超声波辅助化学镀法制备铝酸盐尖晶石粉体的研究
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摘要
铝酸盐尖晶石化合物由于其结构的特殊性而成为一种具有很大潜力的功能材料,近年来它在磁性材料、介电陶瓷、半导体和催化剂等领域受到极大关注。常规的制备铝酸盐尖晶石的方法主要有溶胶凝胶法、固态反应法和水热合成法等,然而上述制备方法有许多缺点比如反应温度过高,颗粒过于粗大并且难于人为控制等等。
本文尝试了一种新的制备方法-化学镀包覆法来制备尖晶石粉体,主要步骤包括:Me/Al_2O_3→MeO/Al_2O_3,即首先通过镀覆方法制备金属包覆氧化铝生成Me/Al_2O_3复合超细粉体,经特定煅烧工艺生成金属氧化物.氧化铝(MeO/Al_2O_3)即铝酸盐尖晶石化合物复合粉体。
本文以超声波辅助化学镀法研究制备COAl_2O_4尖晶石粉体为例,采用化学镀包覆法合成了Co/Al_2O_3复合粉体,经高温热处理获得CoAl_2O_4尖晶石粉体;为了研究化学镀包覆法制备CoAl_2O_4尖晶石粉体的组织性能特点,利用常规溶胶凝胶法制备CoAl_2O_4尖晶石粉体以作对比。采用DTA、TEM、SEM和XRD等手段,对包覆法制备的Co/Al_2O_3复合粉体及COAl_2O_4尖晶石粉体的微观形貌,组织成分进行了测试,并对Co/Al_2O_3复合粉体的尖晶石转变温度进行了测定;以溶胶凝胶法制备的粉体为对比,对两种粉体的微观形貌,组织成分结构等作了测试与对比表征。
主要研究结果有:氧化铝粉体的镀前预处理对后续镀覆过程影响很大:原始粉体粗化后颗粒表面经腐蚀形成了凹坑和台阶等微细结构,使粉体表面变得粗糙;粗化粉体经敏化后表面吸附了具有还原性的Sn~(2+)离子;活化后粉体表面吸附贵金属钯,成为化学镀时具有自催化功能的形核中心。利用超声波辅助化学镀法制备了Co/Al_2O_3复合粉体,包覆前Al_2O_3粉体颗粒紧密堆积,单个颗粒呈现多角状,边缘清晰;包覆后镀层覆盖完整,粉体粒径显著长大,颗粒分散性好。镀覆后复合粉体的主要组成元素为Al、O和Co,相组成为Al_2O_3和Co。复合粉体的两相Al_2O_3和金属Co的组成形态:以Al_2O_3粉体为核心,大量Co微粒包覆在其表面。Co/Al_2O_3复合粉体经高温热处理获得了COAl_2O_4尖晶石粉体,尖晶石转变温度测定为890℃,尖晶石粉体后保留了包覆型结构的特征,最终获得的粉体是一种CoAl_2O_4/Al_2O_3壳--核型复合粉体,粉体主要由CoAl_2O_4和Al_2O_3两相组成。复合粉体的空间构型为:以Al_2O_3为核心,CoAl_2O_4包裹在其表面。与包覆-烧结制备的粉体作对比,溶胶凝胶法制备的CoAl_2O_4尖晶石粉体具有以下特点:溶胶凝胶法和化学镀法制备CoAl_2O_4尖晶石粉体的方法工艺不同,但有相同的尖晶石转变温度;溶胶凝胶法制得尖晶石相粉体成分严格符合化学计量比,而化学镀法制备的粉体由COAl_2O_4尖晶石相和Al_2O_3相组成;两种方法制备的粉体从微观形貌上来说,化学镀法制备的粉体粒度小而且一致均匀,比表面积大。
Aluminate spinel has been one kind of potential functional material due to its structural speciality and draws great attentions in magnetic materials,dielectric ceramics,semiconductors and catalysts in recent years.The conventional methods of preparing aluminate spinels include such as sol-gel,solid state reaction and hydrothermal synthesis etc.There are many defects in these conventional methods like that the reaction temperature is too high,the particle scales are overly coarse and can't be controlled efficiently.
A new synthesis of aluminate spinels-electroless plating has been tried as following steps:Me/Al_2O_3→MeO/Al_2O_3,first,the Me/Al_2O_3 composite powder is prepared via electroless plating and then transforms to MeO/Al_2O_3 composite powder which is just the aluminate spinel by special heat-treatment process.
The CoAl_2O_4 spinel was prepared as an example via ultrasonic assisted electroless plating.The Co/Al_2O_3 composite powder was prepared by electroless plating and transformed to CoAl_2O_4 spinels by heat-treatment.Another kind of CoAl_2O_4 spinel was prepared by sol-gel method in order to study the structure and properties of CoAl_2O_4 spinel prepared via electroless plating.The morphology, composition and crystalline structure were characterized by SEM,TEM and XRD.The spinel transition temperature of the Co/Al_2O_3 composite powder was characterized by DTA.Compared to the powder prepared by sol-gel process,the morphology, composition and structure of these two kinds of powder were tested in the same methods.
The result shows that:the pretreatment of Al_2O_3 powder evidently affects the later plating process.Microstructures as dents and ledges form at the surface of powder particles after coarsening which make the powder surface coarse.Sn_(2+)ions are adsorbed by the powder surface after sensitization and palladium forms at the particle surface via powder activation which is just the nucleation centre with autocatalytic properties in electroless plating.Co/Al_2O_3 composite powder was prepared via ultrasonic assisted electroless plating.The Al_2O_3 particles distribute closely and single particle is horned with clear edge before plating,but after plating the particles become bigger and disperse well due to the loose coating.The composition elements of the composite powder are Al,O,Co and composition phases are Al_2O_3 and Co which have a special structure that a large amount of Co particles enwrap the Al_2O_3 cores.Co/Al_2O_3 composite powder transform to CoAl_2O_4 spinels by heat-treatment and the transition temperature is 890℃.The powder after transition is one kind of CoAl_2O_4/Al_2O_3 composite powder with CoAl_2O_4 and Al_2O_3 composition phases and the structure is still as before that CoAl_2O_3 particles enwrap the Al_2O_3 cores.Another kind of CoAl_2O_4 spinel was prepared by sol-gel method as a comparison with the powder prepared via electroless plating.The results shows as follows:The powder prepared by these two methods gain spinel structure at the same temperature.The powder prepared by sol-gel meets to the stoichiometric proportion of cobalt aluminate.,but the element of Al is excessive in the powder prepared by electroless plating.Compared to sol-gel process, preparation of cobalt aluminate by electroless plating can not only gain smaller particle size and larger specific area but also control the particle size of the product. and reduce the cost since Al_2O_3 substitutes for part of CoAl-2O_4 and CoAl_2O_4 is more expensive.So,electroless plating is one effective method of preparing cobalt aluminate.
本文尝试了一种新的制备方法-化学镀包覆法来制备尖晶石粉体,主要步骤包括:Me/Al_2O_3→MeO/Al_2O_3,即首先通过镀覆方法制备金属包覆氧化铝生成Me/Al_2O_3复合超细粉体,经特定煅烧工艺生成金属氧化物.氧化铝(MeO/Al_2O_3)即铝酸盐尖晶石化合物复合粉体。
本文以超声波辅助化学镀法研究制备COAl_2O_4尖晶石粉体为例,采用化学镀包覆法合成了Co/Al_2O_3复合粉体,经高温热处理获得CoAl_2O_4尖晶石粉体;为了研究化学镀包覆法制备CoAl_2O_4尖晶石粉体的组织性能特点,利用常规溶胶凝胶法制备CoAl_2O_4尖晶石粉体以作对比。采用DTA、TEM、SEM和XRD等手段,对包覆法制备的Co/Al_2O_3复合粉体及COAl_2O_4尖晶石粉体的微观形貌,组织成分进行了测试,并对Co/Al_2O_3复合粉体的尖晶石转变温度进行了测定;以溶胶凝胶法制备的粉体为对比,对两种粉体的微观形貌,组织成分结构等作了测试与对比表征。
主要研究结果有:氧化铝粉体的镀前预处理对后续镀覆过程影响很大:原始粉体粗化后颗粒表面经腐蚀形成了凹坑和台阶等微细结构,使粉体表面变得粗糙;粗化粉体经敏化后表面吸附了具有还原性的Sn~(2+)离子;活化后粉体表面吸附贵金属钯,成为化学镀时具有自催化功能的形核中心。利用超声波辅助化学镀法制备了Co/Al_2O_3复合粉体,包覆前Al_2O_3粉体颗粒紧密堆积,单个颗粒呈现多角状,边缘清晰;包覆后镀层覆盖完整,粉体粒径显著长大,颗粒分散性好。镀覆后复合粉体的主要组成元素为Al、O和Co,相组成为Al_2O_3和Co。复合粉体的两相Al_2O_3和金属Co的组成形态:以Al_2O_3粉体为核心,大量Co微粒包覆在其表面。Co/Al_2O_3复合粉体经高温热处理获得了COAl_2O_4尖晶石粉体,尖晶石转变温度测定为890℃,尖晶石粉体后保留了包覆型结构的特征,最终获得的粉体是一种CoAl_2O_4/Al_2O_3壳--核型复合粉体,粉体主要由CoAl_2O_4和Al_2O_3两相组成。复合粉体的空间构型为:以Al_2O_3为核心,CoAl_2O_4包裹在其表面。与包覆-烧结制备的粉体作对比,溶胶凝胶法制备的CoAl_2O_4尖晶石粉体具有以下特点:溶胶凝胶法和化学镀法制备CoAl_2O_4尖晶石粉体的方法工艺不同,但有相同的尖晶石转变温度;溶胶凝胶法制得尖晶石相粉体成分严格符合化学计量比,而化学镀法制备的粉体由COAl_2O_4尖晶石相和Al_2O_3相组成;两种方法制备的粉体从微观形貌上来说,化学镀法制备的粉体粒度小而且一致均匀,比表面积大。
Aluminate spinel has been one kind of potential functional material due to its structural speciality and draws great attentions in magnetic materials,dielectric ceramics,semiconductors and catalysts in recent years.The conventional methods of preparing aluminate spinels include such as sol-gel,solid state reaction and hydrothermal synthesis etc.There are many defects in these conventional methods like that the reaction temperature is too high,the particle scales are overly coarse and can't be controlled efficiently.
A new synthesis of aluminate spinels-electroless plating has been tried as following steps:Me/Al_2O_3→MeO/Al_2O_3,first,the Me/Al_2O_3 composite powder is prepared via electroless plating and then transforms to MeO/Al_2O_3 composite powder which is just the aluminate spinel by special heat-treatment process.
The CoAl_2O_4 spinel was prepared as an example via ultrasonic assisted electroless plating.The Co/Al_2O_3 composite powder was prepared by electroless plating and transformed to CoAl_2O_4 spinels by heat-treatment.Another kind of CoAl_2O_4 spinel was prepared by sol-gel method in order to study the structure and properties of CoAl_2O_4 spinel prepared via electroless plating.The morphology, composition and crystalline structure were characterized by SEM,TEM and XRD.The spinel transition temperature of the Co/Al_2O_3 composite powder was characterized by DTA.Compared to the powder prepared by sol-gel process,the morphology, composition and structure of these two kinds of powder were tested in the same methods.
The result shows that:the pretreatment of Al_2O_3 powder evidently affects the later plating process.Microstructures as dents and ledges form at the surface of powder particles after coarsening which make the powder surface coarse.Sn_(2+)ions are adsorbed by the powder surface after sensitization and palladium forms at the particle surface via powder activation which is just the nucleation centre with autocatalytic properties in electroless plating.Co/Al_2O_3 composite powder was prepared via ultrasonic assisted electroless plating.The Al_2O_3 particles distribute closely and single particle is horned with clear edge before plating,but after plating the particles become bigger and disperse well due to the loose coating.The composition elements of the composite powder are Al,O,Co and composition phases are Al_2O_3 and Co which have a special structure that a large amount of Co particles enwrap the Al_2O_3 cores.Co/Al_2O_3 composite powder transform to CoAl_2O_4 spinels by heat-treatment and the transition temperature is 890℃.The powder after transition is one kind of CoAl_2O_4/Al_2O_3 composite powder with CoAl_2O_4 and Al_2O_3 composition phases and the structure is still as before that CoAl_2O_3 particles enwrap the Al_2O_3 cores.Another kind of CoAl_2O_4 spinel was prepared by sol-gel method as a comparison with the powder prepared via electroless plating.The results shows as follows:The powder prepared by these two methods gain spinel structure at the same temperature.The powder prepared by sol-gel meets to the stoichiometric proportion of cobalt aluminate.,but the element of Al is excessive in the powder prepared by electroless plating.Compared to sol-gel process, preparation of cobalt aluminate by electroless plating can not only gain smaller particle size and larger specific area but also control the particle size of the product. and reduce the cost since Al_2O_3 substitutes for part of CoAl-2O_4 and CoAl_2O_4 is more expensive.So,electroless plating is one effective method of preparing cobalt aluminate.
引文
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