CN108546093A - Short fine magnesium oxide-based crucible of enhancing of a kind of aluminium oxide and preparation method thereof - Google Patents

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

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CN108546093A
CN108546093A CN201810306499.7A CN201810306499A CN108546093A CN 108546093 A CN108546093 A CN 108546093A CN 201810306499 A CN201810306499 A CN 201810306499A CN 108546093 A CN108546093 A CN 108546093A
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crucible
oxide
temperature
aluminium oxide
magnesium oxide
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CN108546093B (en
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刘子利
刘希琴
叶兵
刘思雨
丁之光
丁文江
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FENGYANG L-S LIGHT ALLOY NET FORMING Co Ltd
Nanjing University of Aeronautics and Astronautics
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FENGYANG L-S LIGHT ALLOY NET FORMING Co Ltd
Nanjing University of Aeronautics and Astronautics
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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 crucible and preparation method thereof, this approach 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 the electrically molten magnesia ceramic powder containing nano lanthanum oxide, the short fibre of aluminium oxide, it adds that suitable deionized water is uniform through ball milling mixing, the ceramic slurry that solid content is 70%~80% then is made through being vacuum-evacuated；(2) crucible biscuit is prepared；(3) crucible blank is prepared；(4) magnesium oxide-based crucible blank in Aluminum sol is subjected to vacuum infiltration processing, then carries out surface grinding processing, carried out high temperature double sintering after drying at a temperature of 1400 DEG C~1600 DEG C, cool to room temperature with the furnace and obtain magnesium oxide-based crucible.

Description

Short fine magnesium oxide-based crucible 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 crucibles and preparation method thereof, the specifically short fine magnesium oxide-based earthenware of enhancing of aluminium oxide Crucible and preparation method thereof belongs to metal material and field of metallurgy.Magnesium oxide-based crucible prepared by the present invention is especially suitable for magnesium And its alloy melting.
Background technology
In recent years, light-weighted demand makes magnesium alloy and aluminium alloy application obtains quick development, either deformed Mg, Aluminium alloy still casts magnesium, the production of aluminium alloy all be unable to do without smelting-casting equipment.The chemical property of magnesium is active, easily with oxygen, nitrogen and Vapor chemically reacts, fusing and easy oxidization burning loss in refining process, and the product generated remains in magnesium and can dislike Change the internal soundness and performance of product, the aluminium alloy that when crucible furnace continuous smelting melts not with flame contact, alloying element oxidation Scaling loss is low, and therefore, crucible melting is the equipment that melting magnesium alloy generally uses although being limited by crucible capacity.It is right For aluminium alloy, in addition to large-scale manufacturing enterprise relatively mostly uses large size reverberatory furnace, crucible furnace is still middle-size and small-size foundry enterprise so far The capital equipment of founding aluminium alloy.
Crucible is the key that determine crucible melting quality, and the metal casting crucible industrially applied is mainly Iron reutilization (such as cast iron, stainless steel) and two kinds of nonmetallic crucible.Iron reutilization (carbon steel, stainless steel etc.) is that current magnesium, aluminum alloy melt casting are general All over the crucible used, but the aluminium alloy and liquid flux melted during heating easily corrodes crucible and reduces it and use the longevity Life, and iron is easily accessible in the aluminium alloy of melting and pollutes alloy.In nonmetallic crucible, graphite crucible intensity is low, operation Crucible is easily broken when improper or uneven heating is even, and is decreased obviously with thermal conductivity after long, and therefore, graphite crucible is at present very It is few to use.
The application of ceramic crucible is greatly promoted the development of the special smelting of metallurgical industry especially nuclear material.Magnesium alloy is molten Refining using ceramic crucible or it is ceramic-lined can avoid to the maximum extent in Normal Casting of Magnesium Alloy using Iron reutilization be mixed into Fe, The harmful elements such as Cu, Cr improve the corrosion resistance of magnesium alloy product.Although the smelting temperature of magnesium alloy is not high (with aluminium alloy phase Closely, 700 DEG C or so), but the chemical property of magnesium alloy is very active, and the standard generation free enthalpy of MgO is very low, in fusion process It easily aoxidizes, the loose magnesia of generation cannot provide melt the heat meeting accelerated oxidizing combustion protected and generated；It is another The vapour pressure of aspect, magnesium is quite high (being 1037Pa at 727 DEG C), and liquid magnesium alloy and steam easily penetrate into porous ceramic film material Internal simultaneously to react, the physical properties such as reaction product and the coefficient of thermal expansion of ceramic substrate, elasticity modulus are different, easy to produce Stress makes reaction product fall off from ceramic substrate, leads to the rotten of ceramics, short texture and damage and pollutes alloy melt, such as The very high Serum Magnesium of activity is very easy to and has obtained widely applied Al at present2O3, ZrO2, SiC, SiO2Ceramic matrix crucible Material occurs the reaction of (1)~(4) formula and damages simultaneously contamination on magnesium alloy melt rapidly, therefore, magnesium alloy smelting ceramic material It is required that harsher, existing Al2O3, ZrO2, SiC, SiO2Base ceramic crucible is not suitable for magnesium and magnesium alloy founding, about magnesium The relevant report of alloy melting ceramic material is less.
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 with magnesium and its alloy melt there is good stability at elevated temperature, temperature in use to be up to 1600- 1850 DEG C, the flux mixture formed with the villaumite and fluorate of melting does not react, and it is smaller with flux to be mingled with angle of wetting And the flux being easy in absorption Serum Magnesium is mingled with, therefore, MgO ceramic crucibles are the ideal choses of liquid magnesium alloy melting and purifying.This Outside, fine and close MgO ceramics are also considered as melting carbonyl iron and its alloy and nickel, uranium, thorium, zinc, tin, aluminium and its alloy are excellent The smelting vessel material of choosing.
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 CN103030407B (a kind of high intensity, the preparation method of high density, high-purity magnesium oxide crucible), Chinese patent literature CN1011306B (filter of purifying magnesium oxide foam pottery and its reparation technology) etc. prepares magnesia pottery by raw material of pure zirconia magnesium Porcelain, because MgO has very high fusing point and coefficient of thermal expansion (13.5 × 10-6/ DEG C) high, therefore, lead to difficult (the sintering temperature of its sintering Degree is not less than 0.8 times of its fusing point) and thermal shock resistance it is poor, limit the application and development of MgO ceramics.
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 ceramic sintering temperatures by adding sintering aid.Add V2O5When powder, MgO exists 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.In State patent document CN100434390C (composition and its method that make crucible), CN101785944B (are used for magnesium and Serum Magnesium The preparation method of filtering magnesia ceramic foam filter) in addition fluorite (1423 DEG C of fusing point) and magnesium fluoride (fusing point 1248 DEG C), the solid solution of fluoride not only increases the distortion of lattice of matrix magnesia in sintering process, and itself easily forms eutectic Point liquid phase, to reduce the sintering temperature of magnesia ceramics；However, the F in sintering process in fluoride and Si, Al, Fe, Ca In conjunction with most of (accounting for about 70% in ceramic tile production) volatilizees in a gaseous form not only itself corrodes green body and damage sintering ceramics Quality, fluoride pollution can be caused by being more seriously discharged into air, and fluoride can be through respiratory tract, alimentary canal and skin Into human body, Central nervous system, the toxic effect of cardiac muscle, low dose fluoride pollution can lead to tooth and the crisp calcification of bone,《Pottery Porcelain emission of industrial pollutants standard》(GB25464-2010) discharge standard of regulation fluoride has to be lower than 5.0mg/m in3, with Fluoride necessarily increases the discharge of vapor-phase fluoride as the low-temperature sintering auxiliary agent of magnesia ceramics and aggravates Environmental Inputs burden； In addition, fluorine ion is existed in the form of replacing oxonium ion in remaining solid solution fluoride in ceramics, intercrystalline is caused to combine Chemical stability reduces, it is difficult to which the long-time for resisting flux in Serum Magnesium corrodes.Chinese patent literature CN104496492B is (a kind of Compound magnesium carbon fire-clay crucible and preparation method thereof) etc. disclosed in ceramic foam filter prepare in slurry using the works such as Ludox For bonding agent, SiO between the ceramic particle of sintering2The presence of ingredient makes it easily be reacted by (4) formula with magnesium and its alloy melt, together Sample reduces the chemical stability of ceramics.Chinese patent literature CN100536986C (magnesium oxide foam ceramic filter), In the patent documents such as CN103553686A (a kind of magnesium aluminate spinel foamed ceramic filter and preparation method thereof), three oxidations two The low-temperature sintering auxiliary agent of boron and borax as magnesia ceramics, diboron trioxide form liquid phase when being higher than 450 DEG C, in sintering temperature When degree is more than 1350 DEG C, is reacted with magnesia and generate antifungin so that liquid form exists and reduces sintering temperature.However, three oxygen Change two boron easily with magnesium, reactive aluminum, it is in magnesium, aluminium alloy melt and unstable；Simultaneously as diboron trioxide is dissolved in water and ethyl alcohol Equal solvent, can consumingly absorb water generate boric acid in air, and the diboron trioxide added in ceramic preparation process is dissolved in Water forms boric acid aqueous solution, easily reacts to form boric acid magnesium precipitate and reduce its effect with magnesia.Gallium oxide is diboron trioxide Oxide of the same clan, at a lower temperature with magnesia formed spinel-type MgGa2O4And play the work for reducing sintering temperature With, but gallium stock number is seldom (gallium is strategic reserves metal), its answering in conventional ceramic of the higher price limit of gallium oxide With.
For ceramic crucible industry production method in addition to cannon pot is using dry pressing, casting and isostatic pressing are two kinds Common technology of preparing.Although the crucible of isostatic pressing is caused with crucible green body in density and high yield rate, sintering process not Yielding advantage, but find isostatic pressing machine molding crucible simultaneously there is of high cost, efficiency is low, thermal stability is poor, quickly plus The problems such as but crucible is easily cracking in the process and peels off for hot and cold, short life.Slip casting is crucible or other hollow systems The method the most rational of product, if other conditions are the same, slip casting can be obtained compared with other forming methods The packing density of particle green compact of bigger (compare 2000kg/cm3Product under briquetting pressure also wants fine and close), and the firing temperature needed It spends relatively low.
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 Magnesia crystal whisker fabricated in situ spinelle enhances the preparation method of magnesium oxide-based crucible.
In order to reach above-mentioned technical purpose, the technical scheme is that：
A kind of short fine magnesium oxide-based crucible of enhancing of aluminium oxide, it is characterised in that：It will be short fine containing nano lanthanum oxide, aluminium oxide Electrically molten magnesia base ceramic slurry casting in plaster mold is obtained through drying, sintering.
A kind of short fine preparation method for enhancing magnesium oxide-based crucible of aluminium oxide comprising following steps：
(1) according to mass percent by 15%~25% nanometer of Aluminum sol, 0.8%~1.5% rheological agent, remaining is containing receiving The electrically molten magnesia ceramic powder progress dispensing of rice lanthana, the short fibre of aluminium oxide, adds suitable deionized water through ball milling mixing Uniformly, the ceramic slurry that solid content is 70%~80% then is made through being vacuum-evacuated.
The nanometer Aluminum sol of addition forms γ-Al on the short fine surface of aluminium oxide that magnesium oxide particle and high uniformity disperse2O3 Coating film, the Al in sintering process2O3Magnesium aluminate spinel (MgAl is generated with MgO reaction in-situs2O4, MA) and phase, by cristobalite MgO Crystal grain is directly fused together.
The nanometer La that the nanometer Aluminum sol of addition can not only disperse in electrically molten magnesia particle and high uniformity2O3Powder and The short fine surface of aluminium oxide forms γ-Al2O3Coating film and play the role of binder, the Al in sintering process2O3With La2O3Together The MgAl that there is chemical stability to magnesium and its alloy melt is generated respectively with MgO reaction in-situs2O4And MgLa2O4Spinel (the electronegativity value ratio Mg and aluminium of La is small, MgLa2O4The chemical stability ratio MgAl of Spinel2O4Higher), therefore, the present invention Synthetic spinel in situ is mutually directly fused together by cristobalite MgO crystal grain in prepared crucible, which is woven in Serum Magnesium With good chemical stability, avoids existing product and the binders such as Ludox, silester are added to ceramic chemical stabilization The damage of property；Meanwhile sodium salt (not using sodium carboxymethylcellulose in such as rheological agent) is also free of in ceramic composition, avoid residual The larger Na of ionic radius+To the obstruction of ceramic post sintering.
The solid content of the nanometer Aluminum sol is 20%~25%.
The rheological agent is the mixture of polyvinyl alcohol and cellulose ether, wherein the polyvinyl alcohol accounts for rheological agent quality 40%, the cellulose ether is or mixtures thereof one kind in industrial hydroxyethyl cellulose and hydroxypropyl methyl cellulose；
The ceramic powder is nano lanthanum oxide, short fine and electrically molten magnesia the mixture of aluminium oxide；It is described nano oxidized Lanthanum accounts for the 1%~3% of ceramic powder quality, and the short fibre of aluminium oxide accounts for the 1%~3% of ceramic powder quality, remaining is electric smelting Magnesia.The grain size of the nano lanthanum oxide 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), the grain size of the electrically molten magnesia powder is Mesh (the central diameter d of 250 mesh~50050It it is 58 μm).
The nano lanthanum oxide of addition is reacted with fusion-cast MgO generates the MgLa with excellent high temperature stability2O4Spinel (2030 DEG C of fusing point).
Nanometer Aluminum sol and nano lanthanum oxide, which can be dissolved into sintering process in the lattice of MgO, makes MgO crystal occur Distortion of lattice activates lattice, while generating new compound Mg Al by reaction-sintered between MgO particles2O4And MgLa2O4Point Spar phase, to promote sintering and the alternate combination of particle.Nano-powder refers to particle size<The ultramicro powder of 100nm, Have the characteristics that large specific surface area, surface energy height, high activity, therefore, nano-powder is easy to be combined with other atoms, therefore it is molten Point and sintering temperature ratio micro mist are much lower.The sintering aid being added in the form of nanometer Aluminum sol and nano lanthanum oxide, can fill out Fill the gap between raw material micro powder granule, optimize ceramic particle grading and mixing uniformity, meanwhile, nano-powder because its own Surface and interface effect, the nanometer γ-Al of high reaction activity in Aluminum sol2O3Being come into full contact with MgO particles with nano lanthanum oxide makes Reaction speed improves rapidly, reduces sintering temperature, improves the consistency and mechanical property of ceramics, and the reduction of sintering temperature has Conducive to the production cost of reduction energy consumption and ceramic crucible.
Select electrically molten magnesia, hydration-resisting ability strong.Because magnesia and aluminium oxide reaction-sintered form MA meeting generating bodies Product expands (linear expansivity 2.3%, cubical expansivity 6.9%) and increases sintering burden.
The mechanical property of ceramic matric composite can be improved as reinforcement using fiber and whisker.It is carried in the present invention In the scheme of confession, nanometer Aluminum sol forms continuous film on the short fine surface of aluminium oxide of electrically molten magnesia particle and high degree of dispersion, Magnesium aluminate spinel MA phases are generated with MgO reaction in-situs in sintering process, MA is directly fused together by cristobalite MgO crystal grain. Almost without O in the forming process of MA2-The diffusion of ion, and only Mg2+And Al3+By fixed oxygen lattice phase counterdiffusion, Due to Al3+Diffusion velocity it is slow, in Al2O3The generated MA in side will make 4.75 times of the sides MgO, the oxygen with certain orientation The form for changing the short fibre of aluminium is more advantageous to and is formed by MA phases and inherits, and the pinning effect of MA phases inhibits magnesium oxide particle Fast growth, to refine the tissue of ceramics and improve ceramic consistency.
The preparation method of the ceramic slurry is：Electrically molten magnesia powder is added in ball grinder according to proportioning, by nanometer Nano lanthanum oxide, the short fibre of aluminium oxide is added after being prepared into solution in Aluminum sol, rheological agent and suitable deionized water, is ultrasonically treated 30min~60min make nano lanthanum oxide, aluminium oxide it is short it is fine it is fully dispersed in the solution after be added in ball grinder, according still further to ball Expect ratio 2:Corundum ball is added in 1 ratio, so that it is uniformly mixed with 60~120rpm rotating speed ball millings 2h~4h, then in 0.02MPa Vacuum exhaust 10min~15min is carried out under the negative pressure of~0.05MPa to obtain.
(2) ceramic slurry is poured into gypsum mold by slip casting, is demoulded, and divulged information at 80 DEG C~120 DEG C Indoor drying obtains crucible biscuit.Specifically, the preparation method of the crucible biscuit is：Ceramic slurry is injected into rapidly plaster mold In tool, it is placed on vibration moulding on vibrating forming machine, waits for that slurry is fully populated with mold, stops vibration when pulp surface bleeding is uniform, Equating bleeding surface, billet surface water is demoulded when escaping, and is dried to obtain crucible biscuit 80 DEG C~120 DEG C draft chambers.
(3) dry biscuit is put into sintering furnace, high temperature sintering is carried out at a temperature of being warming up to 1400 DEG C~1600 DEG C, with Stove is cooled to room temperature to obtain magnesium oxide-based crucible blank.The sintering process is：It is heated to 550 DEG C with the heating rate of 60 DEG C/h So that the organic matter decomposition gasification in biscuit is discharged, 1100 DEG C of temperature is heated to the heating rate of 200 DEG C/h, then with 50 DEG C/h Heating rate be heated to 1400 DEG C~1600 DEG C temperature, and keep the temperature 2~3h at such a temperature.
(4) magnesium oxide-based crucible blank in Aluminum sol is subjected to vacuum infiltration processing, then carries out surface grinding processing, High temperature double sintering is carried out after drying at a temperature of 1400 DEG C~1600 DEG C, room temperature is cooled to the furnace and obtains magnesium oxide-based crucible.
Magnesium oxide-based crucible blank vacuum infiltration processing method in Aluminum sol is：Magnesium oxide-based crucible blank is set In Aluminum sol, vacuum infiltration processing 30min is carried out under the negative pressure of 0.02MPa~0.05MPa, in 120 DEG C ± 10 DEG C of baking After being toasted 24 hours in case, it is repeated as stated above twice；Then on grinding machine surface is carried out by coolant liquid of Aluminum sol Polishing is handled, then is toasted 24 hours in 120 DEG C ± 10 DEG C of baking oven；Finally the drying crucible blank of surface grinding is carried out high Warm double sintering, the double sintering technique are：600 DEG C are heated to the heating rate of 60 DEG C/h, then with the liter of 300 DEG C/h Warm speed is heated to 1380 DEG C~1480 DEG C temperature and keeps the temperature 2~3h at such a temperature.
Low-temperature sintering stage lower heating rate can prevent rheological agent decomposition rate it is too fast cause biscuit collapse or Deformed damaged is more than after 1100 DEG C in high temperature sintering stage sintering temperature, 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 magnesium oxide-based crucible of the present invention uses injection forming preparation method, have simple process equipment, crucible uniform wall thickness, The advantages that at low cost, efficient, suitable large-scale production；Prepared magnesium oxide-based crucible is free of any its chemical stabilization of reduction Property component, the nanometer Aluminum sol being added, nano lanthanum oxide can not only play the role of reduce sintering temperature, and height Evenly spreading in magnesia ceramics powder granule and reacting to generate has chemical stability to magnesium and its alloy melt Magnesium oxide particle is mutually welded together by spinel solid solution, while having the form of the short fibre of the aluminium oxide of certain orientation by institute The magnesium aluminate spinel of formation is mutually inherited, and therefore, prepared magnesium oxide-based crucible has good intensity, chemical stability and resists Thermal shock resistance, the melting especially suitable for magnesium and aluminium alloy.Specially：
One, the short fine preparation method for enhancing magnesium oxide-based crucible of aluminium oxide of the invention has excellent chemical stability. The nano lanthanum oxide of addition is reacted with fusion-cast MgO generates the MgLa with excellent high temperature stability2O4Spinel (fusing point 2030 ℃).Although containing the γ-Al reacted with magnesium liquid in raw material Aluminum sol component2O3With the short fibre of aluminium oxide, but be added nano aluminum it is molten Glue forms γ-Al on the short fine surface of aluminium oxide that magnesium oxide particle and high uniformity disperse2O3Coating film, in sintering process Al2O3Magnesium aluminate spinel (MgAl is generated with MgO reaction in-situs2O4, MA) and phase, cristobalite MgO crystal grain is directly fused together.
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 reacted in magnesium aluminate spinel reaction system
Changes delta G result of calculations
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 stabilization of reduction is free of in the short fine preparation method for enhancing magnesium oxide-based crucible of aluminium oxide of the present invention Property component, the nanometer La that the nanometer Aluminum sol of addition can not only disperse in electrically molten magnesia particle and high uniformity2O3Powder and The short fine surface of aluminium oxide forms γ-Al2O3Coating film and play the role of binder, the Al in sintering process2O3With La2O3Together The MgAl that there is chemical stability to magnesium and its alloy melt is generated respectively with MgO reaction in-situs2O4And MgLa2O4Spinel (the electronegativity value ratio Mg and aluminium of La is small, MgLa2O4The chemical stability ratio MgAl of Spinel2O4Higher), therefore, the present invention Synthetic spinel in situ is mutually directly fused together by cristobalite MgO crystal grain in prepared crucible, which is woven in Serum Magnesium With good chemical stability, avoids existing product and the binders such as Ludox, silester are added to ceramic chemical stabilization The damage of property；Meanwhile sodium salt (not using sodium carboxymethylcellulose in such as rheological agent) is also free of in ceramic composition, avoid residual The larger Na of ionic radius+To the obstruction of ceramic post sintering.
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 ceramics chemical stability in aluminium and its alloy melt is (even if contain 1% SiO in material2, aluminium and its alloy melt It at high temperature also can be with SiO in ceramics2Al+SiO occurs2→Al2O3The reaction of+Si)；Therefore, the short fine increasing of prepared aluminium oxide Strong oxdiative magnesium ceramic crucible can also be used for the melting and purifying of aluminium and its alloy.Further it is proposed that be used to prepare crucible Slip casting slurry can also be used as aluminium alloy reflective smelting furnace lay bricks and inner wall smooth out slurry.
Two, the short fine preparation method for enhancing magnesium oxide-based crucible of aluminium oxide of the invention has good low-temperature sintering Energy.Nanometer Aluminum sol and nano lanthanum oxide, which can be dissolved into sintering process in the lattice of MgO, keeps MgO crystal generation lattice abnormal Become, activates lattice, while generating new compound Mg Al by reaction-sintered between MgO particles2O4And MgLa2O4Spinel, To promote sintering and the alternate combination of particle.Nano-powder refers to particle size<The ultramicro powder of 100nm, have than The features such as surface area is big, surface energy is high, high activity, therefore, nano-powder are easy to be combined with other atoms, therefore its fusing point and burning Junction temperature is more much lower than micro mist.The sintering aid being added in the form of nanometer Aluminum sol and nano lanthanum oxide, can fill raw material Gap between micro powder granule optimizes ceramic particle grading and mixing uniformity, meanwhile, nano-powder because of the surface of its own and Interfacial effect, the nanometer γ-Al of high reaction activity in Aluminum sol2O3Being come into full contact with MgO particles with nano lanthanum oxide makes to react speed Degree is rapid to be improved, and is reduced sintering temperature, is improved the consistency and mechanical property of ceramics, and the reduction of sintering temperature is conducive to drop The production cost of low energy consumption and ceramic crucible.Experiments have shown that tissue combines the short fine magnesium oxide-based crucible of enhancing of good aluminium oxide Preparation method sintering temperature be 1400 DEG C~1600 DEG C.
Three, the short fine preparation method for enhancing magnesium oxide-based crucible of aluminium oxide of the invention has good thermal shock resistance.Choosing With electrically molten magnesia, hydration-resisting ability is strong.Because volume expansion can occur for magnesia and aluminium oxide reaction-sintered formation MA, (line is swollen Swollen rate is 2.3%, cubical expansivity 6.9%) and increase sintering burden.γ-Al2O3Aluminium oxide is a kind of porous material, It is approximately that cube center of area is tightly packed, Al with oxonium ion3+It is irregularly distributed in the octahedron surrounded by oxonium ion and four sides Jie's stability transitional crystal structure among body gap is identical as magnesium aluminate spinel MA crystal structures.Using γ-Al2O3Replace α- Al2O3The sintering characteristic of MgO-MA materials will be changed, volume contraction 2.7% when forming MA, to improve the compactness of sintering. The mechanical property of ceramic matric composite can be improved as reinforcement using fiber and whisker.In scheme provided by the present invention In, nanometer Aluminum sol forms continuous film on the short fine surface of aluminium oxide of electrically molten magnesia particle and high degree of dispersion, sintered Magnesium aluminate spinel MA phases are generated with MgO reaction in-situs in journey, MA is directly fused together by cristobalite MgO crystal grain.In the shape of MA At in the process almost without O2-The diffusion of ion, and only Mg2+And Al3+By fixed oxygen lattice phase counterdiffusion, due to Al3+ Diffusion velocity it is slow, in Al2O3The generated MA in side will make 4.75 times of the sides MgO, the short fibre of aluminium oxide with certain orientation Form be more advantageous to and be formed by MA phases and inherit, and the pinning effect of MA phases inhibits the quick length of magnesium oxide particle Greatly, to refine the tissue of ceramics and improve ceramic consistency；With MgO and Al2O3It compares, mutually heat is swollen for magnesium aluminate spinel Swollen coefficient is small, thermal coefficient is low, and therefore, the short fine preparation method for enhancing magnesium oxide-based crucible of prepared aluminium oxide has higher Mechanical property, high temperature impact resistance and thermal shock resistance.
In addition, still aluminium oxide is not short fine and nano lanthanum oxide powder for cellulose ether and polyvinyl alcohol as rheological agent Fine dispersion agent can prevent slurry from generating agglomeration, and can also play the role of bonding agent when preparing biscuit, make element Base has higher intensity, while easily escaping in sintering process without polluting product, hereby it is ensured that the sintering matter of crucible Amount.
Description of the drawings
Fig. 1 is the short fine preparation process flow with the magnesium oxide-based crucible of alkali magnesium sulfate crystal whisker composite strengthening of zirconium dioxide Figure.
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 crucible of enhancing of aluminium oxide, will make pottery containing the electrically molten magnesia base of nano lanthanum oxide, the short fibre of aluminium oxide Porcelain slurry casting in plaster mold is obtained through drying, sintering.Specific preparation process is as shown in Figure 1.
Embodiment 1
It is 1% to account for ceramic powder mass percent according to nano lanthanum oxide, and the short fibre of aluminium oxide is 1%, remaining is electric smelting oxygen The proportioning for changing magnesium, nano lanthanum oxide, the small draw ratio polymorph A l of commercialization by grain size for 60nm2O3Staple fiber (a diameter of 10 μm~ 20 μm, length is 50 μm~100 μm) and grain size be 250 mesh (central diameter d50Be 58 μm) electrically molten magnesia powder mixed preparing pottery Ceramic powder；It is 2 according to the mass ratio of polyvinyl alcohol and hydroxyethyl cellulose:3 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 electrically molten magnesia powder Material is added in ball grinder, and nanometer Aluminum sol, rheological agent and suitable deionized water (are determined it according to the solid content of ceramic slurry Addition, similarly hereinafter) it is prepared into addition nano lanthanum oxide, the short fibre of aluminium oxide after solution, it is mixed and sonicated for 30min, makes nanometer Lanthana, aluminium oxide it is short it is fine it is fully dispersed in the solution after be added in ball grinder, according still further to ratio of grinding media to material 2:1 ratio is added rigid Beautiful ball makes it be uniformly mixed with 60rpm rotating speed ball millings 4h, and vacuum exhaust 15min is then carried out under the negative pressure of 0.02MPa and is obtained The ceramic slurry that solid content is 70%；
Ceramic slurry is injected in gypsum mold rapidly, vibration moulding on vibrating forming machine is placed on, waits for that slurry is fully populated with Mold stops vibration, equating bleeding surface when pulp surface bleeding is uniform.It is demoulded when the anhydrous effusion of billet surface, and 80 DEG C of draft chambers are dried to obtain crucible biscuit.
Dry biscuit is put into sintering furnace, 550 DEG C is heated to the heating rate of 60 DEG C/h, makes the rheology in biscuit The organic matters decomposition gasification such as agent is discharged, and 1100 DEG C of temperature is heated to the heating rate of 200 DEG C/h, then with the heating of 50 DEG C/h Speed is heated to 1600 DEG C of temperature, and keeps the temperature 2.5h at such a temperature, cools to room temperature with the furnace and obtains magnesium oxide-based crucible blank.
Magnesium oxide-based crucible blank is placed in Aluminum sol, vacuum infiltration processing is carried out under the negative pressure of 0.02MPa 30min is repeated twice as stated above after being toasted 24 hours in 120 DEG C ± 10 DEG C of baking oven；Then on grinding machine with Aluminum sol is that coolant liquid carries out surface grinding processing, then is toasted 24 hours in 120 DEG C ± 10 DEG C of baking oven；Finally surface is ground The drying crucible blank of light carries out high temperature double sintering, and double sintering technique is to be heated to 1100 with the heating rate of 200 DEG C/h DEG C, 1600 DEG C then are heated to the heating rate of 50 DEG C/h, and keep the temperature 2.5h at such a temperature, cool to room temperature with the furnace and obtain Magnesium oxide-based crucible blank.
Embodiment 2
It is 3% to account for ceramic powder mass percent according to nano lanthanum oxide, and the short fibre of aluminium oxide is 3%, remaining is electric smelting oxygen The proportioning for changing magnesium, nano lanthanum oxide, the small draw ratio polymorph A l of commercialization by grain size for 30nm2O3Staple fiber (a diameter of 10 μm~ 20 μm, length is 50 μm~100 μm) and grain size be 500 mesh (central diameter d50Be 25 μm) electrically molten magnesia powder mixed preparing pottery Ceramic powder；It is 2 according to the mass ratio of polyvinyl alcohol and hydroxypropyl cellulose:3 ratio mixed preparing rheological agent.
The nanometer Aluminum sol 25% for being 25% by solid content according to mass percent, rheological agent 1.5%, remaining is ceramic powder Material carries out dispensing.Electrically molten magnesia powder is added in ball grinder first, in accordance with proportioning, by nanometer Aluminum sol, rheological agent and appropriate Deionized water be prepared into after solution nano lanthanum oxide, the short fibre of aluminium oxide be added, be mixed and sonicated for 60min, make nano oxygen Change lanthanum, aluminium oxide it is short it is fine it is fully dispersed in the solution after be added in ball grinder, according still further to ratio of grinding media to material 2:Corundum is added in 1 ratio Ball makes it be uniformly mixed with 120rpm rotating speed ball millings 2h, and vacuum exhaust 10min is then carried out under the negative pressure of 0.05MPa and is obtained The ceramic slurry that solid content is 80%.
Ceramic slurry is injected in gypsum mold rapidly, vibration moulding on vibrating forming machine is placed on, waits for that slurry is fully populated with Mold stops vibration, equating bleeding surface when pulp surface bleeding is uniform.It is demoulded when the anhydrous effusion of billet surface, and 120 DEG C of draft chambers are dried to obtain crucible biscuit.
Dry biscuit is put into sintering furnace, 550 DEG C is heated to the heating rate of 60 DEG C/h, makes the rheology in biscuit The organic matters decomposition gasification such as agent is discharged, and 1100 DEG C of temperature is heated to the heating rate of 200 DEG C/h, then with the heating of 50 DEG C/h Speed is heated to 1450 DEG C of temperature, and keeps the temperature 2h at such a temperature, cools to room temperature with the furnace and obtains magnesium oxide-based crucible blank.
Magnesium oxide-based crucible blank is placed in Aluminum sol, vacuum infiltration processing is carried out under the negative pressure of 0.05MPa 30min is repeated twice as stated above after being toasted 24 hours in 120 DEG C ± 10 DEG C of baking oven；Then on grinding machine with Aluminum sol is that coolant liquid carries out surface grinding processing, then is toasted 24 hours in 120 DEG C ± 10 DEG C of baking oven；Finally surface is ground The drying crucible blank of light carries out high temperature double sintering, and double sintering technique is to be heated to 1100 with the heating rate of 200 DEG C/h DEG C, 1450 DEG C then are heated to the heating rate of 50 DEG C/h, and keep the temperature 2h at such a temperature, cool to room temperature with the furnace and obtain oxygen Change magnesium-based crucible blank.
Embodiment 3
It is 2% to account for ceramic powder mass percent according to nano lanthanum oxide, and the short fibre of aluminium oxide is 2%, remaining is electric smelting oxygen The proportioning for changing magnesium, nano lanthanum oxide, the small draw ratio polymorph A l of commercialization by grain size for 45nm2O3Staple fiber (a diameter of 10 μm~ 20 μm, length is 50 μm~100 μm) and grain size be 325 mesh (central diameter d50Be 45 μm) electrically molten magnesia powder mixed preparing pottery Ceramic powder；It is 2 according to the mass ratio of polyvinyl alcohol and hydroxyethyl cellulose:3 ratio mixed preparing rheological agent.
The nanometer Aluminum sol 20% for being 22% by solid content according to mass percent, rheological agent 1%, remaining is ceramic powder Carry out dispensing.Electrically molten magnesia powder is added in ball grinder first, in accordance with proportioning, by nanometer Aluminum sol, rheological agent and suitable Nano lanthanum oxide, the short fibre of aluminium oxide is added after being prepared into solution in deionized water, is mixed and sonicated for 45min, makes nano oxidized Lanthanum, aluminium oxide it is short it is fine it is fully dispersed in the solution after be added in ball grinder, according still further to ratio of grinding media to material 2:Corundum is added in 1 ratio Ball makes it be uniformly mixed with 100rpm rotating speed ball millings 3h, and vacuum exhaust 12min is then carried out under the negative pressure of 0.03MPa and is obtained The ceramic slurry that solid content is 75%.
Ceramic slurry is injected in gypsum mold rapidly, vibration moulding on vibrating forming machine is placed on, waits for that slurry is fully populated with Mold stops vibration, equating bleeding surface when pulp surface bleeding is uniform.It is demoulded when the anhydrous effusion of billet surface, and 100 DEG C of draft chambers are dried to obtain crucible biscuit.
Dry biscuit is put into sintering furnace, 550 DEG C is heated to the heating rate of 60 DEG C/h, makes the rheology in biscuit The organic matters decomposition gasification such as agent is discharged, and 1100 DEG C of temperature is heated to the heating rate of 200 DEG C/h, then with the heating of 50 DEG C/h Speed is heated to 1400 DEG C of temperature, and keeps the temperature 3h at such a temperature, cools to room temperature with the furnace and obtains magnesium oxide-based crucible blank.
Magnesium oxide-based crucible blank is placed in Aluminum sol, vacuum infiltration processing is carried out under the negative pressure of 0.03MPa 30min is repeated twice as stated above after being toasted 24 hours in 120 DEG C ± 10 DEG C of baking oven；Then on grinding machine with Aluminum sol is that coolant liquid carries out surface grinding processing, then is toasted 24 hours in 120 DEG C ± 10 DEG C of baking oven；Finally surface is ground The drying crucible blank of light carries out high temperature double sintering, and double sintering technique is to be heated to 1100 with the heating rate of 200 DEG C/h DEG C, 1400 DEG C then are heated to the heating rate of 50 DEG C/h, and keep the temperature 3h at such a temperature, cool to room temperature with the furnace and obtain oxygen Change magnesium-based crucible blank.
Embodiment 4
It is 1.5% to account for ceramic powder mass percent according to nano lanthanum oxide, and aluminium oxide is short by fine 2.5%, remaining is electric smelting The proportioning of magnesia, nano lanthanum oxide, the small draw ratio polymorph A l of commercialization by grain size for 30nm2O3(a diameter of 10 μm of staple fiber ~20 μm, length is 50 μm~100 μm) and grain size be 325 mesh (central diameter d50Be 45 μm) electrically molten magnesia powder mixed preparing Ceramic powder；According to polyvinyl alcohol：Hydroxypropyl methyl cellulose：The mass ratio of hydroxyethyl cellulose is 4:3:3 ratio mixing Prepare rheological agent.
The nanometer Aluminum sol 20% for being 20% by solid content according to mass percent, rheological agent 1.2%, remaining is ceramic powder Material carries out dispensing.Electrically molten magnesia powder is added in ball grinder first, in accordance with proportioning, by nanometer Aluminum sol, rheological agent and appropriate Deionized water be prepared into after solution nano lanthanum oxide, the short fibre of aluminium oxide be added, being ultrasonically treated 45min makes nano lanthanum oxide, oxygen Change aluminium it is short it is fine it is fully dispersed in the solution after be added in ball grinder, according still further to ratio of grinding media to material 2:Corundum ball is added in 1 ratio, with 80rpm rotating speed ball millings 3h makes it be uniformly mixed, and vacuum exhaust 12min is then carried out under the negative pressure of 0.04MPa and obtains solid content For 75% ceramic slurry.
Ceramic slurry is injected in gypsum mold rapidly, vibration moulding on vibrating forming machine is placed on, waits for that slurry is fully populated with Mold stops vibration, equating bleeding surface when pulp surface bleeding is uniform.It is demoulded when the anhydrous effusion of billet surface, and 100 DEG C of draft chambers are dried to obtain crucible biscuit.
Dry biscuit is put into sintering furnace, 550 DEG C is heated to the heating rate of 60 DEG C/h, makes the rheology in biscuit The organic matters decomposition gasification such as agent is discharged, and 1100 DEG C of temperature is heated to the heating rate of 200 DEG C/h, then with the heating of 50 DEG C/h Speed is heated to 1500 DEG C of temperature, and keeps the temperature 2.5h at such a temperature, cools to room temperature with the furnace and obtains magnesium oxide-based crucible blank.
Magnesium oxide-based crucible blank is placed in Aluminum sol, vacuum infiltration processing is carried out under the negative pressure of 0.03MPa 30min is repeated twice as stated above after being toasted 24 hours in 120 DEG C ± 10 DEG C of baking oven；Then on grinding machine with Aluminum sol is that coolant liquid carries out surface grinding processing, then is toasted 24 hours in 120 DEG C ± 10 DEG C of baking oven；Finally surface is ground The drying crucible blank of light carries out high temperature double sintering, and double sintering technique is to be heated to 1100 with the heating rate of 200 DEG C/h DEG C, 1500 DEG C then are heated to the heating rate of 50 DEG C/h, and keep the temperature 2.5h at such a temperature, cool to room temperature with the furnace and obtain Magnesium oxide-based crucible blank.
In above-described embodiment, prepared magnesium oxide-based crucible has excellent thermal shock resistance and intensity, in 1000 DEG C of skies It is cooled down 100 times in gas and is showed no cracking；The room temperature crushing strength of sintered crucible is not less than 150MPa.
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 crucible of enhancing of aluminium oxide, it is characterised in that：By the electricity containing nano lanthanum oxide, the short fibre of aluminium oxide Magnesium oxide-based ceramic slurry casting in plaster mold is melted, is obtained through drying, sintering.
2. a kind of short fine preparation method for enhancing magnesium oxide-based crucible of aluminium oxide, it is characterised in that include the following steps：
(1) according to mass percent by 15%~25% nanometer of Aluminum sol, 0.8%~1.5% rheological agent, remaining is containing nano oxygen Change the electrically molten magnesia ceramic powder progress dispensing of lanthanum, the short fibre of aluminium oxide, addition deionized water is uniform through ball milling mixing, then passes through It is vacuum-evacuated and the ceramic slurry that solid content is 70%~80% is made；The rheological agent is the mixing of polyvinyl alcohol and cellulose ether Object, wherein the polyvinyl alcohol accounts for the 40% of rheological agent quality, the cellulose ether is industrial hydroxyethyl cellulose and hydroxypropyl Or mixtures thereof one kind in ylmethyl cellulose；The ceramic powder is nano lanthanum oxide, the short fine and electric smelting oxidation of aluminium oxide The mixture of magnesium；
(2) ceramic slurry is poured into gypsum mold by slip casting, is demoulded, and in 80 DEG C~120 DEG C draft chambers Drying obtains crucible biscuit；
(3) dry biscuit is put into sintering furnace, high temperature sintering is carried out at a temperature of being warming up to 1400 DEG C~1600 DEG C, with furnace cooling But magnesium oxide-based crucible blank is obtained to room temperature；
(4) magnesium oxide-based crucible blank in Aluminum sol is subjected to vacuum infiltration processing, then carries out surface grinding processing, drying High temperature double sintering is carried out at a temperature of 1400 DEG C~1600 DEG C afterwards, room temperature is cooled to the furnace and obtains magnesium oxide-based crucible.
3. a kind of short fine preparation method for enhancing magnesium oxide-based crucible of aluminium oxide according to claim 2, it is characterised in that： The solid content of the nanometer Aluminum sol is 20%~25%.
4. a kind of short fine preparation method for enhancing magnesium oxide-based crucible of aluminium oxide according to claim 2, it is characterised in that： The nano lanthanum oxide accounts for the 1%~3% of ceramic powder quality, the short fibre of aluminium oxide account for ceramic powder quality 1%~ 3%, remaining is electrically molten magnesia.
5. a kind of short fine preparation method for enhancing magnesium oxide-based crucible of aluminium oxide according to claim 2, it is characterised in that： The grain size of the nano lanthanum oxide is 30~60nm, and short fine select of the aluminium oxide is commercialized small draw ratio polymorph A l2O3Short fibre Dimension, a diameter of 10 μm~20 μm, length is 50 μm~100 μm), the grain size of the electrically molten magnesia powder is 250 mesh~500 Mesh.
6. a kind of short fine preparation method for enhancing magnesium oxide-based crucible of aluminium oxide according to claim 4, it is characterised in that The preparation method of the ceramic slurry is：Electrically molten magnesia powder is added in ball grinder according to proportioning, by nanometer Aluminum sol, stream Become agent and deionized water is prepared into addition nano lanthanum oxide, the short fibre of aluminium oxide after solution, being ultrasonically treated 30min~60min makes to receive Rice lanthana, aluminium oxide it is short it is fine it is fully dispersed in the solution after be added in ball grinder, according still further to ratio of grinding media to material 2:1 ratio is added Corundum ball makes it be uniformly mixed, then under the negative pressure of 0.02MPa~0.05MPa with 60~120rpm rotating speed ball millings 2h~4h Vacuum exhaust 10min~15min is carried out to obtain.
7. a kind of short fine preparation method for enhancing magnesium oxide-based crucible of aluminium oxide according to claim 2, it is characterised in that The preparation method of the crucible biscuit is：Ceramic slurry is injected in gypsum mold rapidly, be placed on vibrating forming machine vibration at Type waits for that slurry is fully populated with mold, stops vibration, equating bleeding surface, the effusion of billet surface water when pulp surface bleeding is uniform Shi Jinhang is demoulded, and is dried to obtain crucible biscuit 80 DEG C~120 DEG C draft chambers.
8. a kind of short fine preparation method for enhancing magnesium oxide-based crucible of aluminium oxide according to claim 2, it is characterised in that： In the step (3), the sintering process is：It is heated to 550 DEG C of organic matters made in biscuit with the heating rate of 60 DEG C/h Decomposition gasification is discharged, and is heated to 1100 DEG C of temperature with the heating rate of 200 DEG C/h, is then heated to the heating rate of 50 DEG C/h 1400 DEG C~1600 DEG C temperature, and 2~3h is kept the temperature at such a temperature.
9. a kind of short fine preparation method for enhancing magnesium oxide-based crucible of aluminium oxide according to claim 2, it is characterised in that： Magnesium oxide-based crucible blank vacuum infiltration processing method in Aluminum sol is：Magnesium oxide-based crucible blank is placed in Aluminum sol In, vacuum infiltration processing 30min is carried out under the negative pressure of 0.02MPa~0.05MPa, is toasted in 120 DEG C ± 10 DEG C of baking oven After 24 hours, it is repeated as stated above twice；Then surface grinding processing is carried out by coolant liquid of Aluminum sol on grinding machine, It is toasted 24 hours in 120 DEG C ± 10 DEG C of baking oven again；The drying crucible blank of surface grinding is finally subjected to the secondary burning of high temperature Knot, the double sintering technique are：600 DEG C are heated to the heating rate of 60 DEG C/h, is then added with the heating rate of 300 DEG C/h Heat is to 1380 DEG C~1480 DEG C temperature and keeps the temperature 2~3h at such a temperature.
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