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MA-MF composite spinel reinforced magnesium oxide based foam ceramic filter and preparation method thereof

A technology of magnesia-based ceramics and foam ceramics, which is applied in the field of metal materials and metallurgy, can solve the problems of reducing sintering temperature of magnesia ceramics, operating restrictions, increasing matrix distortion of magnesia matrix, etc., and achieves lower sintering temperature and good strength , The effect of simple process

Active Publication Date: 2018-09-18
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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Problems solved by technology

Chinese patent documents CN1011306B (pure magnesia foam ceramic filter and its preparation process), CN101138691A (preparation method of magnesia foam ceramic filter for casting), etc., prepare foam ceramics with pure magnesia as raw material, because MgO has a very high melting point and coefficient of thermal expansion (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 foam 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
Fluoride is a strong co-solvent and mineralizer commonly used in ceramic industry sintering, Chinese patent documents CN100536986C (magnesia foam ceramic filter), CN1473947A (foam ceramic for magnesium and magnesium alloy melt purification), CN101785944B (for magnesium Fluorite (melting point 1423°C) and magnesium fluoride (melting point 1248°C) are added to the preparation method of magnesium oxide foam ceramic filter for magnesium melt filtration. The solid solution of fluoride not only increases the oxidation of the matrix during the sintering process The lattice of magnesium is distorted, and it is easy to form a low-melting liquid phase, thereby reducing the sintering temperature of magnesia ceramics; however, during the sintering process, F in fluoride combines with Si, Al, Fe, and Ca, and most (in ceramic tiles) About 70% in production) volatilization in gaseous form not only erodes the green body itself and damages the quality of sintered ceramics, but more seriously, it will cause fluoride pollution when discharged into the atmosphere. Fluoride can enter the human body through the respiratory tract, digestive tract and skin , has a toxic effect on the central nervous system and myocardium, and low-concentration fluorine pollution can lead to brittle calcification of teeth and bones. The discharge standard of fluoride must be lower than 5.0mg / m2 in the "Ceramic Industry Pollutant Discharge Standard" (GB25464-2010) 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 flux inclusions in the magnesium melt
Water glass, silica sol and ethyl silicate are used as binders in the preparation slurry of the disclosed ceramic foam filters such as Chinese patent literature CN101138691A, and the SiO between the sintered ceramic foam particles 2 The presence of components makes it easy to react with magnesium and its alloy melts according to (4), which also reduces the chemical stability of foamed ceramics
However, diboron trioxide is easy to react with magnesium and aluminum, and is not stable in magnesium and aluminum alloy melts; at the same time, because diboron trioxide is soluble in solvents such as water and ethanol, it can strongly absorb water in the air to form boric acid. The diboron trioxide added in the preparation process of foam ceramics is dissolved in water to form a boric acid aqueous solution, which is easy to react with magnesium oxide to form magnesium borate precipitation and reduce its effect
Gallium oxide is a homogeneous oxide of diboron trioxide, which forms spinel-type MgGa with magnesium oxide at a lower temperature 2 o 4 It plays a role in reducing the sintering temperature, but the amount of gallium resources is very small (gallium is a strategic reserve metal), and the high price of gallium oxide limits its application in ordinary ceramics.

Method used

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  • MA-MF composite spinel reinforced magnesium oxide based foam ceramic filter and preparation method thereof
  • MA-MF composite spinel reinforced magnesium oxide based foam ceramic filter and preparation method thereof

Examples

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Effect test

Embodiment 1

[0048] Account for the proportioning of 1% of the ceramic powder quality according to nanometer ferric oxide, be that the nanometer ferric oxide of 30nm and particle diameter are 250 orders (middle diameter d 50 58 μm) light-burned magnesia powder was mixed to prepare ceramic powder; the mass ratio of polyvinyl butyral and hydroxypropyl methylcellulose was mixed to prepare a rheological agent at a ratio of 1:1.

[0049] According to mass percentage, 25% of nano-alumina sol with a solid content of 25% (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 light-burned magnesia powder into the ball mill tank according to the proportioning ratio, and add nano-alumina sol, nano-ferric oxide, rheological agent and an appropriate amount of absolute ethanol (the addition amount is determined according to the solid content of the ceramic slurry, the following Mix wit...

Embodiment 2

[0053] Account for the proportioning of 2% of the ceramic powder quality according to nanometer ferric oxide, be that the nanometer ferric oxide of 60nm and particle diameter are 500 orders (middle diameter d 50 The ceramic powder is prepared by mixing lightly burned magnesia powder with a thickness of 25 μm; the rheological agent is prepared by mixing the mass ratio of polyvinyl butyral and hydroxypropyl methylcellulose at a ratio of 1:1.

[0054] According to mass percentage, 15% of nano-alumina sol with a solid content of 20%, 1.5% of rheological agent, and the rest are ceramic powder for batching. First, add the light-burned magnesia powder into the ball mill tank according to the proportion, mix the nano-aluminum sol, nano-ferric oxide, rheological agent and an appropriate amount of absolute ethanol and ultrasonically treat it for 60 minutes to fully disperse the nano-lanthanum oxide powder Then add it into the ball mill jar, then add corundum balls according to the ratio...

Embodiment 3

[0058]Account for the proportioning of 1.5% of the ceramic powder quality according to nanometer ferric oxide, be that the nanometer ferric oxide of 50nm and particle diameter are 325 orders (medium diameter d 50 The ceramic powder is prepared by mixing light-burned magnesia powder with a thickness of 45 μm; the rheological agent is prepared by mixing the mass ratio of polyvinyl butyral and hydroxyethyl cellulose at a ratio of 1:1.

[0059] According to mass percentage, 20% of nano-alumina sol with a solid content of 22%, 1.0% of rheological agent, and the rest are ceramic powder for batching. First, add the light-burned magnesia powder into the ball mill tank according to the proportion, mix the nano-alumina sol, nano-ferric oxide, rheological agent and an appropriate amount of absolute ethanol and ultrasonically treat it for 45 minutes to fully disperse the nano-lanthanum oxide powder Then add it into the ball mill tank, then add corundum balls according to the ratio of ball...

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Abstract

The invention discloses a MA-MF composite spinel reinforced magnesium oxide based foam ceramic filter capable of realizing low temperature sintering and excellent chemical stability and thermal shockresistance and a preparation method thereof, the preparation method comprises the following steps: (1) proportioning 15% to 25% by mass of nano-aluminum sol, 0.8% to 1.5% by mass of a rheological agent, and balance of magnesium oxide ceramic powder containing a nano-ferric oxide sintering aid, and adding anhydrous ethanol for even mixing by ball milling to obtain ceramic slurry having a solid content of 60% to 70%; (2) immersing a polyurethane foam plastic template into the ceramic slurry, extruding the polyurethane foam plastic template by a roll press to remove excess immersing slurry to obtain a green body, and removing an ethanol solvent in a ventilating chamber at 40 DEG C to 50 DEG C to dry the green body; and (3) putting the dried green body in a sintering furnace, heating to 1350 to 1550 DEG C for high temperature sintering, and cooling in the furnace to room temperature to obtain the magnesium oxide based ceramic foam filter.

Description

technical field [0001] The invention relates to a magnesium oxide-based foam ceramic filter and a preparation method thereof, in particular to a MA-MF composite spinel-reinforced magnesium oxide-based foam ceramic filter and a preparation method thereof, belonging to the field of metal materials and metallurgy. The filter prepared by the invention is particularly suitable for filtering and purifying magnesium and its alloy melts, and can also be used for filtering and purifying aluminum and its alloy melts. Background technique [0002] Magnesium is chemically active. During casting and processing, it is very easy to chemically react with oxygen, nitrogen and water vapor. The resulting products remain in the magnesium, affecting the internal quality of the product and deteriorating the performance of the product. According to the types and properties of inclusions in magnesium alloys, inclusions are generally divided into two categories: metal inclusions and non-metal inclus...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/053C04B35/63C04B35/634C04B35/636C04B35/64C04B38/06B01D39/20C04B35/66
CPCB01D39/2093C04B35/053C04B35/6303C04B35/63416C04B35/6365C04B35/64C04B35/66C04B38/0615C04B2235/3218C04B2235/322C04B2235/3222C04B2235/3272C04B2235/5436C04B2235/5454C04B2235/6562C04B2235/6567
Inventor 刘希琴刘子利刘思雨
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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