CN107721406A - A kind of method for preparing high light transmittance light-weight magnesite-alumina spinel refractories - Google Patents

A kind of method for preparing high light transmittance light-weight magnesite-alumina spinel refractories Download PDF

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CN107721406A
CN107721406A CN201710947819.2A CN201710947819A CN107721406A CN 107721406 A CN107721406 A CN 107721406A CN 201710947819 A CN201710947819 A CN 201710947819A CN 107721406 A CN107721406 A CN 107721406A
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sintering aid
sintering
powder
mgo
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CN107721406B (en
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韩丹
章健
王士维
刘鹏
李桂
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Shanghai Institute of Ceramics of CAS
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Abstract

The present invention relates to a kind of method for preparing high light transmittance light-weight magnesite-alumina spinel refractories, the chemical formula of described light-weight magnesite-alumina spinel refractories is MgO ﹒ nAl2O3, 0.98 ＜ n ＜ 3, methods described includes：Using MgO powders, γ Al2O3Powder and sintering aid, light-weight magnesite-alumina spinel refractories are prepared by reaction sintering, the sintering aid is at least one of Y, La, Ca oxide, nitrate and metal alkoxide.

Description

A kind of method for preparing high light transmittance light-weight magnesite-alumina spinel refractories
Technical field
The present invention relates to a kind of method for preparing high light transmittance light-weight magnesite-alumina spinel refractories, belongs to ceramic material technology neck Domain.
Background technology
Light-weight magnesite-alumina spinel refractories have good optical property, high mechanical strength and stable physical chemistry Can, increasingly obtain the concern of people.The transparency range of magnesium aluminate spinel is 0.2-6.0 μm, covers and ultraviolet arrives middle infrared Domain, its density is low in addition, hardness is big, wear-resistant and physico-chemical attack, under the high temperature conditions under optical quality and mechanical strength Unobvious are dropped, can be widely applied to transparent armor, intelligent display device form, infrared optical window/target seeker rectification capouch The military, civilian field such as cover, ultraviolet photolithographic machine lens, high temperature window.
1961, GE found the transparency of magnesium-aluminum spinel ceramic first, using solid reaction process Synthetic MgAl spinal powder, with Li2O and SiO2For sintering aid, half is prepared first with vacuum-sintering or hydrogen atmosphere sintering Transparent magnesium-aluminum spinel ceramic, preparation and its cause of the multinational researcher in the subsequent world to light-weight magnesite-alumina spinel refractories Numerous studies have been carried out in terms of densification mechanism.
The sintering process of ceramic powders depends on the diffusivity of atom, for ionic crystals, the diffusion energy of material Power depends on the chemical potential gradient of zwitterion, point defect caused by point defect (intrinsic defect) caused by warm-up movement and doping (extrinsic defect).Chemical potential gradient and intrinsic defect are the inherent features of crystal, not malleable, therefore increase extrinsic defect Exactly improve the important channel of diffusion coefficient.Sintering aid can be generally added during ceramic post sintering and produces zwitterion room To improve sintering rate.Vacancy defect negligible amounts inside magnesium aluminate spinel, are unfavorable for the progress of densification process, easily produce Residual Pores.For preparation for high optical quality light-weight magnesite-alumina spinel refractories, control Residual Pores are most important, therefore It is generally necessary to adding sintering aid promotes densification process.Transmitance loss caused by order to eliminate the second phase is, it is necessary to tight simultaneously Lattice control the addition of sintering aid.
The mechanism of action of sintering aid is divided into two kinds：One kind is ionic radius and MgAl2O4It is more or less the same, ion occurs and replaces In generation, produce the point defects such as zwitterion room；Another kind is ionic radius and MgAl2O4Differ larger, ion substitution can not be passed through Room is produced, liquid phase can only be produced by generating eutectic compound come acceleration of sintering.Since the seventies, AUS experiment Room, naval laboratory, Colorado School of Mines, Deng Duojia research institutions of TA＆T companies are developing progressively ripe using LiF as sintering Auxiliary agent, the process route for preparing using vacuum hotpressing combination heat and other static pressuring processes light-weight magnesite-alumina spinel refractories, people are to LiF's Densification mechanism has carried out numerous studies.LiF fusing point is relatively low, can produce liquid phase, while F at low temperature-O can be substituted2-Shape Into cation vacancy, Diffusion Activation Energy is reduced, promotes the densification of ceramics, it is easy to accomplish the preparation of crystalline ceramics.But with LiF Generally to be combined for sintering aid with hot pressed sintering, be unfavorable for the mass production of product and the preparation of complicated shape sample, And LiF can cause abnormal grain growth and crystal boundary micro-crack, it is difficult to avoid the generation of transgranular stomata, reduce the mechanics of material And optical property.Krell etc. reports prepares light-weight magnesite-alumina spinel refractories by sintering aid of CaO.Due to selecting business magnesium Aluminate powder is raw material, and its CaO addition needs that enough liquid phase promotion densifications could be produced in more than 1000ppm Change.And after high temperature sintering, substantial amounts of CaO easily causes the precipitation of abnormal grain growth and calcium-aluminate, has a strong impact on The optical quality of ceramics.
The content of the invention
In view of the above-mentioned problems, it is an object of the invention to provide a kind of high printing opacity light-weight magnesite-alumina spinel refractories and its preparation Method.
The invention provides a kind of method for preparing high printing opacity light-weight magnesite-alumina spinel refractories, described magnesium aluminate spinel are saturating Bright ceramic chemical formula is MgO ﹒ nAl2O3, 0.98 ＜ n ＜ 3, methods described includes：
Using MgO powders, γ-Al2O3 powders and sintering aid, the transparent pottery of magnesium aluminate spinel is prepared by reaction sintering Porcelain, the sintering aid are at least one of Y, La, Ca oxide, nitrate and metal alkoxide.
The present invention is using wide material sources, price relatively low high-purity MgO and γ-Al2O3It is transparent that magnesium aluminate spinel is prepared for raw material In the process of ceramics, because diameter of particle is smaller, the residual of nanometer stomata is easily caused, causes sample in UV-visible region Transmitance it is relatively low.On the other hand, the present invention is by adding a small amount of sintering aid (such as Y2O3、La2O3With CaO and its corresponding nitric acid At least one of salt and metal alkoxide etc.), acceleration of sintering densification and stomata exclude.The mechanism of action of several sintering aids has Institute is different.Wherein two kinds of rare earth element ions of yttrium and lanthanum effectively facilitate burning by substituting aluminium ion to produce cation vacancy defect Material diffusion rate during knot.And calcium oxide easily generates the calcium aluminate compound of low melting point with aluminum oxide, give birth at high temperature Promote particle re-arrangement and mass transfer, and then acceleration of sintering process into liquid phase.Adding appropriate sintering aid can effectively eliminate Residual Pores, improve the transmitance in sample UV, visible light region, prepare high optical quality, have different magnaliums than magnalium point Spar crystalline ceramics.
It is preferred that MgO powder purity >=99.9%, particle diameter are 100~300nm, γ-Al2O3The purity of powder >= 99.9%th, particle diameter is 50~200nm, and purity >=99.8%, the particle diameter of sintering aid are 100~500nm.
It is preferred that with MgO powders and γ-Al2O3The gross mass of powder is calculated as 100%, and the quality of the sintering aid is dense Spend for 50~1000ppm, preferably 50~500ppm；
Preferably, when the sintering aid is yittrium oxide, mass concentration is 50~100ppm；
Preferably, when the sintering aid is lanthana, mass concentration is 50~100ppm；
Preferably, when the sintering aid is calcium oxide, mass concentration is 100~500ppm.
It is preferred that the reaction sintering includes：
(1) by MgO powders and γ-Al2O3Powder and sintering aid are well mixed, and obtain material powder；
(2) it is gained material powder is compressing, obtain biscuit；
(3) by gained biscuit first through biscuiting, without pressure pre-burning and HIP sintering after, obtain the transparent pottery of the magnesium aluminate spinel Porcelain.
Also, it is preferred that by MgO powders and γ-Al2O3After powder and sintering aid ball milling mixing, then through drying, sieve, forge After burning, material powder is obtained；
Preferably, the technique of the ball milling is in 250 revs/min of ball millings 6~12 hours；
Preferably, the drying is to be dried 24~48 hours at 50~80 DEG C；
Preferably, the sieving was 100 mesh sieves；
Preferably, the calcining is to be incubated 6 hours in air atmosphere, at 800 DEG C.
Also, it is preferred that the method for the shaping is dry-pressing formed or and cold isostatic compaction；The dry-pressing formed pressure It it is 1~3 minute for 10~20MPa, time, the pressure of the cold isostatic compaction is 150~250MPa, the time is 5~20 points Clock.
Also, it is preferred that the temperature of the biscuiting is 600~800 DEG C, the time is 6~10 hours.
Also, it is preferred that the temperature without pressure pre-burning is 1300~1600 DEG C, the time is 1~6 hour, and atmosphere is air Atmosphere or vacuum.
Also, it is preferred that the temperature of the HIP sintering is 1400~1900 DEG C, the time is 1~6 hour, and pressure is 120~200MPa, the atmosphere of preferably described HIP sintering is nitrogen or/and argon gas.
Also, it is preferred that by gained light-weight magnesite-alumina spinel refractories in air atmosphere at 1100~1300 DEG C of annealing Reason 6~30 hours.
On the other hand, present invention also offers a kind of light-weight magnesite-alumina spinel refractories prepared according to above-mentioned method.
Compared with prior art, preparation method provided by the invention produces vacancy defect by adding appropriate sintering aid Or liquid phase, sintering densification process can be effectively facilitated and stomata excludes, so as to improve ceramic ultraviolet~visibility region Transmitance.Sample (4mm is thick) after twin polishing can reach more than 85% in the transmitance of visible~region of ultra-red, connect The theoretical transmission of nearly magnesium aluminate spinel, can meet its application requirement in fields such as infrared window, the transparent armors.In addition, this The sintering temperatures such as calcined temperature and heat needed for the preparation method of invention ratio is relatively low, and the raw material sources of selection are extensive, cost is low, hold The accurate control and mass production of material component are easily realized, is especially suitable for preparing different MgO/Al2O3The magnesium aluminate spinel of ratio is saturating Bright ceramics.
Brief description of the drawings
Fig. 1 is that obtained add of the methods described of embodiment 1 has 100ppmY2O3Light-weight magnesite-alumina spinel refractories photo；
Fig. 2 is the saturating of the light-weight magnesite-alumina spinel refractories that thickness is 4mm after twin polishing made from the methods described of embodiment 1 is handled Cross rate curve map；
Fig. 3 is the saturating of the light-weight magnesite-alumina spinel refractories that thickness is 4mm after twin polishing made from the methods described of embodiment 2 is handled Cross rate curve comparison figure；
Fig. 4 is the obtained addition 100ppm Y of the methods described of embodiment 22O3The microstructure on surface after sample polishing, heat erosion Figure；
Fig. 5 is the saturating of the light-weight magnesite-alumina spinel refractories that thickness is 4mm after twin polishing made from the methods described of embodiment 3 is handled Cross rate curve comparison figure；
Fig. 6 is the obtained addition 100ppm La of the methods described of embodiment 32O3The microstructure on surface after sample polishing, heat erosion Figure；
Fig. 7 is the saturating of the light-weight magnesite-alumina spinel refractories that thickness is 4mm after twin polishing made from the methods described of embodiment 4 is handled Cross rate curve comparison figure；
Fig. 8 is the microstructure on surface after the obtained addition 500ppm CaO samples polishing of the methods described of embodiment 4, heat erosion Figure；Fig. 9 is the saturating of the light-weight magnesite-alumina spinel refractories that thickness is 4mm after twin polishing made from the methods described of embodiment 5 is handled Cross rate curve map.
Embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this Invention, is not intended to limit the present invention.
The present invention is to be commercialized high-purity MgO powder and γ-Al2O3Powder is raw material, by adding a small amount of sintering aid, is adopted The light-weight magnesite-alumina spinel refractories of high optical quality are prepared with reaction sintering.It is mainly by adding a small amount of sintering aid Promote densification process and stomata to exclude, improve the transmitance of ceramics.Wherein, sintering aid may include yittrium oxide (Y2O3), oxidation Lanthanum (La2O3), at least one of three kinds of calcium oxide (CaO), purity is higher than 99.8%.Sintering aid can be added individually, can also It is several to add simultaneously.Its incorporation way also includes but is not limited in addition to directly adding oxide；1) it is corresponding by adding Nitrate (lanthanum nitrate, calcium nitrate, yttrium nitrate etc.) pyrolytic obtains oxide；2) by adding corresponding metal alkoxide high temperature Decomposition obtains oxide.
In the present invention, used raw material is high-purity MgO and γ-Al2O3.Wherein, MgO powder purity >=99.9%, grain Footpath is 100~300nm.γ-Al2O3Purity >=99.9%, the particle diameter of powder are 50~200nm.The purity of sintering aid >= 99.8%th, particle diameter is 100~500nm.
Illustrate to following exemplary the preparation method of high light transmittance light-weight magnesite-alumina spinel refractories provided by the invention.This hair The technical process of bright methods described includes four steps such as powder preparation, shaping, densification, annealing.It is heretofore described (chemical formula is MgO ﹒ nAl to the suitable light-weight magnesite-alumina spinel refractories of method2O3, 0.98 ＜ n ＜ 3) preparation, be especially suitable for 3 ＞ n ＞ 1, i.e., the preparation of rich aluminium sample.
It is prepared by powder.By MgO powders and γ-Al2O3Powder and sintering aid are well mixed, and obtain material powder.It is specific next Say, by MgO powders and γ-Al2O3After powder and sintering aid ball milling mixing, then after drying, sieving, calcining, raw material powder is obtained Body.Described a certain amount of sintering aid refers to：With MgO powders and γ-Al2O3The gross mass of powder is calculated as 100%, described The mass concentration of sintering aid can be 50~1000ppm, preferably can be 50~500ppm.It should be noted that the sintering aid introduced can To be individually added into, several it can also add simultaneously, but the total amount introduced is total to be not to be exceeded 1000ppm.When the sintering helps When agent is yittrium oxide, mass concentration can be 50~100ppm.When the sintering aid is lanthana, mass concentration can be 50~ 100ppm.When the sintering aid is calcium oxide, mass concentration can be 100~500ppm.The technique of the ball milling is 250 Rev/min ball milling 6~12 hours.The drying is to be dried 24~48 hours at 50~80 DEG C.The sieving was 100 mesh Sieve.The calcining is to be incubated 6~12 hours in air atmosphere, at 600~800 DEG C.
The example prepared as a material powder, according to MgO:Al2O3Mol ratio be 1：N (0.98 ＜ n ＜ 3) is respectively Weigh MgO powders and γ-Al2O3Powder, a certain amount of sintering aid is then added, using absolute ethyl alcohol as decentralized medium, high pure oxygen It is that ball-milling medium carries out ball milling mixing to material powder to change aluminium ball, then dries, sieves, calcining removal of impurities.Described ball-milling technology For ball milling under conditions of 250rmp 12 hours, described drying condition was to be dried 24 hours at 60 DEG C, and described sieving technique is 100 mesh sieves are crossed, described calcining impurity removal process is incubated 6 hours for 800 DEG C in air atmosphere.
Shaping.Material powder is compressing, obtain biscuit.The method of the shaping can be it is dry-pressing formed or with it is cold etc. quiet Molded, preferably first dry-pressing combination cold isostatic compaction or powder directly carry out cold isostatic compaction.Its specific steps is such as Under：The material powder handled well is fitted into mould, pressurize 1~3 minute is dry-pressing formed under normal temperature, 10~20MPa pressure；Will Isostatic cool pressing processing is carried out after biscuit or powder jacket after dry-pressing, pressure is 150~250MPa, and the dwell time is 5~20 Minute.
Densification.By biscuit first through biscuiting, without pressure pre-burning and HIP sintering after, it is transparent to obtain the magnesium aluminate spinel Ceramics.Specifically, biscuit prior in Muffle furnace under the conditions of 600~800 DEG C biscuiting 6~10 hours remove powder handling and into The impurity introduced during type, then pre-burning (no pressure pre-burning) under the conditions of air atmosphere or vacuum are without pressure, finally by pre-burning sample Product, which are put into high temperature insostatic pressing (HIP) stove, carries out HIP sintering.The described temperature without pressure pre-burning can be 1300~1600 DEG C, insulation Time can be 3~10 hours.HIP sintering temperature can be 1400~1900 DEG C, and soaking time can be 1~6 hour, used Air pressure is 120~200MPa.The pressure medium (atmosphere) of the HIP sintering can be nitrogen or/and argon gas etc..
Annealing.The light-weight magnesite-alumina spinel refractories of preparation are incubated 6~30 in air atmosphere at 1100~1300 DEG C Hour, transmitance is lost caused by eliminating Lacking oxygen.
Embodiment is enumerated further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this Invention is further described, it is impossible to is interpreted as limiting the scope of the invention, those skilled in the art is according to this hair Some nonessential modifications and adaptations that bright the above is made belong to protection scope of the present invention.Following examples are specific Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by this paper explanation In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.If without specified otherwise, in following embodiments, MgO powder Body purity >=99.9%, particle diameter are 100~300nm, γ-Al2O3Purity >=99.9%, the particle diameter of powder are 50~200nm, Y2O3Purity >=99.8%, particle diameter 500nm, CaO purity >=99.8%, particle diameter 200nm, La2O3Purity >= 99.8%th, particle diameter 400nm.
Embodiment 1
(1) powder handling：According to MgO:Al2O3Mol ratio be 1:1.3 weigh MgO and γ-Al respectively2O3Powder, it is separately added into 0ppmY2O3, 100ppm (mass fraction) Y2O3, using absolute ethyl alcohol as decentralized medium, high purity aluminium oxide ball is ball-milling medium, Ball milling mixing 12 hours under conditions of 250rmp, the slurry after ball milling, which is placed in 60 DEG C of baking oven, to be dried 24 hours, then crosses 100 Sieve, finally by the powder after sieving be placed in Muffle furnace in 800 DEG C calcining 6 hours remove ball millings and sieving during introduce it is miscellaneous Matter；
(2) it is molded：Mixed powder after processing combines isostatic cool pressing (200MPa, pressurize using dry-pressing (10MPa, pressurize 1 minute) 3 minutes) method shaping, obtain magnesium-aluminum spinel ceramic biscuit；
(3) it is densified：Biscuit after shaping first in air atmosphere in 800 DEG C of biscuitings 6 hours, removes what is introduced in forming process Impurity, then in a vacuum furnace in 1400 DEG C of pre-burnings 6 hours, the sample after pre-burning carries out high temperature insostatic pressing (HIP) burning under 200MPa pressure Knot, sintering temperature are 1550 DEG C, and soaking time is 4 hours；
(4) anneal：Sample after sintering is placed in Muffle furnace and is incubated 6 hours in 1200 DEG C, obtains the transparent pottery of magnesium aluminate spinel Porcelain.
Fig. 1 is that the obtained addition through twin polishing processing of embodiment 1 has 100ppmY2O3Sample photo, as seen from Figure 1, Obtained light-weight magnesite-alumina spinel refractories material has good translucency in visible-range.Fig. 2 is made for embodiment 1 Sample and under identical sintering condition it is obtained not plus sintering aid sample transmitance comparison diagram, sample through twin polishing at Reason, thickness 4mm, adds appropriate Y as seen from Figure 22O3Transmitance of the sample in UV-visible region can be significantly improved, is added Enter to have 100ppmY2O3Transmitance of the light-weight magnesite-alumina spinel refractories at 400nm (do not add sample obtained by auxiliary agent for 82.6% 69%) transmitance at 400nm is.
Embodiment 2：
Preparation flow is similar to Example 1, and difference is MgO:Al2O3Mol ratio be 1.5, be separately added into 0ppm, 100ppm, 300ppm and 500ppmY2O3As sintering aid, biscuit pre-burning in Muffle furnace after shaping, calcined temperature is 1450 DEG C, soaking time is 3 hours；
Fig. 3 is the transmittance curve figure of sample made from embodiment 2, and sample is handled through twin polishing, thickness 4mm.Can by Fig. 3 See：The transmitance of sample is with Y2O3The increase of addition, which substantially reduces, (wherein, has been separately added into 0ppm, 100ppm, 300ppm And 500ppmY2O3Magnesium-aluminum spinel ceramic corresponding to the transmitance at 400nm be respectively 78%, 83%, 70%, 35%), optimal addition is 100ppm, and its transmitance illustrates a small amount of Y apparently higher than the sample for not adding sintering aid2O3Can To improve the optical quality of sample；
Fig. 4 is the obtained addition 100ppmY of embodiment 22O3Micro-structure diagram after sample surfaces polishing, heat erosion.Can by figure See, sample even grain size exist without obvious stomata and rare Zr addition, illustrate that the sintering aid of addition does not separate out, because This has higher optical quality.
Embodiment 3：
Preparation flow is similar to Example 2, and difference is to be separately added into 0ppm, 50ppm, 100ppm and 200ppm La2O3Make For sintering aid.Fig. 5 is the transmittance curve figure of sample made from embodiment 3, and sample is handled through twin polishing, thickness 4mm. As seen from the figure：The transmitance of sample is with La2O3The increase of addition substantially reduce (wherein, be separately added into 0ppm, 100ppm, 300ppm and 500ppm La2O3Magnesium-aluminum spinel ceramic corresponding to the transmitance at 400nm be respectively 78%, 79.5%th, 78.6%, 62.2%), optimal addition is 100ppm, and its transmitance is higher than the sample for being not added with sintering aid, Illustrate a small amount of La2O3It is favorably improved the transmitance of sample.Fig. 6 is the obtained addition 100ppm La of embodiment 32O3Sample table Micro-structure diagram after mirror polish, heat erosion.As seen from the figure, sample even grain size, without obvious stomata exist, grain boundaries without Second Phase Precipitation.
Embodiment 4：
Preparation flow is similar to Example 2, and difference is to be separately added into 0ppm, 100ppm, 500ppm and 1000ppm CaO works For sintering aid, and wherein hip treatment temperature is respectively 1600 DEG C, 1650 DEG C, 1550 DEG C, 1800 DEG C, and it is small to be incubated 3 When.Fig. 7 is the transmittance curve figure of sample made from embodiment 4, and sample is handled through twin polishing, thickness 4mm.Can by Fig. 7 See, the transmitance of the sample added with CaO be above being not added with sintering aid sample (wherein, be separately added into 0ppm, The transmitance at 400nm corresponding to 100ppm, 500ppm and 1000ppm CaO magnesium-aluminum spinel ceramic is respectively 78%th, 82%, 82.3%, 83.1%), when addition is 500ppm, can under relatively low hot equitemperature (1550 DEG C) it is complete Residual Pores and the second phase are eliminated, effectively improves the optical quality of sample, especially (CaO adds the transmitance of UV-visible region When dosage is less than 500ppm, such as 100ppm, caused liquid phase are less, it is therefore desirable to higher hot equitemperature, nanoporous It is not easy to discharge, ultraviolet region transmitance is relatively low；When CaO additions are higher than 500ppm, such as 1000ppm, calcium oxide and aluminum oxide The phase of calcium aluminate second of a large amount of non-cubic phases of generation, its fusing point is higher, under relatively low hot equitemperature easily aggregation formed it is bar-shaped Crystalline substance, the optical quality of sample is had a strong impact on, only hot equitemperature can just be such that calcium aluminate compound uniformly divides when being higher than its fusing point Magnesium aluminate spinel Medium Culture is dispersed in, eliminates its scattering process to incident light, therefore can greatly improve the sintering such as heat of sample Temperature).Fig. 8 is the micro-structure diagram after the obtained addition 500ppm CaO sample surfaces polishing of embodiment 4, heat erosion.By Fig. 8 It can be seen that sample even grain size, exists without obvious stomata and rare Zr addition.
Embodiment 5：
Preparation flow is similar to Example 2, and difference is to add 100ppm Y simultaneously2O3Helped with 500ppmCaO as sintering Agent.Fig. 9 is the transmittance curve figure of sample made from embodiment 5, and sample is handled through twin polishing, thickness 4mm.Can by Fig. 9 See, while add two kinds of sintering aids to significantly improve transmitance of the sample in UV-visible region, it is at 400nm Transmitance is 82.2% (the magnalium point crystalline substance for being added without sintering aid preparation that wherein, " no auxiliary agent " refers to preparing in embodiment 2 The transmittance curve of stone).

Claims (10)

  1. A kind of 1. method for preparing high printing opacity light-weight magnesite-alumina spinel refractories, it is characterised in that described magnesium aluminate spinel is transparent The chemical formula of ceramics is MgO ﹒ nAl2O3, 0.98 ＜ n ＜ 3, methods described includes：
    Using MgO powders, γ-Al2O3Powder and sintering aid, the transparent pottery of magnesium aluminate spinel is prepared by reaction sintering Porcelain, the sintering aid are at least one of Y, La, Ca oxide, nitrate and metal alkoxide.
  2. 2. according to the method for claim 1, it is characterised in that MgO powder purity >=99.9%, particle diameter are 100~300 Nm, γ-Al2O3The % of the purity of powder >=99.9, particle diameter are 50~200 nm, purity >=99.8%, the particle diameter 100 of sintering aid ~500 nm.
  3. 3. method according to claim 1 or 2, it is characterised in that with MgO powders and γ-Al2O3The gross mass meter of powder For 100%, the mass concentration of the sintering aid is 50~1000 ppm, preferably 50~500 ppm；
    Preferably, when the sintering aid is yittrium oxide, mass concentration is 50~100 ppm；
    Preferably, when the sintering aid is lanthana, mass concentration is 50~100 ppm；
    Preferably, when the sintering aid is calcium oxide, mass concentration is 100~500 ppm.
  4. 4. according to the method any one of claim 1-3, it is characterised in that the reaction sintering includes：
    （1）By MgO powders and γ-Al2O3Powder and sintering aid are well mixed, and obtain material powder；
    （2）Gained material powder is compressing, obtain biscuit；
    （3）By gained biscuit first through biscuiting, without pressure pre-burning and HIP sintering after, obtain the transparent pottery of the magnesium aluminate spinel Porcelain.
  5. 5. according to the method for claim 4, it is characterised in that by MgO powders and γ-Al2O3Powder and sintering aid ball milling After mixing, then after drying, sieving, calcining, obtain material powder；
    Preferably, the technique of the ball milling is in 250 revs/min of ball millings 6~12 hours；
    Preferably, the drying is to be dried 24~48 hours at 50~80 DEG C；
    Preferably, the sieving was 100 mesh sieves；
    Preferably, the calcining is to be incubated 6 hours in air atmosphere, at 800 DEG C.
  6. 6. the method according to claim 4 or 5, it is characterised in that the method for the shaping for it is dry-pressing formed or with it is cold etc. Hydrostatic profile, be preferably it is first dry-pressing formed after cold isostatic compaction again；The dry-pressing formed pressure is 10~20MPa, time For 1~3 minute, the pressure of the cold isostatic compaction was 150~250 MPa, the time is 5~20 minutes.
  7. 7. according to the method any one of claim 4-6, it is characterised in that the temperature of the biscuiting is 600~800 DEG C, the time is 6~10 hours.
  8. 8. according to the method any one of claim 4-7, it is characterised in that the temperature without pressure pre-burning for 1300~ 1600 DEG C, the time is 1~6 hour, and atmosphere is air atmosphere or vacuum.
  9. 9. according to the method any one of claim 4-8, it is characterised in that the temperature of the HIP sintering is 1400~1900 DEG C, the time is 1~6 hour, and pressure is 120~200 MPa, and the atmosphere of preferably described HIP sintering is Nitrogen or/and argon gas.
  10. 10. according to the method any one of claim 1-9, it is characterised in that by gained light-weight magnesite-alumina spinel refractories Made annealing treatment 6~30 hours in 1100~1300 DEG C in air atmosphere.
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CN111848184A (en) * 2020-07-30 2020-10-30 武汉理工大学 High-aluminum-content magnesia-alumina spinel transparent ceramic powder and preparation method thereof
CN113603475A (en) * 2021-07-27 2021-11-05 西南科技大学 Preparation method of trivalent chromium ion doped magnesium aluminate spinel transparent ceramic
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