添加剂对氧化铝粉体微观结构影响研究
摘要
氧化铝具有多种微观形貌,其晶粒的结构特性直接决定了最终产品的应用性能,因此氧化铝粉体的微观结构控制引起了广泛关注。
本文采用异丙醇铝水解法结合水热处理工艺制备氧化铝粉体。在制备过程中分别引入氟化铝、冰乙酸和尿素作为添加剂,利用XRD、TG、TEM、SEM等检测方法系统地分析研究了添加剂含量、热处理温度、前驱体的选择、水热温度、水热处理时间、添加剂引入方式等制备条件对氧化铝的晶相转变及微观形貌的影响。
研究结果表明:AlF3可以显著的促进氧化铝的晶相转变过程,使其在900℃即可以完全的完成α相变而得到α-Al2O3,并且随着热处理温度的继续升高,氧化铝均保持α相不变。在一定水热条件下,随AlF3加入量增大,α-Al2O3的微观形貌是从不规则的板状多面体向规则的六角平板状发展;随水热温度升高,α-Al2O3微观形貌则由多面体结构向六角板状结构再到“蠕虫状”结构转变。
以冰乙酸作添加剂时,其对氧化铝的α相变温度影响不大。所制备得到的α-Al2O3晶粒间具有相互交联的趋势。随冰乙酸加入量的增加,参与拼合成为一体而加剧交联的晶粒数目增大,并且随水热处理温度的升高也具有与此相同的趋势。
引入尿素作为添加剂对α-Al2O3晶粒的粒径尺寸产生影响。粒径随尿素加入量的增加而增大,随水热温度的提高而减小。
在以上所得研究结果的基础上对各影响因素对氧化铝粉体微观结构的影响机理进行了详细的分析与讨论。
There are many kinds of microstructure for alumina. And the microstructure of powders will determine the applications of the ultimate productions directly. So particle shape control has aroused increasingly extensive attention.
In this dissertation powders of alumina were synthesized by the hydrolysis of aluminum isopropoxide and hydrothermal treatment. During the preparing process AlF3, acetic acid and carbamide were respectively introduced as additives. The effects of additive concentration, heat-treated temperature, kind of alumina precursor, hydrothermal temperature, hydrothermal time and way of additive introduced on the phase transformation and microstructure were investigated systemically by XRD, TG, TEM and SEM.
The results indicate that adding AlF3 can enhance the kinetic rate of the phase transformation for gamma to alpha alumina and reduce the transformation temperature of alpha phase to 900℃. And no significant change of phase has been found after increasing the calcination temperature up to 1200℃.α-Al2O3 passes through the morphology transformation of irregular platelet to flat hexangular platelet with increasing AlF3 concentration at the certain hydrothermal conditions; then the morphology ofα-Al2O3 passes through the transformation of polyhedron to hexangular platelet to vermiform morphology with increasing hydrothermal temperature.
It is shown that the effect of acetic acid as additive on transformation temperature of alpha phase is quite feeble. Theα-Al2O3 particles prepared are seriously hard aggregated. The quantity of particles joined into combination is amplified with increasing acetic acid concentration. And there is the same trend with increasing hydrothermal temperature.
Carbamide introduced as additive has the influence on the size ofα-Al2O3 particles. The sizes of particles are amplified with increasing carbamide concentration and reducing hydrothermal temperature.
And the mechanism of influence for varied factors on the microstructure of alumina powders was analyzed and discussed in detail on the base of experimental results.
本文采用异丙醇铝水解法结合水热处理工艺制备氧化铝粉体。在制备过程中分别引入氟化铝、冰乙酸和尿素作为添加剂,利用XRD、TG、TEM、SEM等检测方法系统地分析研究了添加剂含量、热处理温度、前驱体的选择、水热温度、水热处理时间、添加剂引入方式等制备条件对氧化铝的晶相转变及微观形貌的影响。
研究结果表明:AlF3可以显著的促进氧化铝的晶相转变过程,使其在900℃即可以完全的完成α相变而得到α-Al2O3,并且随着热处理温度的继续升高,氧化铝均保持α相不变。在一定水热条件下,随AlF3加入量增大,α-Al2O3的微观形貌是从不规则的板状多面体向规则的六角平板状发展;随水热温度升高,α-Al2O3微观形貌则由多面体结构向六角板状结构再到“蠕虫状”结构转变。
以冰乙酸作添加剂时,其对氧化铝的α相变温度影响不大。所制备得到的α-Al2O3晶粒间具有相互交联的趋势。随冰乙酸加入量的增加,参与拼合成为一体而加剧交联的晶粒数目增大,并且随水热处理温度的升高也具有与此相同的趋势。
引入尿素作为添加剂对α-Al2O3晶粒的粒径尺寸产生影响。粒径随尿素加入量的增加而增大,随水热温度的提高而减小。
在以上所得研究结果的基础上对各影响因素对氧化铝粉体微观结构的影响机理进行了详细的分析与讨论。
There are many kinds of microstructure for alumina. And the microstructure of powders will determine the applications of the ultimate productions directly. So particle shape control has aroused increasingly extensive attention.
In this dissertation powders of alumina were synthesized by the hydrolysis of aluminum isopropoxide and hydrothermal treatment. During the preparing process AlF3, acetic acid and carbamide were respectively introduced as additives. The effects of additive concentration, heat-treated temperature, kind of alumina precursor, hydrothermal temperature, hydrothermal time and way of additive introduced on the phase transformation and microstructure were investigated systemically by XRD, TG, TEM and SEM.
The results indicate that adding AlF3 can enhance the kinetic rate of the phase transformation for gamma to alpha alumina and reduce the transformation temperature of alpha phase to 900℃. And no significant change of phase has been found after increasing the calcination temperature up to 1200℃.α-Al2O3 passes through the morphology transformation of irregular platelet to flat hexangular platelet with increasing AlF3 concentration at the certain hydrothermal conditions; then the morphology ofα-Al2O3 passes through the transformation of polyhedron to hexangular platelet to vermiform morphology with increasing hydrothermal temperature.
It is shown that the effect of acetic acid as additive on transformation temperature of alpha phase is quite feeble. Theα-Al2O3 particles prepared are seriously hard aggregated. The quantity of particles joined into combination is amplified with increasing acetic acid concentration. And there is the same trend with increasing hydrothermal temperature.
Carbamide introduced as additive has the influence on the size ofα-Al2O3 particles. The sizes of particles are amplified with increasing carbamide concentration and reducing hydrothermal temperature.
And the mechanism of influence for varied factors on the microstructure of alumina powders was analyzed and discussed in detail on the base of experimental results.
引文
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[4] Jiang Li, Yusong Wu, Yubai Pan, et al. Influence of fluorides on phase transition ofα-Al2O3 formation [J]. Ceramics International, 2006, xxx-xxx
[5] Pierre Alphonse, Matthieu Courty. Structure and thermal behavior of nanocrystalline boehmite [J]. Thermochimica Acta, 2005, 425:75-89
[6] H.L.Wen, Y.Y.Chen, F.S.Yen, et al. Size characterization ofθ-andα-Al2O3 crystallites during phase transformation [J]. Nanostructured Materials, 1999, 11(1):89
[7]杨重愚.氧化铝生产工艺学[M].第1版.北京:冶金工业出版社,1993
[8]陈玮,尹周澜,李晋峰.影响γ-Al2O3→α-Al2O3物相转变过程的因素研究[J].轻金属,2006,(3): 12-15
[9] James H.Adair, Ender Suvaci. Morphological control of particles [J]. Current Opinion in Colloid & Interface Science, 2000, 5:160-167
[10]秦麟卿,吴伯麟.α-Al2O3颗粒形貌对其坯体烧结性能的影响[J].武汉理工大学学报,2006, 28(2):7-9
[11] George V.Franks, Fred F.Lange. Mechanical behavior of saturated, consolidated, alumina powder compacts:effect of particle size and morphology on the plastic-to-brittle transition [J].Colloids and Surfaces A:Physicochemical and Engineering Aspects, 1999, 146:5-17
[12]张克从,张乐惠.晶体生长科学与技术[M].北京:科学出版社,1996
[13]李继光,孙旭东,茹红强等.湿化学法合成单分散陶瓷超微粉体的基本原理[J].功能材料,1997, 28(4):333
[14]邓三毛,叶红齐,苏周等.片状氧化物粉体的合成与性能[J].化工新型材料,2004,32(7):13-15
[15]董岩,蒋建清,刘刚等.作为荧光粉原料的氧化铝的制备及其形貌控制[J].硅酸盐学报,2004, 32(4):393-397
[16]董岩,蒋建清,梁超等.小粒径氧化铝粉的制备及其在荧光粉合成中的应用[J].中国陶瓷,2005, 41(3):12-15
[17]周振君,杨正方,袁启明等.溶胶-凝胶法合成小尺寸板状氧化铝[J].硅酸盐通报,2003,(4): 11-15
[18]周建新,沈湘黔,景茂祥.板状氧化铝制备过程中影响因素的研究[J].矿冶工程,2005,25(2): 73-76
[19] L.M.Sheppard. Enhancing performance of ceramic composites [J]. J. Am. Ceram, 1992,71:617-631
[20] P.Bowen, J. Sheng, N. Jongen. Particle size distribution measurement of anisotropic-particles cylinders and platelets-practical examples [J]. Powder Technology, 2002, 128:256– 261
[21] L.C.Pathak, T.B. Singh, S. Das, et al. Effect of pH on the combustion synthesis of nano-crystalline alumina powder [J]. Materials Letters, 2002, 57:380–385
[22] Yiquan Wu, Yufeng Zhang, Xiaoxian Huang, et al. Preparation of platelike nano alpha aluminaparticles [J]. Ceramics International, 2001, 27:265-268
[23]丁祥金,张继周,桂子清等.粉料形貌对多孔Al2O3支撑体的影响[J].膜科学与技术, 2001,21(2):17-21
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