CN108484181A - Short fine magnesium oxide-based ceramic foam filter of enhancing of a kind of aluminium oxide and preparation method thereof - Google Patents

Short fine magnesium oxide-based ceramic foam filter of enhancing of a kind of aluminium oxide and preparation method thereof Download PDF

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Publication number
CN108484181A
CN108484181A CN201810307628.4A CN201810307628A CN108484181A CN 108484181 A CN108484181 A CN 108484181A CN 201810307628 A CN201810307628 A CN 201810307628A CN 108484181 A CN108484181 A CN 108484181A
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China
Prior art keywords
aluminium oxide
ceramic
oxide
short fine
magnesium oxide
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CN201810307628.4A
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Chinese (zh)
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CN108484181B (en
Inventor
刘子利
刘思雨
刘希琴
李健
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Jiangsu Favour Automotive New Stuff Sci-Tech Co Ltd
Nanjing University of Aeronautics and Astronautics
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Jiangsu Favour Automotive New Stuff Sci-Tech Co Ltd
Nanjing University of Aeronautics and Astronautics
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Application filed by Jiangsu Favour Automotive New Stuff Sci-Tech Co Ltd, Nanjing University of Aeronautics and Astronautics filed Critical Jiangsu Favour Automotive New Stuff Sci-Tech Co Ltd
Priority to CN201810307628.4A priority Critical patent/CN108484181B/en
Priority to PCT/CN2018/089570 priority patent/WO2019196181A1/en
Publication of CN108484181A publication Critical patent/CN108484181A/en
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    • C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Filtering Materials (AREA)

Abstract

The invention discloses it is a kind of can realize at low temperature sintering, chemical stability and thermal shock resistance it is excellent aluminium oxide it is short it is fine enhance magnesium oxide-based ceramic foam filter and preparation method thereof, which includes the following steps：(1) according to mass percent by 15%~25% nanometer of Aluminum sol, 0.8%~1.5% rheological agent, remaining carries out dispensing for salic short fine, nano-titanium dioxide magnesia ceramics powder, and the ceramic slurry that solid content is 60%~70% is made after addition absolute ethyl alcohol ball milling mixing is uniform；(2) polyurethane foam plastics masterplate is immersed in ceramic slurry, is squeezed after polyurethane foam plastics masterplate removes extra leaching hanging material by roll squeezer and biscuit is made, then so that biscuit is dried in 40 DEG C~50 DEG C draft chamber's removal alcohol solvents；(3) dry biscuit is put into sintering furnace, high temperature sintering is carried out at a temperature of being warming up to 1350 DEG C~1550 DEG C, cooled to room temperature with the furnace and obtain magnesium oxide-based ceramic foam filter.

Description

Short fine magnesium oxide-based ceramic foam filter of enhancing of a kind of aluminium oxide and preparation method thereof
Technical field
The present invention relates to a kind of magnesium oxide-based ceramic foam filter and preparation method thereof, specifically a kind of short fibre of aluminium oxide Enhance magnesium oxide-based ceramic foam filter and preparation method thereof, belongs to metal material and field of metallurgy.Prepared by the present invention Filter can also be used for the filtration, purification of aluminium and its alloy melt especially suitable for magnesium and its filtration, purification of alloy melt.
Background technology
The chemical property of magnesium is active, in casting and process, is easily chemically reacted with oxygen, nitrogen and vapor, The product of generation remains in magnesium, influences the internal soundness of product, deteriorates product properties.According to the type of field trash in magnesium alloy And property, field trash is generally divided into metal inclusion and nonmetal inclusion two major classes：(1) metallic inclusion：Magnesium alloy is in former magnesium During production and post-production, it can inevitably introduce some metal simple-substances or metallic compound is mingled with, they are with grain The forms such as sub- shape, tufted remain on the matrix or crystal boundary of magnesium alloy, and main includes metal simple-substance α-Fe particles, manganese-iron Metallic compound such as (Fe, Mn)3Si, (Fe, Mn)5Si3Deng；(2) non-metallic inclusion：Nonmetal inclusion owner in magnesium alloy It will be based on the oxynitrides of magnesium, such as MgO, Mg3N2Deng；Magnesium alloy added in fusion process with chloride (KCl, NaCl, MgCl2Deng) based on refining agent, flux cannot completely remove in refining process, and having a small amount of flux remains in Serum Magnesium, Magnesium metal flux is caused to be mingled with.The oxide inclusion of suspension is pushed to crystal boundary in crystallization by crystallization front, and field trash is generally with thin Membranaceous, particle shape, the form of tufted remain in magnesium alloy grain boundaries.There is statistics to show that MgO accounts for all of magnesium alloy and is mingled with 80% or more of object, distributional pattern are film-form, particle shape and tufted.The field trash generated in Normal Casting of Magnesium Alloy is not only tight Deteriorate the mechanical property and corrosion resisting property of alloy again, and reduces the surface quality of its machining and anodized.It is right For diecast magnesium alloy, the content of film-form and particle shape oxide inside alloy needs to control in 100cm2/ kg and 100mm3/ kg or less could meet normal requirement.Therefore, the field trash in Serum Magnesium is removed in fusion-casting process to carry The purification technique of the degree of purity of high melt becomes the key of magnesium alloy production.
Cleaning molten technique can be divided into flux refining and non-flux purification two major classes.Flux refining technique is because of dust removal rate It is high, at low cost, easy to operate and as the purification technique that generally uses in magnesium alloy production, but there is also gold for flux refining Category loss increases, flux is mingled with, is unable to the deficiencies of degasification, and especially in melting magnesium-rare earth, flux can also be consumed largely Rare earth element in alloy.Non-flux purification technique not only can overcome the disadvantages that the deficiency of flux refining technique but also have excellent purification Effect becomes the important cleaning molten technique of current application development and develops filtration, purification, rotary blowing purification, electromagnetism in succession A variety of non-flux purification technologies such as purification, ultrasonication.Compared to simple metal mesh melt filtration, have special three-dimensional more Hole ceramic structure ceramic foam filter, because of its porosity high (70%~90%), adsorption capacity is strong, the spies such as resistant to chemical etching Point can have filtering well by filter cake effect, adsorption effect and rectifying effect to the inclusion particle in alloy melt Effect.Foam ceramic filter method can not only filter as low as 10 μm~20 μm in alloy melt of microinclusions particle, and The liquid flux that general filter medium is difficult to filter out can be filtered out to be mingled with.
American documentation literature US3962081A (Ceramic foam filter), US4024212A
(Ceramic foam and method of preparation), a kind of Chinese patent literature CN103787691A (oxygen Change aluminum foam ceramics preparation method) etc. all disclose some for aluminium alloy, steel fusant filtering field trash Al2O3, ZrO2, SiC, SiO2The method of base foamed ceramics, however, the standard of MgO generates, free enthalpy is very low, and the very high Serum Magnesium of activity is non- It is often easy to react with foamed ceramics basis material generation (1)~(4) formula and dissolve rapidly, filter hole or corrode to block it Become harmful components in into magnesium and its alloy melt, therefore, the foam filters of these existing materials be not suitable for magnesium and The filtering of magnesium alloy fused mass.
3Mg(l)+Al2O3(s)=3MgO(s)+2Al(l) (1)
2Mg(l)+ZrO2(s)=2MgO (s) (2)+Zr (s)
6Mg (l)+4Al (l)+3SiC (s)=3Mg2Si(s)+Al4C3(s) (3)
4Mg(l)+SiO2(s)=2MgO (s)+Mg2Si(s) (4)
MgO is cubic system NaCl type structures, and lattice constant 0.411nm belongs to ion key compound, and fusing point is 2852 DEG C, it is far above common Al2O3(2054 DEG C) and SiO2(1650 ± 50 DEG C), therefore, magnesia product have goodization It learns stability, high resistivity and has the characteristics such as stronger corrosion resistance to metal, slag and alkaline solution.With it is common Ceramic material is compared, and MgO has good stability at elevated temperature, villaumite and fluorate with melting with magnesium and its alloy melt The flux mixture of composition does not react, and is mingled with the flux in the smaller and easy absorption Serum Magnesium of angle of wetting with flux and presss from both sides Miscellaneous, therefore, MgO material foamed ceramicses are the ideal materials of liquid magnesium alloy melting and purifying.
Carried out under the melting temperature formed less than oxide firing prepare necessary to ceramic material, most critical Step, and the sintering that is occurred at high temperature, crystal grain are grown up etc., processes decide the microscopic structure and performance of ceramic material.China Patent document CN1011306B (filter of purifying magnesium oxide foam pottery and its reparation technology), CN101138691A (casting magnesium The preparation method of foam ceramic filter) etc. prepare foamed ceramics using pure zirconia magnesium as raw material, because MgO have very high fusing point With coefficient of thermal expansion (13.5 × 10-6/ DEG C) high, therefore, cause its sintering difficult (sintering temperature is not less than 0.8 times of its fusing point) It is poor with thermal shock resistance, limit the application and development of MgO foamed ceramicses.
Research shows that：Firing temperature often reduces by 100 DEG C during being sintered ceramics, unit product heat consumption can reduce by 10% with On, it is the important technical for reducing MgO foamed ceramics sintering temperatures by adding sintering aid.Add V2O5When powder, MgO Meeting and V at 1190 DEG C2O5Formation proximate composition is Mg3V2O8Liquid phase, acceleration of sintering can significantly reduce MgO foamed ceramicses Sintering temperature, but V2O5There is detrimental effect to respiratory system and skin in use, has stringent limitation to operation. With V2O5Identical, cobalt oxide is also good low-temperature sintering auxiliary agent, but also limits application as highly toxic substance and scarce resource. Fluoride is common strong cosolvent and mineralizer, Chinese patent literature CN100536986C (magnesia in ceramic industry sintering Foam ceramic filter), CN1473947A (magnesium and magnesium alloy fused mass purification foamed ceramics), CN101785944B (be used for The preparation method of magnesium and Serum Magnesium filtering magnesia ceramic foam filter) in addition fluorite (1423 DEG C of fusing point) and magnesium fluoride (1248 DEG C of fusing point), in sintering process the solid solution of fluoride not only increase the distortion of lattice of matrix magnesia, and itself Low melting point liquid phase is easily formed, to reduce the sintering temperature of magnesia ceramics；However, F in sintering process in fluoride with Si, Al, Fe, Ca are combined, most of (accounting for about 70% in ceramic tile production) volatilize in a gaseous form not only itself corrode green body and Damage sintering ceramics quality, fluoride pollution can be caused by being more seriously discharged into air, fluoride can through respiratory tract, Alimentary canal and skin enter human body, Central nervous system, the toxic effect of cardiac muscle, and low dose fluoride pollution can lead to tooth and bone The crisp calcification of bone,《Ceramic industry pollutant emission standard》(GB25464-2010) discharge standard of regulation fluoride has to be lower than in 5.0mg/m3, the low-temperature sintering auxiliary agent using fluoride as magnesia ceramics necessarily increases the discharge of vapor-phase fluoride and aggravates ring Protect input burden；In addition, fluorine ion is existed in the form of replacing oxonium ion in remaining solid solution fluoride in ceramics, crystalline substance is caused The chemical stability that intergranular combines reduces, it is difficult to resist the long-time that flux in Serum Magnesium is mingled with and corrode.Chinese patent literature Preparing for ceramic foam filter disclosed in CN101138691A etc. uses waterglass, Ludox and silester conduct in slurry Bonding agent, SiO between the foamed ceramics particle of sintering2The presence of ingredient makes it easily be reacted by (4) formula with magnesium and its alloy melt, Equally reduce the chemical stability of foamed ceramics.(magnesium oxide foam ceramic filters Chinese patent literature CN100536986C Device), in the patent documents such as CN103553686A (a kind of magnesium aluminate spinel foamed ceramic filter and preparation method thereof), three oxygen Change the low-temperature sintering auxiliary agent of two boron and borax as magnesia ceramics, diboron trioxide forms liquid phase when being higher than 450 DEG C, burning When junction temperature is more than 1350 DEG C, is reacted with magnesia and generate antifungin so that liquid form exists and reduces sintering temperature.However, Diboron trioxide is in magnesium, aluminium alloy melt and unstable easily with magnesium, reactive aluminum；Simultaneously as diboron trioxide be dissolved in water and Ethyl alcohol equal solvent can consumingly absorb water generate boric acid in air, three oxidations two added in the preparation process of foamed ceramics Boron is dissolved in water and forms boric acid aqueous solution, easily reacts to form boric acid magnesium precipitate and reduce its effect with magnesia.Gallium oxide is three oxygen Change the oxide of the same clan of two boron, forms the MgGa of spinel-type with magnesia at a lower temperature2O4And play reduction sintering temperature The effect of degree, but gallium stock number is seldom (gallium is strategic reserves metal), the higher price limit of gallium oxide its in conventional ceramic In application.
Invention content
The object of the present invention is to provide it is a kind of can realize at low temperature sintering, chemical stability and thermal shock resistance it is excellent Short fine magnesium oxide-based ceramic foam filter of enhancing of aluminium oxide and preparation method thereof.
In order to reach above-mentioned technical purpose, the technical scheme is that：
The short fine magnesium oxide-based ceramic foam filter of enhancing of a kind of aluminium oxide, by salic short fine, nano-titanium dioxide Light calcined magnesia base ceramic slurry be coated in polyurethane foam carrier on, through drying, sintering obtain.
A kind of short fine preparation method for enhancing magnesium oxide-based ceramic foam filter of aluminium oxide, includes the following steps：
(1) according to mass percent by 15%~25% nanometer of Aluminum sol, 0.8%~1.5% rheological agent, remaining is oxygen-containing Change short fine, nano-titanium dioxide the magnesia ceramics powder of aluminium and carry out dispensing, is made after addition absolute ethyl alcohol ball milling mixing is uniform The ceramic slurry that solid content is 60%~70%.The nanometer Aluminum sol of addition is not only by light calcined magnesia particle, nanometer titanium dioxide Titanium and aluminium oxide it is short it is fine bonded together by forming continuous film, can play the role of binder, and with high degree of dispersion Nano-titanium dioxide powder reacts generation with magnesium oxide powder particle in-situ together has chemical stabilization to magnesium and its alloy melt Property Spinel, avoid existing product and Ludox, the binders such as silester be added to foamed ceramics chemical stability Damage.
Solid-phase component is the porous gamma-Al of high activity in Aluminum sol2O3, with magnesium aluminate spinel (MgAl2O4) crystal structure phase Together.The mechanical property of ceramic matric composite can be improved as reinforcement using fiber and whisker.
The rheological agent is the mixture of polyvinyl butyral and cellulose ether, wherein the polyvinyl butyral accounts for The 50% of rheological agent quality, cellulose ether is industrial hydroxypropyl methyl cellulose, one kind in hydroxyethyl cellulose or it is mixed Close object.Cellulose ether and the polyvinyl butyral not still fine dispersion agent of the short fine powder of nano-titanium dioxide, aluminium oxide, energy It enough prevents slurry from generating agglomeration, and bonding agent can be played the role of when preparing biscuit, slurry can be comparatively after dipping Being firmly attached on polyurethane foam plank makes biscuit have prodigious intensity, while easily being escaped without dirt in sintering process Dying product, hereby it is ensured that the quality of ceramic foam filter.Sodium carboxymethylcellulose etc. is not used to contain the salt received in rheological agent Class avoids the larger Na of remaining ionic radius+To the obstruction of ceramic post sintering.
The ceramic powder is the mixture of light calcined magnesia, nano-titanium dioxide and the short fibre of aluminium oxide.Wherein, described to receive Rice titanium oxide accounts for the 1%~2% of ceramic powder quality, and the short fibre of aluminium oxide accounts for the 1%~3% of ceramic powder quality, described Nano-titanium oxide grain size is 30~60nm, and short fine select of the aluminium oxide is commercialized small draw ratio polymorph A l2O3Staple fiber is straight Diameter is 10 μm~20 μm, and length is 50 μm~100 μm.The grain size of the light calcined magnesia powder is the mesh (central diameter of 250 mesh~500 d50It it is 25 μm~58 μm).
Light calcined magnesia fine powder of use itself has very high sintering activity, and nanometer titanium dioxide is added in ceramic composition Titanium, titanium ion diffuse into periclase grain boundary, form Ti4+Ion exchange Mg2+The solid solution of ion and promote intergranular direct In conjunction with.Al2O3Lattice constant it is close with MgO, can be dissolved into MgO lattices in sintering process and to cause MgO crystal to occur brilliant Lattice distort；Al3+Diffusion velocity it is small, Al2O3Solubility very little (Al in periclase MgO2O31700 DEG C in periclase MgO When solubility only 3%), nanometer Aluminum sol, which can be dissolved into sintering process in the light-burned MgO lattices of high activity, makes MgO crystal Distortion of lattice occurs, activates lattice, while generating new compound-magnesium aluminate spinel by reaction-sintered between MgO particles MgAl2O4Phase, to promote sintering and the alternate combination of particle.On the other hand, nano-powder has large specific surface area, surface The features such as energy height, high activity, therefore, nano-powder is easy to be combined with other atoms, therefore its fusing point and sintering temperature compare micro mist It is much lower.The sintering aid being added in the form of nano-titanium oxide and nanometer Aluminum sol can fill between raw material micro powder granule Gap optimizes ceramic particle grading and mixing uniformity, meanwhile, nano-powder is received because of the surface and interface effect of its own Nanometer γ-the Al of high reaction activity in rice titanium oxide and Aluminum sol2O3Keep reaction speed fast with coming into full contact with for light-burned MgO particles Speed improves, and reduces sintering temperature, improves the consistency and mechanical property of ceramics, and the reduction of sintering temperature advantageously reduces energy The production cost of consumption and ceramic foam filter.
Height is sintered active light calcined magnesia particle and the short fibre of nano-titanium dioxide, aluminium oxide of high degree of dispersion is continuous Nano aluminum dissolved glue film surrounds, and reaction in-situ generates magnesium aluminate spinel MA and magnesium ulvospinel M in sintering process2T-phase, MA and M2T It dissolves each other completely at 1350 DEG C or more, in sintering process that cristobalite MgO crystal grain is directly fused together, precipitation is precipitated while cooling Intergranular secondary spinel (intergranular spinelle) M2T and MA can compensate for the stress on each phase critical surface, make material when being burnt into cooling The stress relaxation of generation.
Preferably, the nanometer Aluminum sol solid content is 20%~25%, pH value >=4.
The preparation method of the ceramic slurry is：Light calcined magnesia powder is added in ball grinder according to proportioning, by nanometer The short fine, rheological agent of Aluminum sol, nano-titanium dioxide, aluminium oxide and absolute ethyl alcohol are mixed and sonicated for 30min~60min, make It is added in ball grinder after the short fibre of aluminium oxide is fully dispersed, according still further to ratio of grinding media to material 2:Corundum ball is added in 1 ratio, with 60~ 120rpm rotating speed ball millings 2h~4h make its be uniformly mixed obtain.
(2) polyurethane foam plastics masterplate is immersed in ceramic slurry, polyurethane foam plastics is squeezed by roll squeezer Biscuit is made after removing extra leaching hanging material in masterplate, then keeps biscuit dry in 40 DEG C~50 DEG C draft chamber's removal alcohol solvents It is dry.
When squeezing the polyurethane foam plastics masterplate of leaching hanging material by roll squeezer, the short fibre of aluminium oxide in made biscuit It is arranged to a certain extent along rolling direction, the form of the short fibre of aluminium oxide with certain orientation is brilliant by being formed by magnalium point Stone is mutually inherited, and therefore, the Spinel of package periclase MgO crystal grain makes have the group combined closely between the ceramic crystalline grain of sintering It knits, and the pinning effect of Spinel inhibits the growth of magnesium oxide particle, to refine the tissue of foamed ceramics and carry Consistency between high ceramic crystalline grain.
The polyurethane foam plastics masterplate specification is 10PPI~20PPI (Pores per inch, inches length On average number of pores)；Using it is preceding impregnated in 40 DEG C~50 DEG C of 15%~20%NaOH aqueous solutions surface etch 40min~ Naturally dry is washed with clear water after 60min, after being then immersed in the aqueous solution of 2%~4% dodecyl benzene sulfonic acid wetting agent It is obtained after taking out drying.Make its surface roughening by NaOH etchings, then passes through the water-soluble of dodecyl benzene sulfonate wetting agent After liquid processing, ceramic slurry, which is easy to uniformly apply, to be suspended on polyurethane foam plank.
(3) dry biscuit is put into sintering furnace, high temperature sintering is carried out at a temperature of being warming up to 1350 DEG C~1550 DEG C, with Stove is cooled to room temperature to obtain magnesium oxide-based ceramic foam filter.
The sintering process is to be heated to 550 DEG C with the heating rate of 30 DEG C/h to make having in ceramic foam filter biscuit Machine object (polyurethane foam and rheological agent etc.) decomposition gasification is discharged, and is then heated to 1100 DEG C of temperature with the heating rate of 200 DEG C/h Degree, in the low-temperature sintering stage, lower heating rate can prevent polyurethane foam and rheological agent decomposition rate is too fast leads to element Base collapses or deformed damaged.1350 DEG C~1550 DEG C temperature are finally heated to the heating rate of 50 DEG C/h and are protected at such a temperature 2~3h of temperature.In the high temperature sintering stage, sintering temperature is more than after 1100 DEG C, and lower heating rate can ensure in sintered body Temperature is consistent, while avoiding the formation speed for generating spinelle uniform and the transformation stress of too fast generation is avoided to cause sintered body Deformation and cracking.
The short fine preparation method for enhancing magnesium oxide-based ceramic foam filter of aluminium oxide provided by the present invention has technique Simply, the advantages that at low cost, efficient, suitable large-scale production, the short fine magnesium oxide-based foam pottery of enhancing of prepared aluminium oxide Porcelain filter is without any component for reducing its chemical stability, and the nanometer Aluminum sol being added is not only by light calcined magnesia Grain, nano-titanium dioxide and the short fibre of aluminium oxide are continuously bonded together by being formed, and can play the role of binder, Er Qiehe The nano-titanium dioxide powder of high degree of dispersion reacts generation with magnesium oxide powder particle in-situ together has magnesium and its alloy melt There is the Spinel of chemical stability to be welded together magnesium oxide particle, while there is the short fibre of the aluminium oxide of certain orientation Form is mutually inherited by being formed by magnesium aluminate spinel, therefore, ceramic foam filter have good intensity, chemical stability and Thermal shock resistance also can be used for aluminium and its alloy melt mistake especially suitable for the field trash in filtration, purification magnesium and its alloy melt Filter purification.Compared with the prior art scheme, technique effect of the invention：
One, the short fine magnesium oxide-based ceramic foam filter of enhancing of aluminium oxide of the invention has excellent chemical stability. The nano-titanium oxide added in the present invention program can promote the sintering of MgO, and react generation with higher chemical stabilization with MgO Magnesium ulvospinel (the Mg of property2TiO4, M2T) phase.Although containing the γ-Al reacted with Serum Magnesium in raw material Aluminum sol component2O3With The short fibre of aluminium oxide, but nanometer Aluminum sol can form γ-on light calcined magnesia particle, nano-titanium dioxide and the short fine surface of aluminium oxide Al2O3Coating film, the Al in sintering process2O3Light-burned MgO reactions with high activity generate the high-melting-point with face-centered cubic lattice MgAl2O4Phase (2135 DEG C of fusing point), MA and M2T dissolves each other completely at 1350 DEG C or more, according to XRD analysis the result shows that, institute of the present invention The ceramic foam filter of preparation only has periclase MgO and MA-M2T spinel solid solution phases.
In the MgO-Al of Serum Magnesium and addition aluminium oxide2O3It is sintered in the reaction system of ceramics, in addition to there are reaction equation (1), There is likely to be following reactions：
3Mg(l)+4Al2O3(s)=3MgAl2O4(s)+2Al(l) (5)
Aluminium oxide generates magnesium aluminate spinel MgAl with magnesia2O4Reaction be：
MgO(s)+Al2O3(s)=MgAl2O4(s) (6)
Serum Magnesium and magnesium aluminate spinel MgAl2O4The reaction of generation is：
3Mg(l)+MgAl2O4(s)=2Al(l)+4MgO(s) (7)
According to《Pure material thermochemical data handbook》(Yi Hesang baluns are edited, and Cheng Nailiang etc. is translated, Beijing：Scientific publication Society, 2003), the substance Gibbs free energys data of Serum Magnesium and magnesium aluminate spinel reaction system and instead in 900~1200K Answer (1), 5), the Gibbs Gibbs free Δs G of (6) and (7)1、ΔG5、ΔG6、ΔG7Result of calculation it is as shown in table 1.
Table 1 is in 900~1200K Serum Magnesiums and each gibbs free energy change Δ G reacted in magnesium aluminate spinel reaction system Result of calculation
Reaction equation Serum Magnesium generates the Gibbs free energy Δs G of (5) formula of magnesium aluminate spinel with aluminium oxide5In different temperatures It is lower minimum, illustrate that the reaction can preferentially occur under the common smelting temperature of magnesium alloy.Magnesium liquid is reacted with magnesium aluminate spinel Formula (7) is the decomposition product oxygen of magnesium liquid and magnesium aluminate spinel in the reacting quintessence although from can thermodynamically carry out Change and react between aluminium, but as shown in Table 1, under the smelting temperature of magnesium alloy, magnesium aluminate spinel is decomposed into aluminium oxide and magnesia Reaction is difficult to carry out (back reaction of reaction equation (6)), while remaining aluminium oxide also can preferentially be pressed with magnesium liquid in the ceramics being sintered Reaction equation (5) generates magnesium aluminate spinel；On the other hand, MgO-Al2O3The sides MgO are that periclase solid solution and MA points are brilliant in phasor Stone solid solution eutectic phasor, in situ reaction generate MA in the process almost without O2-Diffusion, only Mg2+And Al3+By fixed Oxygen lattice phase counterdiffusion, formation speed is by spreading slower Al3+It is determined, MA phases are mainly in Al2O3Side passes through Nei Yansheng Long mode generates, and leads to content of MgO in the MA outer layers for forming limit solid solution between MA phases and MgO, while being contacted with MgO particles Far above its average value, and MgO is not reacted with Serum Magnesium, therefore, is sintered magnesium oxide particle welding in ceramic structure one The magnesium aluminate spinel risen is mutually that can be stabilized in Serum Magnesium.
Any its chemical stability of reduction is free of in the short fine enhancing magnesia ceramic foam filter of aluminium oxide of the present invention Component, the nanometer Aluminum sol of addition not only passes through light calcined magnesia particle, nano-titanium dioxide and the short fibre of aluminium oxide to be formed Continuous film bonds together, and can play the role of binder, and with the nano-titanium dioxide powder of high degree of dispersion together with The reaction of magnesium oxide powder particle in-situ generates the Spinel for having chemical stability to magnesium and its alloy melt, avoids existing The damages of the binders to foamed ceramics chemical stability such as Ludox, silester are added in product；Meanwhile in ceramic composition also not Containing sodium salt (not using sodium carboxymethylcellulose in such as rheological agent), the larger Na of remaining ionic radius is avoided+Ceramics are burnt The obstruction of knot.
Because reaction equation (1), (5) spontaneous can carry out under the common smelting temperature of magnesium alloy, and aluminium and its alloy is molten It is identical with magnesium and its alloy melting temp to refine temperature, MgO and MA Spinels and aluminium and its alloy melt will not react formula (1), the back reaction of (5)；It is identical as magnesium and its alloy melt, it avoids and the binders pair such as Ludox, silester is added The damage of foamed ceramics chemical stability in aluminium and its alloy melt is (even if contain 1% SiO in material2, aluminium and its alloy Melt at high temperature also can be with SiO in ceramics2Al+SiO occurs2→Al2O3The reaction of+Si)；Therefore, prepared aluminium oxide is short Fibre enhancing magnesia ceramic foam filter can also be used for the melting and purifying of aluminium and its alloy.
Two, the short fine magnesium oxide-based ceramic foam filter of enhancing of aluminium oxide of the invention has good low-temperature sintering Energy.Light calcined magnesia fine powder employed in technical scheme of the present invention itself has very high sintering activity, in ceramic composition Middle addition nano-titanium dioxide, titanium ion diffuse into periclase grain boundary, form Ti4+Ion exchange Mg2+The solid solution of ion Body and promote intergranular to bind directly.Al2O3Lattice constant it is close with MgO, MgO lattices can be dissolved into sintering process and Cause MgO crystal that distortion of lattice occurs；Al3+Diffusion velocity it is small, Al2O3Solubility very little (Al in periclase MgO2O3 Only 3%), it is light-burned that nanometer Aluminum sol can be dissolved into high activity to solubility in periclase MgO at 1700 DEG C in sintering process Make MgO crystal that distortion of lattice occur in MgO lattices, activates lattice, while new change is generated by reaction-sintered between MgO particles Close object-magnesium aluminate spinel MgAl2O4Phase, to promote sintering and the alternate combination of particle.On the other hand, nano-powder has The features such as large specific surface area, surface energy be high, high activity, therefore, nano-powder is easy to be combined with other atoms, thus its fusing point with Sintering temperature is more much lower than micro mist.The sintering aid being added in the form of nano-titanium oxide and nanometer Aluminum sol, can fill original Expect the gap between micro powder granule, optimizes ceramic particle grading and mixing uniformity, meanwhile, surface of the nano-powder because of its own And interfacial effect, the nanometer γ-Al of high reaction activity in nano-titanium oxide and Aluminum sol2O3With coming into full contact with for light-burned MgO particles So that reaction speed is improved rapidly, reduce sintering temperature, improves the consistency and mechanical property of ceramics, and the reduction of sintering temperature Advantageously reduce the production cost of energy consumption and ceramic foam filter.Test result shows oxygen when sintering temperature is less than 1350 DEG C Sintering structure, which combines to be not enough, between change magnesium granules causes its low strength, and tissue combines good magnesia ceramic foam to filter The sintering temperature of device is 1350 DEG C~1550 DEG C.
Three, the short fine magnesium oxide-based ceramic foam filter of enhancing of aluminium oxide of the invention has good thermal shock resistance.Aluminium Solid-phase component is the porous gamma-Al of high activity in colloidal sol2O3, with magnesium aluminate spinel (MgAl2O4) crystal structure is identical.Using fibre Peacekeeping whisker can improve the mechanical property of ceramic matric composite as reinforcement.It is high in scheme provided by the present invention The light calcined magnesia particle of sintering activity and the short fibre of nano-titanium dioxide, the aluminium oxide of high degree of dispersion are by continuous nanometer Aluminum sol Film surrounds, and reaction in-situ generates magnesium aluminate spinel MA and magnesium ulvospinel M in sintering process2T-phase, MA and M2T 1350 DEG C with On dissolve each other completely, it is in sintering process that cristobalite MgO crystal grain is directly fused together, while cooling precipitation be precipitated two hypocone of intergranular Spar (intergranular spinelle) M2T and MA can compensate for the stress on each phase critical surface, the stress for making material be generated when being burnt into cooling Relaxation；When squeezing the polyurethane foam plastics masterplate of leaching hanging material by roll squeezer simultaneously, the aluminium oxide in made biscuit is short Fine to be arranged to a certain extent along rolling direction, the form of the short fibre of aluminium oxide with certain orientation is by being formed by magnalium point Spar is mutually inherited, and therefore, the Spinel of package periclase MgO crystal grain makes have the group combined closely between the ceramic crystalline grain of sintering It knits, and the pinning effect of Spinel inhibits the growth of magnesium oxide particle, to refine the tissue of foamed ceramics and carry Consistency between high ceramic crystalline grain, prepared aluminium oxide it is short it is fine enhance magnesium oxide-based ceramic foam filter have it is higher Mechanical property, high temperature impact resistance and thermal shock resistance.
In addition, polyurethane foam plastics template makes its surface roughening by NaOH etchings in preparation method of the present invention, then After the aqueous solution processing of dodecyl benzene sulfonate wetting agent, ceramic slurry, which is easy to uniformly apply, is suspended to polyurethane foam plank On；Simultaneously as rheological agent cellulose ether and polyvinyl butyral not still nano-titanium dioxide, aluminium oxide it is short fibre powder Fine dispersion agent, can prevent slurry from generating agglomeration, and bonding agent can be played the role of when preparing biscuit, impregnate Slurry, which can be comparatively firmly attached on polyurethane foam plank, afterwards makes biscuit have prodigious intensity, while in sintering process It easily escapes without polluting product, hereby it is ensured that the quality of ceramic foam filter.
Description of the drawings
Fig. 1 is the short fine preparation technology flow chart for enhancing magnesium oxide-based ceramic foam filter of aluminium oxide.
Specific implementation mode
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
The short fine magnesium oxide-based ceramic foam filter of enhancing of a kind of aluminium oxide, by salic short fine, nano-titanium dioxide Light calcined magnesia base ceramic slurry be coated in polyurethane foam carrier on, through drying, sintering obtain.Specific preparation process is such as Shown in Fig. 1.
Embodiment 1
According to nano-titanium oxide account for ceramic powder quality 1%, commercialization aluminium oxide it is short it is fine (about 10 μm~20 μm of diameter, Length is 50 μm~100 μm) 1% proportioning that accounts for ceramic powder quality, weigh the nano-titanium oxide, commercialization that grain size is 30nm The short fine and grain size of aluminium oxide is 250 mesh (central diameter d50Be 58 μm) light calcined magnesia powder prepare ceramic powder；According to polyethylene The mass ratio of butyral and hydroxypropyl methyl cellulose is 1:1 ratio mixed preparing rheological agent.
(commercialization of pH value weakly acidic pH is selected to receive the nanometer Aluminum sol 15% that solid content is 20% according to mass percent Rice Aluminum sol, similarly hereinafter), rheological agent 0.8%, remaining carries out dispensing for ceramic powder.First, in accordance with proportioning by light-magnesite powder Material is added in ball grinder, by nanometer Aluminum sol, nano-titanium dioxide, the short fine, rheological agent of aluminium oxide and suitable absolute ethyl alcohol (root Its addition is determined according to the solid content of ceramic slurry, similarly hereinafter) it is mixed and sonicated for 30min, make nano-titanium dioxide, aluminium oxide It is added in ball grinder after short fibre powder is fully dispersed, according still further to ratio of grinding media to material 2:Corundum ball is added in 1 ratio, with 60rpm rotating speeds Ball milling 4h makes its uniformly mixed ceramic slurry for obtaining solid content and being 60%.
10PPI polyurethane foam plastics masterplates are selected, surface etch 60min is impregnated in 40 DEG C of 15%NaOH aqueous solutions Naturally dry is washed with clear water afterwards, is then immersed in the aqueous solution of 2% dodecyl benzene sulfonic acid wetting agent, drying is taken out.So Polyurethane foam plastics masterplate is immersed in ceramic slurry afterwards, it is more to squeeze the removal of polyurethane foam plastics masterplate by roll squeezer Biscuit is made after remaining leaching hanging material, then so that biscuit is dried in 40 DEG C of draft chamber's removal alcohol solvents, alcohol solvent can pass through Retracting device recycles.
Dry biscuit is put into sintering furnace, being heated to 550 DEG C with the heating rate of 30 DEG C/h makes foam ceramic filter The organic matters decomposition gasification such as polyurethane foam and rheological agent in device biscuit is discharged, and is then heated with the heating rate of 200 DEG C/h To 1100 DEG C of temperature, 1550 DEG C of temperature are finally heated to the heating rate of 50 DEG C/h and keep the temperature 2.5h at such a temperature, with stove It is cooled to room temperature to obtain magnesium oxide-based ceramic foam filter.
Embodiment 2
The 2% of ceramic powder quality, the short fibre of aluminium oxide is accounted for according to nano-titanium oxide account for the 3% of ceramic powder quality match Than it is 500 mesh (central diameter d to weigh the short fine and grain size of the nano-titanium oxide that grain size is 60nm, commercialization aluminium oxide50Be 25 μm) it is light Burned magnesium oxide powder prepares ceramic powder；It is 1 according to the mass ratio of polyvinyl butyral and hydroxypropyl methyl cellulose:1 Ratio mixed preparing rheological agent.
The nanometer Aluminum sol 20% for being 25% by solid content according to mass percent, rheological agent 1.5%, remaining is ceramic powder Material carries out dispensing.Light calcined magnesia powder is added in ball grinder first, in accordance with proportioning, by nanometer Aluminum sol, nanometer titanium dioxide The short fine, rheological agent of titanium, aluminium oxide and suitable absolute ethyl alcohol are mixed and sonicated for 60min, keep the short fine powder of aluminium oxide abundant It is added in ball grinder after dispersion, according still further to ratio of grinding media to material 2:Corundum ball is added in 1 ratio, keeps it mixed with 120rpm rotating speed ball millings 2h It closes and uniformly obtains the ceramic slurry that solid content is 65%.
20PPI polyurethane foam plastics masterplates are selected, surface etch 40min is impregnated in 50 DEG C of 20%NaOH aqueous solutions Naturally dry is washed with clear water afterwards, is then immersed in the aqueous solution of 4% dodecyl benzene sulfonic acid wetting agent, drying is taken out.So Polyurethane foam plastics masterplate is immersed in ceramic slurry afterwards, it is more to squeeze the removal of polyurethane foam plastics masterplate by roll squeezer Biscuit is made after remaining leaching hanging material, then so that biscuit is dried in 50 DEG C of draft chamber's removal alcohol solvents.
Dry biscuit is put into sintering furnace, being heated to 550 DEG C with the heating rate of 30 DEG C/h makes foam ceramic filter The organic matters decomposition gasification such as polyurethane foam and rheological agent in device biscuit is discharged, and is then heated with the heating rate of 200 DEG C/h To 1100 DEG C of temperature, 1350 DEG C of temperature are finally heated to the heating rate of 50 DEG C/h and keep the temperature 3h at such a temperature, with furnace cooling But magnesium oxide-based ceramic foam filter is obtained to room temperature.
Embodiment 3
The 1.5% of ceramic powder quality, the short fibre of aluminium oxide is accounted for according to nano-titanium oxide account for the 2% of ceramic powder quality match Than it is 325 mesh (central diameter d to weigh the short fine and grain size of the nano-titanium oxide that grain size is 50nm, commercialization aluminium oxide50Be 45 μm) it is light Burned magnesium oxide powder prepares ceramic powder；It is 1 according to the mass ratio of polyvinyl butyral and hydroxyethyl cellulose:1 ratio Mixed preparing rheological agent.
The nanometer Aluminum sol 25% for being 22% by solid content according to mass percent, rheological agent 1.0%, remaining is ceramic powder Material carries out dispensing.Light calcined magnesia powder is added in ball grinder first, in accordance with proportioning, by nanometer Aluminum sol, nanometer titanium dioxide The short fine, rheological agent of titanium, aluminium oxide and suitable absolute ethyl alcohol are mixed and sonicated for 45min, keep the short fine powder of aluminium oxide abundant It is added in ball grinder after dispersion, according still further to ratio of grinding media to material 2:Corundum ball is added in 1 ratio, keeps it mixed with 90rpm rotating speed ball millings 3h It closes and uniformly obtains the ceramic slurry that solid content is 70%.
15PPI polyurethane foam plastics masterplates are selected, surface etch 50min is impregnated in 45 DEG C of 18%NaOH aqueous solutions Naturally dry is washed with clear water afterwards, is then immersed in the aqueous solution of 3% dodecyl benzene sulfonic acid wetting agent, drying is taken out.So Polyurethane foam plastics masterplate is immersed in ceramic slurry afterwards, it is more to squeeze the removal of polyurethane foam plastics masterplate by roll squeezer Biscuit is made after remaining leaching hanging material, then so that biscuit is dried in 45 DEG C of draft chamber's removal alcohol solvents.
Dry biscuit is put into sintering furnace, being heated to 550 DEG C with the heating rate of 30 DEG C/h makes foam ceramic filter The organic matters decomposition gasification such as polyurethane foam and rheological agent in device biscuit is discharged, and is then heated with the heating rate of 200 DEG C/h To 1100 DEG C of temperature, 1400 DEG C of temperature are finally heated to the heating rate of 50 DEG C/h and keep the temperature 2h at such a temperature, with furnace cooling But magnesium oxide-based ceramic foam filter is obtained to room temperature.
Embodiment 4
The 2% of ceramic powder quality, the short fibre of aluminium oxide is accounted for according to nano-titanium oxide account for the 2% of ceramic powder quality match Than it is 300 mesh (central diameter d to weigh the short fine and grain size of the nano-titanium oxide that grain size is 60nm, commercialization aluminium oxide50Be 48 μm) it is light Burned magnesium oxide powder prepares ceramic powder；According to polyvinyl butyral：Hydroxypropyl methyl cellulose：The matter of hydroxyethyl cellulose Amount is than being 5:2:3 ratio mixed preparing rheological agent.
The nanometer Aluminum sol 20% for being 20% by solid content according to mass percent, rheological agent 1.0%, remaining is ceramic powder Material carries out dispensing.Light calcined magnesia powder is added in ball grinder first, in accordance with proportioning, by nanometer Aluminum sol, nanometer titanium dioxide The short fine, rheological agent of titanium, aluminium oxide and suitable absolute ethyl alcohol are mixed and sonicated for 45min, keep the short fine powder of aluminium oxide abundant It is added in ball grinder after dispersion, according still further to ratio of grinding media to material 2:Corundum ball is added in 1 ratio, keeps it mixed with 100rpm rotating speed ball millings 3h It closes and uniformly obtains the ceramic slurry that solid content is 65%.
15PPI polyurethane foam plastics masterplates are selected, surface etch 50min is impregnated in 45 DEG C of 15%NaOH aqueous solutions Naturally dry is washed with clear water afterwards, is then immersed in the aqueous solution of 4% dodecyl benzene sulfonic acid wetting agent, drying is taken out.So Polyurethane foam plastics masterplate is immersed in ceramic slurry afterwards, it is more to squeeze the removal of polyurethane foam plastics masterplate by roll squeezer Biscuit is made after remaining leaching hanging material, then so that biscuit is dried in 45 DEG C of draft chamber's removal alcohol solvents.
Dry biscuit is put into sintering furnace, being heated to 550 DEG C with the heating rate of 30 DEG C/h makes foam ceramic filter The organic matters decomposition gasification such as polyurethane foam and rheological agent in device biscuit is discharged, and is then heated with the heating rate of 200 DEG C/h To 1100 DEG C of temperature, 1450 DEG C of temperature are finally heated to the heating rate of 50 DEG C/h and keep the temperature 2h at such a temperature, with furnace cooling But magnesium oxide-based ceramic foam filter is obtained to room temperature.
In above-described embodiment, experiment shows that prepared foamed ceramics has excellent thermal shock resistance and intensity, at 900 DEG C It is cooled down 50 times in air and is showed no cracking；The normal temperature strength of the ceramic foam filter of 75mm × 75mm × 25mm, 10PPI is not low In 3MPa.
Above-described embodiment is not limit the invention in any way, every to be obtained by the way of equivalent substitution or equivalent transformation Technical solution all fall in protection scope of the present invention.

Claims (9)

1. a kind of short fine magnesium oxide-based ceramic foam filter of enhancing of aluminium oxide, it is characterised in that：By salic short fine, nanometer The light calcined magnesia base ceramic slurry of titanium dioxide is coated on polyurethane foam carrier, is obtained through drying, sintering.
2. a kind of short fine preparation method for enhancing magnesium oxide-based ceramic foam filter of aluminium oxide, it is characterised in that including following step Suddenly：
(1) according to mass percent by 15%~25% nanometer of Aluminum sol, 0.8%~1.5% rheological agent, remaining is salic Short fine, nano-titanium dioxide magnesia ceramics powder carries out dispensing, is made after addition absolute ethyl alcohol ball milling mixing is uniform and contains admittedly The ceramic slurry that amount is 60%~70%；The rheological agent is the mixture of polyvinyl butyral and cellulose ether, wherein institute Polyvinyl butyral accounts for rheological agent quality 50% is stated, cellulose ether is industrial hydroxypropyl methyl cellulose, ethoxy fibre Or mixtures thereof one kind in dimension element；The ceramic powder is the mixed of light calcined magnesia, nano-titanium dioxide and the short fibre of aluminium oxide Close object；
(2) polyurethane foam plastics masterplate is immersed in ceramic slurry, polyurethane foam plastics masterplate is squeezed by roll squeezer Biscuit is made after removing extra leaching hanging material, then so that biscuit is dried in 40 DEG C~50 DEG C draft chamber's removal alcohol solvents；
(3) dry biscuit is put into sintering furnace, high temperature sintering is carried out at a temperature of being warming up to 1350 DEG C~1550 DEG C, with furnace cooling But magnesium oxide-based ceramic foam filter is obtained to room temperature.
3. a kind of short fine preparation method for enhancing magnesium oxide-based ceramic foam filter of aluminium oxide according to claim 2, It is characterized in that：The nanometer Aluminum sol solid content is 20%~25%, pH value >=4.
4. a kind of short fine preparation method for enhancing magnesium oxide-based ceramic foam filter of aluminium oxide according to claim 2, It is characterized in that：The nano-titanium oxide accounts for the 1%~2% of ceramic powder quality, and the short fibre of aluminium oxide accounts for ceramic powder matter The 1%~3% of amount.
5. a kind of short fine preparation method for enhancing magnesium oxide-based ceramic foam filter of aluminium oxide according to claim 2, It is characterized in that：The grain size of the light calcined magnesia powder is the mesh of 250 mesh~500.
6. a kind of short fine preparation method for enhancing magnesium oxide-based ceramic foam filter of aluminium oxide according to claim 2, It is characterized in that：The nano-titanium oxide grain size is 30~60nm, and short fine select of the aluminium oxide is commercialized small draw ratio polycrystalline Al2O3Staple fiber, a diameter of 10 μm~20 μm, length is 50 μm~100 μm.
7. a kind of short fine preparation method for enhancing magnesium oxide-based ceramic foam filter of aluminium oxide according to claim 2, It is characterized in that the preparation method of the ceramic slurry is：Light calcined magnesia powder is added in ball grinder according to proportioning, will be received The short fine, rheological agent of rice Aluminum sol, nano-titanium dioxide, aluminium oxide and absolute ethyl alcohol are mixed and sonicated for 30min~60min, Make to be added in ball grinder after the short fibre of aluminium oxide is fully dispersed, according still further to ratio of grinding media to material 2:Corundum ball is added in 1 ratio, with 60~ 120rpm rotating speed ball millings 2h~4h make its be uniformly mixed obtain.
8. a kind of short fine preparation method for enhancing magnesium oxide-based ceramic foam filter of aluminium oxide according to claim 2, It is characterized in that：The polyurethane foam plastics masterplate specification is 10PPI~20PPI；Using it is preceding 40 DEG C~50 DEG C 15% Naturally dry is washed with clear water after immersion surface etch 40min~60min in~20%NaOH aqueous solutions, is then immersed in 2% It is obtained after taking out drying after in the aqueous solution of~4% dodecyl benzene sulfonic acid wetting agent.
9. a kind of short fine preparation method for enhancing magnesium oxide-based ceramic foam filter of aluminium oxide according to claim 2, It is characterized in that in the step (3), the sintering process is：Being heated to 550 DEG C with the heating rate of 30 DEG C/h makes foam The organic matters decomposition gasification such as polyurethane foam and rheological agent in ceramic filter biscuit is discharged, then with the heating of 200 DEG C/h Speed is heated to 1100 DEG C of temperature, finally with the heating rate of 50 DEG C/h is heated to 1350 DEG C~1550 DEG C temperature and in the temperature 2~3h of lower heat preservation.
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CN1410393A (en) * 2002-11-21 2003-04-16 上海交通大学 Preparation method of special foamed ceramic filter for magnesium alloy
US20030146151A1 (en) * 2002-01-23 2003-08-07 Feng Chi Sintered magnesium oxide filter
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CN103553686A (en) * 2013-11-05 2014-02-05 中钢集团洛阳耐火材料研究院有限公司 Magnesium aluminate spinel foamed ceramic filter as well as preparation method thereof

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US20030146151A1 (en) * 2002-01-23 2003-08-07 Feng Chi Sintered magnesium oxide filter
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CN101259347A (en) * 2007-12-14 2008-09-10 济南圣泉集团股份有限公司 Zirconium oxide foamed ceramic filter
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