CN103524139A - Low-creep zircon overflowing brick and preparation method thereof - Google Patents

Low-creep zircon overflowing brick and preparation method thereof Download PDF

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CN103524139A
CN103524139A CN201310539068.2A CN201310539068A CN103524139A CN 103524139 A CN103524139 A CN 103524139A CN 201310539068 A CN201310539068 A CN 201310539068A CN 103524139 A CN103524139 A CN 103524139A
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zircon
preparation
overflow brick
staple fibre
zirconium white
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CN103524139B (en
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张启山
张瑛
李志军
刘杰
逄丽丽
李玉强
蒋绪贵
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Zibo Gongtao New Materials Group Co., Ltd.
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ZIBO INDUSTRIAL CERAMIC REFRACTORY MATERIAL Co Ltd
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Abstract

The invention relates to a low-creep zircon overflowing brick and a preparation method thereof. The low-creep zircon overflowing brick comprises, by mass, 100% of zircon powder, wherein zircon oxide short fibers account for, by mass, 0.0-4.0% of the zircon powder, silicon oxide powder accounts for, by mass, 0.1-2.0% of the zircon powder, and composite additives account for, by mass, 0.1-0.8% of the zircon powder. The composite additives can be La2O3, or CeO2, or combination of La2O3 and Y2O3, or combination of CeO2 and Y2O3, or combination of La2O3, CeO2 and Y2O3. According to the low-creep zircon overflowing brick and the preparation method thereof, strength of green bodies is improved, firing shrinkage of the green bodies is reduced, manufacturing yield of products is improved, bonding strength of crystal boundaries of zircon is enhanced, the high-temperature bend-creep rate of products is effectively lowered, and the service life of super-large-size overflowing bricks is prolonged.

Description

Low creep zircon stone overflow brick and preparation method thereof
Technical field
The present invention relates to a kind of low creep zircon stone overflow brick and preparation method thereof, belong to technical field of refractory materials.
Technical background
Along with manufacturing the development of the overflow downdraw production technology of liquid-crystalline glasses, external liquid-crystalline glasses generally formed with 8.5 generation crystal liquid substrate take the market orientation of product as the leading factor.Glass tube down-drawing is produced more than 8.5 generation liquid-crystalline glasses overflow brick length used reaches 3100mm, in use procedure, overflow brick is at 1000-1200 ℃, bear the weight of self and glass metal, and by melten glass, be delivered to the pulling force on overflow brick in drawn glass process, although conventional zircon material has lower creep speed, and glass manufacturer applies certain pressure from the supported on both sides position of brick and resists flexural deformation, but under these conditions or can bend creep.The height that is in particular in overflow brick middle portion is reduced to below support end height, the glass substrate of the even thickness that causes finally cannot being shaped.In order to solve the bending creep problem in overflow brick use procedure, prior art provides multiple solution.
Publication number is that the Chinese patent of CN1657499A discloses a kind of creep resistant zircon refractory material using in glass making system, has the composition that comprises following component, ZrSiO 4: 98.85-99.68wt%; ZrO 2: 0.01-0.15wt%; TiO 2: 0.23-0.50wt%; Fe 2o 3: this patent of 0.08-0.60wt%. is mainly the creep resistance that improves overflow brick by controlling titanium oxide and ferric oxide, wherein Fe 2o 3although to the shortcoming that promotes the densification of base substrate to have remarkable effect, also exist to cause glass coloring and foaming tendency to increase.
Chinese patent application 200980119562.5(CN102036934A) a kind of zircon particle of multimodal size distribution curve, TiO of at least 0.1% weight of adopting disclosed 2the Y of 10% weight at the most 2o 3mixing, isostatic pressing form green compact, at least at 1500 ℃, sintering obtains the method for fine and close zircon material, adopted multistage grain composition to improve the tap density of goods and reduced as far as possible porosity, to reduce grain boundary concentration, and having improved the bonding strength between zircon particle crystal boundary.But the granularity of considering zircon raw material is relevant to the smooth finish of final overflow brick goods, thereby increasing granularity and raising tap density, to improve the effect of the bending creep performance of overflow brick be finally limited.
Chinese patent application 200880114001.1(CN101842325A) disclose a kind of matrix material, added I, II, III class additive and their combination in zircon, its content is that I class additive accounts for 0.0-0.1 % by weight, is selected from Fe 2o 3, SnO 2, oxide glass and their mixture and combination; II class additive accounts for 0.1-0.8 % by weight, is selected from TiO 2, SiO 2, VO 2, CoO, NiO, NbO and their mixture and combination; III class additive accounts for 0.1-0.8 % by weight, is selected from Y 2o 3, ZrO 2, CaO, MgO, Cr 2o 3, Al 2o 3and their mixture and combination; Wherein the amount of agglutinant is in oxide compound, the per-cent of the gross weight based on composition.The mean particle size of described zircon particle is at least 1um, is at least 3um, 5um, 7um, 10um in some embodiments, and mean particle size is not higher than 15um.By adding II, III class sinter additives, the matrix material making at high temperature has low creep speed and good intensity.But CaO, MgO, Al 2o 3under high temperature, can cause the decomposition of zircon, cause the firing property of material to worsen.
Chinese patent application 200880123970.3(CN101910090A) disclose a kind of zircon that makes and contacted with sintering aid, wherein said sintering aid is liquid, solation or and their composition.Described sintering aid comprises at least one in titanium compound, iron containing compounds or its composition, carrys out the effect of intensified-sintered auxiliary agent by sintering aid being uniformly coated on to zircon powder surface.
Chinese patent application 200880009665.1(CN101641171B) the zircon composition with multimodal granularity is disclosed.Described multimodal zircon composition comprises the median particle that the median particle that is greater than 40% weight part is greater than the thick zircon component of 3 microns to 25 microns and is less than 60% weight part and is less than or equal to the thin zircon component of 3 microns.Described composition also comprises the oxide compound that yttrium phosphate and at least one comprise in titanium, iron, calcium, yttrium, niobium, neodymium at least one, or their combination.Described goods are less than 1 * 10 the creep speed of 1180 ℃ -4inch per hour, but need under helium-atmosphere or vacuum atmosphere, fire, large-sized base substrate is manufactured in industrialization certain difficulty.
Chinese patent application 200780043916.3(CN101558023A) disclose use zircon precursor, silica precursors, sol-gel forming agent and contacted with preformed zircon, fired the method for the fire-resistant body of densification, creep resistance.It is characterized in that adopting zircon precursor fill the hole between preformed zircon and reduce the crystal boundary in structure, thereby reduce the creep properties of zircon material.But the zirconium oxide precursor of various ways, as nitric hydrate zirconium, zirconium dichloride, hydration zirconium or its combination, with silica precursors, as silica gel, tetraethoxysilane, hydration silicon, silicon tetrachloride, amorphous silicon or their combination and sol-gel forming agent comprise in ammonia, ammonium hydroxide, Neutral ammonium fluoride the combination of at least one or they, the chemical reagent , refractory materials manufacturing process that relates to the strict protection of multiple scent of or needs in manufacturing processed need to add extra waste gas cleaning system.
The inventor applies for and the patent (application number 200710013446.8) of having the right discloses a kind of preparation method of large compact zircon overflow brick, the method that large-scale zircon overflow brick is slowly burnt till in rear isostatic pressing, heating and cooling that vacuumizes that adopts is disclosed, solved the problem that large-scale overflow brick very easily ftractures in process of production, wherein fully disclosed the process for making of overflow brick, but and the problem of not mentioned reduction overflow brick bending creep speed.
In actual manufacture and use procedure, increase along with base substrate length and weight, be necessary to take on the one hand other simple and easy to do methods, further reduce the hot bending creep speed of overflow brick material, also be necessary that on the other hand the intensity that improves green compact body is to reduce base substrate fracture or seminess in moulding, loading of kiln process, the contraction of base substrate while simultaneously reducing to burn till, burns till cracking and problem on deformation to solve.
Summary of the invention
The object of the present invention is to provide a kind of low creep zircon stone overflow brick and preparation method thereof, utilize the intensity of the raising green compact of zirconium white staple fibre; Add composite additive to improve the bonding strength between crystal boundary, promote zirconium white and silicon oxide formation zircon generation volumetric expansion in sintering process, reduce the contraction of burning till of base substrate; Effectively reduce the hot bending creep speed of zircon goods.
A kind of low creep zircon stone overflow brick of the present invention, the content of raw material is as follows:
Zircon opaque amount is 100%, and zirconium white staple fibre accounts for zircon opaque amount 0.0-4.0%, and silica powder accounts for zircon opaque amount 0.1-2.0%, and composite additive accounts for zircon opaque amount 0.1-0.8%; Wherein composite additive is La 2o 3or CeO 2or La 2o 3with Y 2o 3combination or CeO 2with Y 2o 3combination or La 2o 3with CeO 2with Y 2o 3combination.
During the compound interpolation of composite additive, preferred Y 2o 3add-on be La 2o 3or CeO 2the 1-2 of quality doubly.The present invention adds composite additive to have accelerating oxidation zirconium staple fibre partly or entirely to change into zircon, increase the consistency between raw material zircon and the new zircon particle forming, thus the effect of reduction hot bending creep speed.
When the present invention does not add zirconium white staple fibre: add separately Y 2o 3sample after burning till, high temperature break resistant intensity is lower, creep speed is higher; Add separately La 2o 3or CeO 2sample after burning till, high temperature break resistant intensity, creep speed are slightly improved.While adding zirconium white staple fibre, add separately La 2o 3or CeO 2burn till rear sample, high temperature break resistant intensity, creep speed have further improvement; Work as La 2o 3with Y 2o 3or CeO 2with Y 2o 3compound interpolation, and Y 2o 3add-on be La 2o 3or CeO 21-2 times time, volume density, the high temperature break resistant intensity of sample obviously improve, 1200 ℃ of bending creep speed obviously reduce, and have reached 1/10th of conventional zircon stone material, even one of 20.
Zircon powder, zirconium white staple fibre, silica powder and composite additive are all selected containing Al 2o 3, Fe 2o 3, CaO, MgO, K 2o, Na 2the raw material that O content is low.
The preferred Al of zircon powder 2o 3≤ 0.2%, Fe 2o 3≤ 0.05%, CaO+MgO≤0.05%, K 2o+Na 2o≤0.03%.Due to Al 2o 3, Fe 2o 3, CaO, MgO, K 2o, Na 2o is the final glassy phase that forms in the sintering process of brick, and in the time of 1200 ℃, glassy phase is softening can bring disadvantageous effect to creep speed.
The diameter of zirconium white staple fibre is 1-7um, and length is less than 3mm, wherein ZrO 2+ Y 2o 3quality>=99%; The diameter of preferential oxidation zirconium staple fibre is 1-5um, and length is less than 2mm; Most preferably the diameter of zirconium white staple fibre is 1-3um, and length is less than 1mm.
The preferred silicon powder of silica powder, silicon powder meso-position radius≤1um, SiO 2content>=99.5%, wherein contained Al 2o 3, Fe 2o 3, CaO, MgO, K 2o, Na 2total mass content≤0.3% of O, preferably total mass content≤0.1%.
La 2o 3preferred meso-position radius≤the 3um of powder, further preferably meso-position radius≤2um, most preferably meso-position radius≤1um, wherein La 2o 3quality>=99%, loss on ignition≤0.5%.
CeO 2preferred meso-position radius≤the 3um of powder, further preferably meso-position radius≤2um, most preferably meso-position radius≤1um, wherein CeO 2quality>=99%, loss on ignition≤0.5%.
Y 2o 3preferred meso-position radius≤the 3um of powder, further preferably meso-position radius≤2um, most preferably meso-position radius≤0.7um, wherein Y 2o 3quality>=99%, loss on ignition≤0.5%.
The zircon stone overflow brick of low creep of the present invention is less than 3.0 * 10 the bending creep speed of 1200 ℃ -7hour -1, bending creep speed is preferably less than 1.0 * 10 -7hour -1.Length is 3100-6000mm, and thickness is that 100-900mm, width are 1000-1700mm.
The preparation method of low creep zircon stone overflow brick of the present invention, after zircon powder wet grinding to meso-position radius is 5-10um, add again zirconium white staple fibre dispersion liquid, silica powder and composite additive, after common grinding, mist projection granulating, dress rubber cast, isostatic pressing make green compact, high temperature burns till to obtain base substrate, and base substrate precision work makes the zircon stone overflow brick of low creep.
The content of raw material is as follows:
Zircon opaque amount is 100%, and zirconium white staple fibre accounts for zircon opaque amount 0.0-4.0%, silica powder accounts for zircon opaque amount 0.1-2.0%, and composite additive accounts for zircon opaque amount 0.1-0.8%; Wherein composite additive is La 2o 3or CeO 2or La 2o 3with Y 2o 3combination or CeO 2with Y 2o 3combination or La 2o 3with CeO 2with Y 2o 3combination.
In green compact, the mass percentage content scope of impurity is Al 2o 3≤ 0.2%, Fe 2o 3≤ 0.05%, CaO+MgO≤0.05% and K 2o+Na 2o≤0.03%.
The preparation method of zirconium white staple fibre dispersion liquid is: in zirconium white staple fibre, add dispersion agent, then add silica powder or add the zircon powder of 1-4% jointly to grind to form zirconium white staple fibre dispersion liquid.
Dispersion agent is Sodium dodecylbenzene sulfonate.
Zirconium white staple fibre adds Sodium dodecylbenzene sulfonate, jointly grinds to form zirconium white staple fibre dispersion liquid use with silica powder or zircon powder raw material.
In order to disperse fully zirconium white staple fibre, make it in monofilament state, with the effect of playing increase blank strength after all the other raw material blendings, zirconium white staple fibre adds Sodium dodecylbenzene sulfonate dispersion agent, jointly grind with silica powder raw material or jointly grind with part zircon powder raw material, until evenly spread in water.Common object of grinding is accelerating oxidation silica flour and the mixing of zirconium white staple fibre, and is conducive to zirconium white staple fibre and changes into zircon, or increase the consistency between the zircon particle of raw material zircon and newly formation.The impurity of introducing in order to reduce dispersion agent, Sodium dodecylbenzene sulfonate can play dissemination, and Sodium dodecylbenzene sulfonate consumption is to be less than 0.1% of zirconium white staple fibre quality, preferably 0.06% or 0.04%.
In raw material, add the short agglutinant that accounts for zircon opaque amount 0.3-0.5%, wherein, short agglutinant is TiO 2powder.TiO 2powder, preferably meso-position radius≤5um, further preferably meso-position radius≤3um, most preferably meso-position radius≤1um, wherein TiO 2tiO in powder 2quality>=99%, loss on ignition≤0.5%.TiO 2powder promotes zircon blank Densification.
In common process of lapping, add ethanol or the Virahol that accounts for zircon opaque amount 2-5%.
Jointly be ground to zircon powder in zirconia ball: zirconium English powder: after the ratio that water is 2-3:2:1 adds and grinds in ball milling, then by zirconium white staple fibre dispersion liquid, be less than the TiO of 1um 2powder, composite additive add in ball mill in proportion, then add ethanol or the Virahol that accounts for zircon opaque amount 2-5%, grind and within 10-15 minute, obtain slip.The slip mist projection granulating mixing, pelletizing packs in mould, and isostatic pressing is large-sized green compact.
Wherein, controlling zircon powder footpath is 5-10um, presents normal particle diameter normal distribution curve.Do not add separately the zircon powder that particle diameter is less than 3um or is greater than 10um, size distribution curve only has a peak.The common Main Function grinding is the particle diameter of adjusting zircon particle, and composite additive is uniformly distributed between zircon particle.Adding ethanol or Virahol can reduce phosphoric acid and fully make particle dispersion≤1um.
Work as TiO 2, La 2o 3, CeO 2or Y 2o 3meso-position radius while being greater than 1um, adopt conventional wet grinding mode, use zirconia ball to be ground in advance meso-position radius to be less than 1um, spraying is dry or to adopt other modes to be fully dried to moisture content rear standby lower than 0.3%.
Dry seasoning or the use equipment of adopting is dried.Selecting, in the situation of seasoning, needs the time of several days, and preferably the natural drying condition of 1-3 days is advisable.
Sintering temperature is 1530-1600 ℃, and preferably sintering temperature is 1550 ± 20 ℃.The soaking time 30-100 hour burning till, 40-100 hour is preferably, more preferably 40-72 hour.
The heat-up rate burning till, at 1 ℃/h-10 ℃/h, is preferably 1 ℃/h-5 ℃/h.Because base substrate is huge, therefore in sintering process, should adopt the warming and cooling rate relaxing very much.Cooling adopts naturally cooling, or by certain cooling rate, is undertaken coolingly, preferably uses and is undertaken cooling by certain cooling rate.
Preferably firing temperature and heating-cooling speed are as follows:
Figure BDA0000407550370000051
After base substrate cool to room temperature, the rule of pressure transmission and heat transmits while burning till feature when waiting static pressure, bear the minimum and minimum position of temperature while burning till of pressure while suppressing in test brick body.From the physics center of gravity of brick, length, thickness, width are all the position of half, cut sample, the bending creep speed at the volume density of working sample, void content, cold crushing strength, 1200 ℃ of high temperature break resistant intensities and 1200 ℃.
Compared with prior art, the present invention has following beneficial effect:
The present invention has added zirconium white staple fibre and silica powder in zircon powder, has changed on the one hand the interpolation state of zircon stone initial feed, has improved the intensity of super zircon green compact, easily loading of kiln and movement; Volumetric expansion while simultaneously having promoted that in sintering process, zirconium white and silicon oxide change zircon into, has reduced the contraction of burning till of base substrate, has reduced cracking and the distortion tendency of base substrate, has improved the manufacture qualification rate of super overflow brick goods; Use on the other hand composite additive, impel zirconium fiber in sintering process, to form the zircon particle of needle-like or column, significantly reduced the bending creep speed of overflow brick, improved the work-ing life of super overflow brick and the quality of glasswork.Prepared zircon stone overflow brick has extremely low bending creep speed, for making super overflow brick.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
In the present invention, volume density and void content adopt the fine and close shaping refractory product volume density of GB/T2997-2000, apparent porosity and true porosity determination of test method; Cold crushing strength adopts GB/T5073-2008 refractory materials cold crushing strength determination of test method; High temperature break resistant intensity adopts GB/T3002-2004 refractory materials high temperature break resistant intensity determination of test method.Bending creep speed adopts JIS R1612-2010 fine ceramics bending creep test method to measure.JIS R1612-2010 adopts four-point bending device, and specimen size is 50mm * 4mm * 2mm, and length of support is 30mm ± 0.5mm, and loading dot spacing is 10mm ± 0.5mm, and probe temperature is 1200 ℃ of maintenances 100 hours, and the pressure applying is 2Mpa.
In the present invention, particle diameter is all measured with laser particle analyzer, and meso-position radius refers to corresponding particle diameter when the cumulative particle sizes percentile of sample reaches 50%.Its physical significance is that the particle that particle diameter is greater than it accounts for 50%, and the particle that is less than it also accounts for 50%, but does not relate to the length-to-diameter ratio of particle.
Embodiment 1
The preparation method of low creep zircon stone overflow brick:
In zircon powder, the mass percent of each component and component thereof is Al 2o 3be 0.12%, Fe 2o 3be 0.03%, CaO is 0.02%, MgO is 0.01%, K 2o is 0.01%, ZrO 2be 66.4%, SiO 2be 33.1%, its surplus is TiO 2and P 2o 5.
In silicon powder, the mass percent of each component and component thereof is Al 2o 3be 0.07%, Fe 2o 3be 0.01%, CaO is 0.01%, MgO is 0.00%, K 2o is 0.00%, and its surplus is SiO 2.
In the present embodiment, the content of each raw material is in Table 1.
The preparation process of zirconium white staple fibre dispersion liquid: be 6um by the diameter that accounts for zircon powder total mass 1%, length is less than 3mm, ZrO 2+ Y 2o 3>=99% zirconium white staple fibre is put into water, adds the Sodium dodecylbenzene sulfonate dispersion agent that accounts for zirconium white staple fibre quality 0.06%, then adds the zircon powder with zirconium white staple fibre equivalent weight, jointly grinds and after 60 minutes, makes zirconium white staple fibre dispersion liquid.Wherein, zirconium white staple fibre dispersion liquid in use stirs, settlement prevention.
The preparation process of low creep zircon stone overflow brick:
In zirconia ball: remaining zircon powder: the ratio that water is 2:2:1 adds in ball milling, grind and make the slip that zircon powder meso-position radius is 6um, add zirconium white staple fibre dispersion liquid, grind after 3 minutes, then by TiO 2powder, La 2o 3powder and silicon powder add in ball mill in proportion, then add ethanol, jointly grind after 10 minutes, and mist projection granulating obtains pelletizing.
Pelletizing packs in mould, and after vacuumizing, at the inferior static pressure of 180Mpa, making length is 5000mm, and thickness is the green compact that 500mm, width are 1300mm.At 1570 ℃, burn till, be incubated 60 hours.Physics center of gravity from brick after cooling cuts sample, and the bending creep speed at the volume density of working sample, void content, cold crushing strength, 1200 ℃ of high temperature break resistant intensities and 1200 ℃, detects data in Table the detected result of 3 embodiment.
Wherein, firing temperature and heating-cooling speed are as follows:
Figure BDA0000407550370000071
Embodiment 2-13
In embodiment 2-13, the preparation method of zircon stone overflow brick is all identical with embodiment 1, and the raw materials used mass ratio of embodiment 2-8, the parameter in preparation process are in Table 1; The raw materials used ratio of embodiment 9-13, the parameter in preparation process are in Table 2.Detection method is identical with embodiment 1, and embodiment 2-8 detects data in Table 3 detected result; Embodiment 9-13 detects data in Table 4 detected result.
In the zircon powder that wherein embodiment 9 is used, each component and constituent mass per-cent thereof are Al 2o 3be 0.35%, Fe 2o 3be 0.06%, CaO is 0.05%, K 2o is 0.02%, Na 2o is 0.02%, ZrO 2be 66.1%, SiO 2be 33.0%, the TiO of its surplus 2and P 2o 5.
Comparative example 1-2
In comparative example 1-2, the preparation method of zircon stone overflow brick is all identical with embodiment, and raw materials used mass ratio and the parameter in preparation process are in Table 2.Detection method is identical with embodiment 1, detects data in Table 4 detected result.
Embodiment 1 has added zirconium white staple fibre and La 2o 3, the bending creep speed of sample at 1200 ℃ is 30% of comparative example 1, embodiment 3 has added zirconium white staple fibre and CeO 2, the bending creep speed of sample at 1200 ℃ is 50% of comparative example 1, although embodiment 2 does not add zirconium white staple fibre, its bending creep speed is only also 50% of comparative example 1.
Embodiment 4-8 adds La 2o 3with Y 2o 3composite additive; Embodiment 9-12 has added CeO 2with Y 2o 3composite additive; Embodiment 13 adds La 2o 3, Y 2o 3and CeO 2three kinds of composite additives.Wherein adopt La 2o 3with Y 2o 3composite additive or CeO 2with Y 2o 3composite additive, Y 2o 3add-on be La 2o 3or CeO 2doubly, and the mass ratio of silica powder and zirconium white staple fibre is 0.50 o'clock to the 1-2 of quality, and embodiment 4 and 11 bending creep speed are only 1/20th of comparative example 1; Add La simultaneously 2o 3, Y 2o 3and CeO 2the embodiment 13 of three kinds of composite additives or add separately La 2o 3or CeO 21200 ℃ of bending creep speed of embodiment 1,2 be 3-5 * 10 -7hour -1, than the bending creep speed of comparative example 1, also have significantly and improve.The bending creep speed of embodiment 9 is also up to 7.86 * 10 -7hour -1, slightly high relevant with foreign matter content in base substrate.
Use in addition diameter for 3um, the sample bending creep speed that length is less than the zirconium white staple fibre of 1mm is slightly better than using diameter for 6um, and length is less than 3mm zirconium white staple fibre.
Above embodiment is only used to disclose implementation process of the present invention and beneficial effect, does not directly limit scope of the present invention.
The mass ratio of table 1 embodiment 1-8 Raw and the parameter in preparation process ()
Figure BDA0000407550370000081
The ratio of table 2 embodiment 9-13 and comparative example 1-2 Raw and the parameter in preparation process (two)
Figure BDA0000407550370000082
Table 3 embodiment 1 -8 detected result (one)
Figure BDA0000407550370000092
The detected result of table 4 embodiment 9-13 and comparative example 1-2 (two)
Figure BDA0000407550370000093

Claims (10)

1. a low creep zircon stone overflow brick, is characterized in that, the content of raw material is as follows:
Zircon opaque amount is 100%, and zirconium white staple fibre accounts for zircon opaque amount 0.0-4.0%, and silica powder accounts for zircon opaque amount 0.1-2.0%, and composite additive accounts for zircon opaque amount 0.1-0.8%; Wherein composite additive is La 2o 3or CeO 2or La 2o 3with Y 2o 3combination or CeO 2with Y 2o 3combination or La 2o 3with CeO 2with Y 2o 3combination.
2. low creep zircon stone overflow brick according to claim 1, is characterized in that, the diameter of zirconium white staple fibre is 1-7um, and length is less than 3mm, ZrO in zirconium white staple fibre 2+ Y 2o 3>=99%.
3. low creep zircon stone overflow brick according to claim 1, is characterized in that, the zircon stone overflow brick of described low creep is less than 3.0 * 10 1200 ℃ of crooked creep speed -7hour -1, length is 3100-6000mm, thickness is that 100-900mm, width are 1000-1700mm.
4. the preparation method of one kind low creep zircon stone overflow brick, it is characterized in that, after zircon powder wet grinding to meso-position radius is 5-10um, add again zirconium white staple fibre dispersion liquid, silica powder, composite additive, after common grinding, mist projection granulating, dress rubber cast, isostatic pressing make green compact, and high temperature burns till base substrate, and base substrate precision work makes the zircon stone overflow brick of low creep.
5. the preparation method of low creep zircon stone overflow brick according to claim 4, is characterized in that, the content of raw material is as follows:
Zircon opaque amount is 100%, and zirconium white staple fibre accounts for zircon opaque amount 0.0-4.0%, silica powder accounts for zircon opaque amount 0.1-2.0%, and composite additive accounts for zircon opaque amount 0.1-0.8%; Wherein composite additive is La 2o 3or CeO 2or La 2o 3with Y 2o 3combination or CeO 2with Y 2o 3combination or La 2o 3with CeO 2with Y 2o 3combination.
6. the preparation method of low creep zircon stone overflow brick according to claim 4, is characterized in that, in green compact, the mass percentage content scope of impurity is Al 2o 3≤ 0.2%, Fe 2o 3≤ 0.05%, CaO+M go≤0.05% and K 2o+Na 2o≤0.03%.
7. the preparation method of low creep zircon stone overflow brick according to claim 4, it is characterized in that, the preparation method of zirconium white staple fibre dispersion liquid is: in zirconium white staple fibre, add dispersion agent, then add silica powder or add the common wet grinding of zirconium English powder of 1-4% to become zirconium white staple fibre dispersion liquid.
8. the preparation method of low creep zircon stone overflow brick according to claim 7, is characterized in that, dispersion agent is Sodium dodecylbenzene sulfonate.
9. the preparation method of low creep zircon stone overflow brick according to claim 4, is characterized in that, adds the short agglutinant that accounts for zircon opaque amount 0.3-0.5% in raw material, and wherein, short agglutinant is TiO 2powder.
10. the preparation method of low creep zircon stone overflow brick according to claim 4, is characterized in that, firing temperature is 1530-1600 ℃, insulation 30-100 hour.
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Publication number Priority date Publication date Assignee Title
CN105060902A (en) * 2015-07-24 2015-11-18 淄博工陶耐火材料有限公司 Modified zircon sintered product and preparation method therefor
CN105218121A (en) * 2015-10-30 2016-01-06 淄博工陶耐火材料有限公司 Low creep, the Undec overflow brick of zircon and preparation method thereof
CN105272187A (en) * 2015-11-10 2016-01-27 浙江大学 Preparation method of zirconite ceramic
CN107117963A (en) * 2017-04-25 2017-09-01 山东君道高温材料有限公司 A kind of manufacturing process of large scale, large span aircon refractory
CN107935608A (en) * 2017-11-17 2018-04-20 淄博工陶耐火材料有限公司 The method that zircon brick is prepared using compact zircon aggregate
CN115650739A (en) * 2022-09-13 2023-01-31 上海利尔耐火材料有限公司 Long-life zirconia metering nozzle and preparation method thereof
CN116573935A (en) * 2023-05-23 2023-08-11 广东新岭南科技有限公司 Ceramic material and preparation method and application thereof

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Cited By (9)

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Publication number Priority date Publication date Assignee Title
CN105060902A (en) * 2015-07-24 2015-11-18 淄博工陶耐火材料有限公司 Modified zircon sintered product and preparation method therefor
CN105060902B (en) * 2015-07-24 2017-05-31 淄博工陶耐火材料有限公司 Modified zircon stone sintered article and preparation method thereof
CN105218121A (en) * 2015-10-30 2016-01-06 淄博工陶耐火材料有限公司 Low creep, the Undec overflow brick of zircon and preparation method thereof
CN105272187A (en) * 2015-11-10 2016-01-27 浙江大学 Preparation method of zirconite ceramic
CN107117963A (en) * 2017-04-25 2017-09-01 山东君道高温材料有限公司 A kind of manufacturing process of large scale, large span aircon refractory
CN107935608A (en) * 2017-11-17 2018-04-20 淄博工陶耐火材料有限公司 The method that zircon brick is prepared using compact zircon aggregate
CN107935608B (en) * 2017-11-17 2020-10-09 淄博工陶新材料集团有限公司 Method for preparing zircon brick by using compact zircon aggregate
CN115650739A (en) * 2022-09-13 2023-01-31 上海利尔耐火材料有限公司 Long-life zirconia metering nozzle and preparation method thereof
CN116573935A (en) * 2023-05-23 2023-08-11 广东新岭南科技有限公司 Ceramic material and preparation method and application thereof

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