Magnesium oxide whisker in-situ synthesis magnesium aluminate spinel enhanced magnesium-oxide-based foam ceramic filter and preparation method thereof

A technology of magnesium oxide-based ceramics and magnesium oxide whiskers, which is applied in the field of metal materials and metallurgy, can solve the problems of reduced chemical stability of bonding between grains, increased lattice distortion of matrix magnesium oxide, and operational limitations, and achieves excellent chemical stability. The effect of stability, simple process and good strength

Active Publication Date: 2018-09-04
JIANGSU FAVOUR AUTOMOTIVE NEW STUFF SCI TECH +1
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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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  • Magnesium oxide whisker in-situ synthesis magnesium aluminate spinel enhanced magnesium-oxide-based foam ceramic filter and preparation method thereof
  • Magnesium oxide whisker in-situ synthesis magnesium aluminate spinel enhanced magnesium-oxide-based foam ceramic filter and preparation method thereof

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Effect test

Embodiment 1

[0048] Account for the proportioning of 1% of the quality of the ceramic powder according to the magnesia whiskers, weighing the commercial magnesia whiskers and particle diameter is 250 orders (median diameter d 50 Prepare ceramic powder for 58 μm) fused magnesia powder; mix and prepare rheological agent according to the mass ratio of urea-formaldehyde resin and hydroxyethyl cellulose at a ratio of 1:4.

[0049] 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, rheological agent and appropriate amount of deionized water (the amount to be added according to the solid content of the ceramic slurry, the same below) to prepare a solution Add magnesium oxide whisker po...

Embodiment 2

[0053] According to the proportion that magnesium oxide whiskers account for 2% of the mass of ceramic powder, weigh commercial magnesium oxide whiskers (with a diameter of 2 to 5 μm and a length of 200 μm to 1000 μm) and a particle size of 500 mesh (median diameter d 50 Prepare ceramic powder for fused magnesia powder (25 μm); mix and prepare rheological agent according to the mass ratio of urea-formaldehyde resin and hydroxypropyl methylcellulose at a ratio of 1:4.

[0054] According to mass percentage, 20% of nano-aluminum 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 ratio, prepare the nano-aluminum sol, rheological agent and appropriate amount of deionized water into a solution, add the magnesia whisker powder, and ultrasonically treat the magnesia whiskers for 45 minutes to make the magnesia whiskers After the powder is fully dispersed...

Embodiment 3

[0058]Account for the proportioning of 1.5% of the ceramic powder quality according to the magnesia whiskers, weighing the commercial magnesia whiskers and particle diameter is 325 orders (middle diameter d 50 Prepare ceramic powder for fused magnesia powder (45 μm); mix and prepare rheological agent according to the mass ratio of urea-formaldehyde resin and hydroxyethyl cellulose at a ratio of 1:4.

[0059] According to mass percentage, 25% 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 fused magnesia powder into the ball mill tank according to the ratio, prepare a solution of nano-alumina sol, rheological agent and an appropriate amount of deionized water, add magnesia whiskers powder, and ultrasonically treat magnesia whiskers for 60 minutes to make the magnesia whiskers After the powder is fully dispersed in the solution, add it to the ball mill tank, and then add corundum balls accor...

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Abstract

The invention discloses a magnesium oxide whisker in-situ synthesis magnesium aluminate spinel enhanced magnesium-oxide-based foam ceramic filter with chemical stability and excellent thermal shock resistance capable of sintering in a low temperature and a preparation method thereof. The preparation method comprises the following steps: (1) according to a mass percent, compounding by 15%-25% of nano-aluminum sol, 0.8%-1.5% of rheological agent, and the balance of magnesia ceramics powder containing magnesium oxide whisker, adding deionized water, ball-milling, uniformly mixing, and preparing ceramic slurry of which the solid content is 60%-70% through vacuum exhaust; (2) immerging a polyurethane foamed plastic template in the ceramic slurry, extruding the polyurethane foamed plastic template through a roller press so as to remove redundant immerging slurry, preparing a biscuit, heating the biscuit to 80-120 DEG C, and drying; and (3) placing the dried biscuit in a sintering furnace, warming to 1400-1600 DEG C, and sintering in a high temperature, cooling to room temperature along with the furnace, to obtain the magnesium-oxide-based foam ceramic 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 magnesium oxide whisker-in-situ synthesized magnesium-aluminum spinel-reinforced magnesium oxide-based foam ceramic filter and a preparation method thereof, belonging to metal materials and metallurgical field. 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 categ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/66C04B35/04C04B38/06
CPCC04B35/04C04B35/66C04B38/067C04B2235/3217C04B2235/602C04B2235/5436C04B2235/5427C04B2235/6567C04B2235/6562C04B2235/656C04B2235/606C04B2235/5276C04B2235/96C04B38/0615C04B35/053C04B2235/5454C04B35/62625C04B35/6263C04B35/63476C04B35/6365C04B2235/3222C04B2235/763C04B2235/80C04B2235/85C04B38/00C04B2111/00793C04B2111/0087C04B2111/00879C04B2111/00887C04B2235/6028B01D39/2093C04B35/80C04B35/443
Inventor 刘思雨刘希琴刘子利李健
Owner JIANGSU FAVOUR AUTOMOTIVE NEW STUFF SCI TECH
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