發(fā)布時(shí)間：2018-05-08 20:27

  本文選題：氧化鎳 + 微波　； 參考：《江西理工大學(xué)》2015年碩士論文

【摘要】：氧化鎳作為一種功能性材料,因其具有良好的電化學(xué)活性與電致光性、較強(qiáng)的熱敏性和催化性,而被廣泛地應(yīng)用在催化劑、超級(jí)電容器、氣敏傳感器、功能陶瓷材料、特種涂料以及光吸收材料等領(lǐng)域。為了制備形貌規(guī)則且分散性良好的氧化鎳粉體,于是單一微波熱合成法、有機(jī)配合物前驅(qū)體法、噴霧熱解法、溶膠-凝膠法、微乳液法等逐漸被開發(fā)出來。其中對(duì)單一微波或超聲波輔助合成氧化鎳的研究較多,但微波與超聲波協(xié)同尚未有公開報(bào)道。因此,本文采用微波與超聲波協(xié)同輔助液相均勻共沉淀法制備超細(xì)氧化鎳,主要的工作和相關(guān)的成果如下:本論文以Ni Cl2·6H2O為原料,CO(NH2)2和H2C2O4為沉淀劑,分別考察了加熱方式、氯化鎳的起始濃度、反應(yīng)溫度、反應(yīng)時(shí)間、反應(yīng)配比、陳化時(shí)間、有無添加修飾劑等的介入對(duì)氧化鎳前驅(qū)體的形貌以及粒徑的影響。實(shí)驗(yàn)結(jié)果表明,微波與超聲波協(xié)同輔助液相均勻共沉淀法制備超細(xì)氧化鎳前驅(qū)體要優(yōu)于單一微波輻射加熱和常規(guī)的水浴加熱模式;以尿素和草酸為沉淀劑分別制備出類球狀與塊狀兩種形貌的氧化鎳前驅(qū)體。在微波與超聲波協(xié)同作用下,Ni2+的濃度為0.1 mol·L-1、CO(NH2)2的濃度為1 mol·L-1、反應(yīng)溫度90℃、反應(yīng)時(shí)間120min、無需陳化,即可得到類球形且分散性良好的氧化鎳前驅(qū)體;修飾劑pvp的添加對(duì)改善氧化鎳前驅(qū)體的團(tuán)聚效果并不明顯;氧化鎳前驅(qū)體在微波干燥箱中采用低檔干燥90min形貌較好。Ni O前驅(qū)體的熱分解過程,主要考察了熱分解溫度和保溫時(shí)間對(duì)氧化鎳粉體形貌以及粒徑的影響。由熱重-差熱分析可知,在熱分解溫度大于300℃時(shí),有氧化物生成;XRD和FT-IR結(jié)果顯示,大于300℃時(shí)所生產(chǎn)的氧化物為立方晶型的Ni O粉體,且隨著熱分解溫度的升高,Ni O顆粒晶型更完整;SEM結(jié)果表明,Ni O粉體繼承了其前驅(qū)體的形貌,呈類球形,分散性良好,粒徑分布在0.8~1.5μm,與前驅(qū)體的粒徑分布相差不大。綜合多種分析表征可知,熱分解溫度過低,則沒有氧化鎳粉體生成或分解不完全;當(dāng)熱分解溫度過高時(shí),粉體容易出現(xiàn)“燒結(jié)”;故焙燒Ni O前驅(qū)體的較優(yōu)工藝:熱分解溫度為300~500℃,保溫時(shí)間為90min。
[Abstract]:As a functional material, nickel oxide has been widely used in catalysts, supercapacitors, gas sensors and functional ceramics because of its good electrochemical activity and electroluminescence, strong thermal sensitivity and catalytic properties. Special coatings and light absorption materials and other areas. In order to prepare nickel oxide powders with regular morphology and good dispersion, single microwave thermal synthesis method, organic complex precursor method, spray pyrolysis method, sol-gel method and microemulsion method were gradually developed. There are many studies on the single microwave or ultrasonic assisted synthesis of nickel oxide, but the cooperation of microwave and ultrasonic has not been reported. Therefore, in this paper, microwave-ultrasonic assisted liquid phase homogeneous coprecipitation method is used to prepare ultrafine nickel oxide. The main work and related results are as follows: in this thesis, Ni Cl2 6H2O was used as raw materials, COG NH _ 2H _ 2 and H2C2O4 as precipitators, and the heating methods were investigated, respectively. The influence of the initial concentration of nickel chloride, reaction temperature, reaction time, reaction ratio, aging time and the addition of modifier on the morphology and particle size of nickel oxide precursor was investigated. The experimental results show that the microwave-ultrasonic assisted liquid phase homogeneous coprecipitation method is superior to single microwave radiation and conventional water bath heating mode in preparing superfine nickel oxide precursor. Using urea and oxalic acid as precipitators, the spherical and bulk nickel oxide precursors were prepared. Under the synergistic action of microwave and ultrasonic wave, the concentration of Ni _ 2 was 0.1 mol L ~ (-1), the concentration of COO _ (2) NH _ (2) was 1 mol / L ~ (-1), the reaction temperature was 90 鈩，

本文編號(hào)：1862952