places 12 ~ 24 hours under room temperature condition, the demoulding;Then the base substrate after the demoulding is dried 24 ~ 36 hours under the conditions of 110 ~ 160 DEG C, under the conditions of 1750 ~ 1850 DEG C, is incubated 5 ~ 8 hours, obtains lightweight micro-closed pore corundum fireproof aggregate in magnesium.
The micro-closed pore of lightweight prepared by the present embodiment contains magnesium corundum fireproof aggregate after testing: bulk density is 2.8 ~ 2.9g/cm3;Apparent porosity is 2 ~ 4%;Average pore size is 0.3 ~ 0.6 μm.
Embodiment
8
A kind of micro-closed pore of lightweight is containing magnesium corundum fireproof aggregate and preparation method thereof.γ-Al with 80 ~ 84wt%2O3The fine magnesium oxide micro-powder of fine powder, the nano alumina powder of 7 ~ 10wt% and 7 ~ 10wt% is raw material, the water of additional described raw material 50 ~ 70wt%, mixing, with planetary ball mill wet-milling 0.5 ~ 1.5 hour, obtains slip;Again described slip is placed in mould, places 12 ~ 24 hours under room temperature condition, the demoulding;Then the base substrate after the demoulding is dried 12 ~ 24 hours under the conditions of 150 ~ 200 DEG C, under the conditions of 1800 ~ 1900 DEG C, is incubated 1 ~ 5 hour, obtains lightweight micro-closed pore corundum fireproof aggregate in magnesium.
The micro-closed pore of lightweight prepared by the present embodiment contains magnesium corundum fireproof aggregate after testing: bulk density is 2.8 ~ 2.95g/cm3;Apparent porosity is 3 ~ 5%;Average pore size is 0.3 ~ 0.6 μm.
This detailed description of the invention compared with prior art has a following good effect:
The nano alumina powder that this detailed description of the invention introduces at high temperature can show superplasticity, under conditions of stress exists, this characteristic can make crystal boundary quickly move, the migration rate of crystal boundary is more than hole migration rate, in sintering process, crystal boundary can be closed before hole is excluded, thus forms a large amount of closed pore.Owing to superplasticity needs competence exertion effect under the promotion of stress, the fine magnesium oxide micro-powder that this detailed description of the invention introduces can react in-situ preparation spinelle with aluminum oxide, along with certain volumetric expansion in course of reaction, thus produces corresponding force in situ.The existence of this original position corresponding force can effectively promote the superplastic performance of nano aluminium oxide, thus form a large amount of closed pore, meanwhile, along with the movement of crystal boundary, macroscopic void is divided into Minute pores, thus reaches the purpose forming the micro-closed pore of lightweight containing magnesium corundum fireproof aggregate.Additionally, the In-suit spinel that the fine magnesium oxide micro-powder introduced is internally formed at aggregate, when with slag contacts, it is possible to the components such as effectively Fe, Mn in solid solution slag, promote aggregate slag resistance.
The micro-closed pore of lightweight prepared by this detailed description of the invention contains magnesium corundum fireproof aggregate after testing: bulk density is 2.8 ~ 3.15g/cm3, apparent porosity is 2 ~ 10%, and average pore size is 0.3 ~ 1 μm.
Therefore, the lightweight micro-closed pore corundum fireproof aggregate in magnesium prepared by this detailed description of the invention have that apparent porosity is low, closed porosity is high, bulk density is less, average pore size is little, thermal conductivity is relatively low, resistance to erosion and the strong feature of slag-resistant erosiveness.