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Alumina short fiber-reinforced magnesium oxide-based crucible and preparation method thereof

A magnesia-based and alumina-based technology is applied to magnesia-based crucibles and preparations thereof, alumina short fiber reinforced magnesia-based crucibles and preparations thereof, and the field of magnesium and its alloy smelting, which can solve the problem of chemical stability between grains It can reduce the sintering temperature of magnesia ceramics, increase the burden of environmental protection investment and other problems, so as to achieve good chemical stability and improve mechanical properties.

Active Publication Date: 2018-09-18
FENGYANG L S NET FORMING CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent document CN103030407B (a kind of preparation method of high-strength, high-density, high-purity magnesia crucible), Chinese patent document CN1011306B (pure magnesia foam ceramic filter and its preparation process) etc. use pure magnesia as raw material to prepare magnesia Ceramics, because MgO has a high melting point and thermal expansion coefficient (13.5×10 -6 / °C) is high, therefore, it leads to difficult sintering (sintering temperature is not lower than 0.8 times its melting point) and poor thermal shock resistance, which limits the application and development of MgO ceramics
add V 2 o 5 In powder form, MgO will react with V at 1190°C 2 o 5 form an approximate composition of Mg 3 V 2 o 8 The liquid phase promotes sintering and can significantly reduce the sintering temperature of MgO foam ceramics, but V 2 o 5 Harmful to the respiratory system and skin during use, and has strict restrictions on operation
with V 2 o 5 Similarly, cobalt oxide is also a good low-temperature sintering aid, but its application is limited as a highly toxic substance and rare resource
Add fluorite (melting point 1423 ℃) and magnesium fluoride ( Melting point 1248°C), the solid solution of fluoride not only increases the lattice distortion of the matrix magnesium oxide during the sintering process, but also easily forms a low melting point liquid phase, thereby reducing the sintering temperature of the magnesia ceramics; however, during the sintering process F in fluoride is combined with Si, Al, Fe, Ca, and most of them (about 70% in ceramic tile production) volatilize in gaseous form, which not only corrodes the green body itself and damages the quality of sintered ceramics, but more seriously, it is discharged to The atmosphere will cause fluoride pollution. Fluoride can enter the human body through the respiratory tract, digestive tract and skin, and has toxic effects on the central nervous system and myocardium. Low-concentration fluorine pollution will cause brittle calcification of teeth and bones. "(GB25464-2010) stipulates that the discharge standard of fluoride must be lower than 5.0mg / m 3 Therefore, using fluoride as a low-temperature sintering aid for magnesia ceramics will inevitably increase the emission of gaseous fluoride and increase the burden of environmental protection investment; in addition, fluoride ions in the residual solid-solution fluoride in ceramics exist in the form of replacing oxygen ions, resulting in crystal The chemical stability of the intergranular bonding is reduced, and it is difficult to resist the long-term erosion of the flux in the magnesium melt
Chinese patent literature CN104496492B (a composite magnesium-carbon refractory crucible and its preparation method) and other disclosed ceramic foam filter preparation slurry adopts silica sol etc. 2 The presence of components makes it easy to react with magnesium and its alloy melts according to formula (4), which also reduces the chemical stability of ceramics
Although the crucible formed by isostatic pressing has the advantages of high density and high yield, and the crucible body is not easily deformed during the sintering process, it is also found that the crucible formed by isostatic pressing has the advantages of high cost, low efficiency, poor thermal stability, rapid heating and During the cooling process, the crucible is prone to cracking and peeling, and the service life is short

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  • Alumina short fiber-reinforced magnesium oxide-based crucible and preparation method thereof
  • Alumina short fiber-reinforced magnesium oxide-based crucible and preparation method thereof

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Embodiment 1

[0055] According to the proportion of nano-lanthanum oxide in the mass percentage of ceramic powder as 1%, alumina short fiber as 1%, and the rest as fused magnesia, the nano-lanthanum oxide with a particle size of 60nm and the commercialized small aspect ratio polycrystalline Al 2 o 3 Short fibers (diameter 10μm-20μm, length 50μm-100μm) and particle size 250 mesh (median diameter d 50 The ceramic powder is prepared by mixing fused magnesia powder with a thickness of 58 μm; the rheological agent is prepared by mixing the mass ratio of polyvinyl alcohol and hydroxyethyl cellulose at a ratio of 2:3.

[0056] According to mass percentage, 15% of nano-alumina sol with a solid content of 20% (select a commercial nano-alumina sol with a nearly neutral pH value, the same below), 0.8% of rheological agent, and the rest are ceramic powders for batching. First, add the fused magnesia powder into the ball mill tank according to the proportion, and prepare the nano-aluminum sol, rheolog...

Embodiment 2

[0061] According to the ratio of nano-lanthanum oxide to the mass percentage of ceramic powder as 3%, alumina short fiber as 3%, and the rest as fused magnesia, the nano-lanthanum oxide with a particle size of 30nm and the commercialized small aspect ratio polycrystalline Al 2 o 3 Short fibers (diameter 10 μm ~ 20 μm, length 50 μm ~ 100 μm) and particle size 500 mesh (median diameter d 50 Mix and prepare ceramic powder with fused magnesia powder (25 μm); mix and prepare rheological agent according to the mass ratio of polyvinyl alcohol and hydroxypropyl cellulose at a ratio of 2:3.

[0062] According to mass percentage, 25% of nano-alumina sol with a solid content of 25%, 1.5% of rheological agent, and the rest are ceramic powder for batching. First, add the fused magnesia powder into the ball mill tank according to the proportion, prepare a solution from nano-aluminum sol, rheological agent and appropriate amount of deionized water, then add nano-lanthanum oxide and alumina...

Embodiment 3

[0067] According to the ratio of nano-lanthanum oxide to the mass percentage of ceramic powder as 2%, alumina short fiber as 2%, and the rest as fused magnesia, the nano-lanthanum oxide with a particle size of 45nm and the commercialized small aspect ratio polycrystalline Al 2 o 3 Short fibers (diameter 10μm-20μm, length 50μm-100μm) and particle size 325 mesh (median diameter d 50 Mix and prepare ceramic powder with fused magnesia powder (45 μm); mix and prepare rheological agent according to the mass ratio of polyvinyl alcohol and hydroxyethyl cellulose at a ratio of 2:3.

[0068] According to mass percentage, 20% of nano-alumina sol with a solid content of 22%, 1% of rheological agent, and the rest are ceramic powder for batching. First, add the fused magnesia powder into the ball mill tank according to the ratio, prepare a solution from nano-alumina sol, rheological agent and an appropriate amount of deionized water, then add nano-lanthanum oxide and alumina short fiber, ...

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Abstract

The invention discloses an alumina short fiber-reinforced magnesium oxide-based crucible which is excellent in chemical stability and thermal shock resistance, and can realize sintering at a low temperature and a preparation method thereof, the method comprises the following steps: (1) proportioning, by mass, 15% to 25% of nano-aluminum sol, 0.8% to 1.5% of a rheological agent, and balance of electro-fused magnesium oxide ceramic powder containing nano-lanthana and alumina short fiber, adding an appropriate amount of deionized water, uniformly mixing by ball milling, and vacuum degassing to obtain a ceramic slurry having a solid content of 70% to 80%; (2) preparing a crucible biscuit; (3) preparing a crucible blank; and (4) putting the magnesium oxide-based crucible blank in the aluminum sol for vacuum impregnation treatment, grinding the surface, drying, performing high-temperature secondary sintering at a temperature of 1400 to 1600 DEG C, and cooling in a furnace to room temperatureto obtain the magnesia-based crucible.

Description

technical field [0001] The invention relates to a magnesium oxide-based crucible and a preparation method thereof, in particular to an alumina short fiber reinforced magnesium oxide-based crucible and a preparation method thereof, belonging to the field of metal materials and metallurgy. The magnesium oxide-based crucible prepared by the invention is particularly suitable for smelting magnesium and its alloys. Background technique [0002] In recent years, the demand for lightweight has led to the rapid development of the application of magnesium alloys and aluminum alloys. Whether it is wrought magnesium, aluminum alloys or cast magnesium, aluminum alloys, the production is inseparable from casting equipment. The chemical properties of magnesium are lively, and it is easy to react with oxygen, nitrogen and water vapor. It is easy to be oxidized and burned during the melting and refining process, and the product remaining in the magnesium will deteriorate the internal qualit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/053C04B35/80C04B35/634C04B35/636C04B35/63C04B35/622C04B41/87C04B35/66
CPCC04B35/803C04B35/053C04B35/622C04B35/6303C04B35/63416C04B35/6365C04B35/66C04B41/009C04B41/5031C04B41/87C04B2235/3218C04B2235/322C04B2235/3222C04B2235/3227C04B2235/5224C04B2235/6022C04B35/04C04B41/4537
Inventor 刘子利刘希琴叶兵刘思雨丁之光丁文江
Owner FENGYANG L S NET FORMING CO LTD
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