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Study On Morphology Evolution And Reaction Mechanism Of α-Al2O3 Synthesized From Industrial Precursors

Posted on:2019-09-03Degree:MasterType:Thesis
Country:ChinaCandidate:C H SunFull Text:PDF
GTID:2371330542494634Subject:Materials engineering
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α-Al2O3 is an important inorganic nonmetallic material,and the morphology ofα-Al2O3 micro-powder is closely related to the application field.With the introduction of milling treatment and additives,α-Al2O3 powders with different morphology were prepared by using three different industrial precursors as raw materials.The morphology evolution and mechanism of alumina with the introduction of AlF3additive during the calcination process were further studied.The study results are mainly as follows:(1)The phase transformation and morphology ofα-Al2O3 powders are closely related to milling treatment of the industrial Al(OH)3 precursor and the introduction of additives.Mil ing activation of the industrial Al(OH)3 precursor led to the acceleration ofα-transformation during calcination,and single-phaseα-Al2O3 was synthesized from a 3h milled precursor at 1150℃.In contrast,the precursor without mil ing was partially converted intoα-Al2O3 at 1150℃,co-existing with transitional phases such asκ-Al2O3,δ-Al2O3 andθ-Al2O3.By the introduction of precursor milling treatment,the neck growth ofα-Al2O3 nuclei formed from the milled precursor has been efficiently suppressed by the morphological changes of the Al(OH)3 precursor.As the gibbsite agglomerates in the size of 100μm were broken into irregularly shaped particles in a≤1μm size range by milling for 9 h,almost-sphericalα-Al2O3 powders of0.5μm in size were synthesized at 1450℃.Furthermore,thin or thick platelet-like,hexagonal,cake-likeα-Al2O3 powders were synthesized from milled precursors with the introduction of different additives,such as AlF3,NH4BF4,NH4F,NH4Cl and their compounds.(2)Mil ing treatment with different rotation modes has great influence on the morphology of Al(OH)3 precursors,phase transformation temperature and morphology ofα-Al2O3 powders synthesized by calcination.In comparison with precursor A(bi-directional rotation)obtained by 9 h milling treatment of industrial Al(OH)3,precursor B(unidirectional rotation)presented a honeycomb microstrucure;meanwhile,the specific surface area of the precursor B was much larger than that of the precursor A.Theα-Al2O3 powders formed by calcination of precursor B with 1 wt.%AlF3 additive at 910℃ was mainly a polyhedralα-Al2O3 with a grain size of about 100nm,and the morphology and grain size ofα-Al2O3 were basically unchanged as the calcination temperature increased into 940℃.During the calcination of precursor A with the addition of 1 wt.%AlF3,the obtained Al2O3 powders firstly inherited the precursor morphology at the temperature below 900℃,and then the shape of Al2O3 powders were obviously changed at the temperature above 900℃,resulting in an octahedral morphology with the exposure of the{101}crystal planes.At the same time,it was also found that the chemically combined water(O-H)in the lattice was reduced rapidly by infrared spectrum.With the increase of calcination time,the{100}crystal planes were exposed gradually,and the morphology ofα-Al2O3 eventually translated into plate-like shape as the calcination temperature increased into 1300℃.(3)The morphology and particle size of theα-Al2O3 powder prepared by the industrial alumina powder are significantly affected by the precursor pretreatment,introduction of additives,additive content and calcination schedule.Square shapedα-Al2O3 was synthesized at 1300℃ for 2 h by using 5 h milled commerciallyγ-Al2O3precursor with the introduction of 1 wt.%NH4F the mixture was calcined.As calcination time increased to 5 h,the edge contour of theα-Al2O3 grains was more rounded and ball-likeα-Al2O3 appeared.By introducing higher content of NH4F(20 wt.%),the morphology ofα-Al2O3 was changed from irregular to regular round cakes with the particle size of1μm when the calcination time prolonged from 2 h to5 h at 1300℃;while the morphology ofα-Al2O3 was changed from irregular block to regular square-like and round cake-like in 200500 nm size range during the same calcination process with the addition of 1 wt.%NH4F and 1 wt.%NH4Cl composite additives.As the calcination temperature increased into 1400℃ and maintained for2 h,the formedα-Al2O3 presented cake-like morphology in a size range of 12μm,accompanied by a small amount of 4μm.
Keywords/Search Tags:α-Al2O3 powders, industrial precursor, additives, morphology evolution
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