【摘要】：氧化鋯具有良好的力學(xué)、熱學(xué)、化學(xué)以及生物相容性等性能,納米化后的氧化鋯的性能發(fā)生變化并且出現(xiàn)一些新的特性。納米玻璃由于具有全新的原子結(jié)構(gòu)排列,因而可能會具有不同于納米陶瓷的新的性能。非晶態(tài)Zr02由于短程有序長程無序的非晶結(jié)構(gòu),熱力學(xué)上的亞穩(wěn)態(tài),高介電常數(shù)特性,在半導(dǎo)體、催化劑、光學(xué)器件等方面有較好的應(yīng)用前景。本文設(shè)想通過壓制非晶態(tài)氧化鋯納米顆粒來制備氧化鋯納米玻璃,因此納米尺寸的、球形的、粒徑分布窄的、團聚少的非晶態(tài)氧化鋯顆粒的制備成為納米玻璃研究的基礎(chǔ)。非晶態(tài)氧化鋯納米顆�？赏ㄟ^低溫煅燒顆粒尺寸細小、形貌規(guī)則、粒徑分布窄、團聚少的氧化鋯前驅(qū)體來制備。文獻報道的制備方法存在團聚嚴(yán)重、成本高、操作復(fù)雜等缺點。因此,探索在低成本下制備高質(zhì)量氧化鋯前驅(qū)體納米顆粒的方法是急需解決的問題。本文采用溶膠-凝膠法和均勻沉淀法來制備氧化鋯前驅(qū)體納米顆粒。將制得的氧化鋯前驅(qū)體在空氣中300℃煅燒,得到非晶態(tài)氧化鋯納米顆粒。通過X射線衍射分析、紅外光譜分析、熱重/差熱分析、掃描電子顯微鏡分析、透射電子顯微鏡分析,對制備的樣品的結(jié)構(gòu)、組成、形貌進行表征。在溶膠-凝膠法中,將氧氯化鋯溶于醇與水的混合溶液中,水浴加熱得到凝膠,再用氨水進行滴定,得到氧化鋯前驅(qū)體。實驗和表征結(jié)果表明,醇的種類、醇-水體積比、水浴溫度、反應(yīng)物濃度、干燥方式均對產(chǎn)物的形貌、尺寸和分散性產(chǎn)生影響。實驗的最佳制備條件如下:水浴溫度60℃,選擇異丙醇,醇與水體積比5:1,氧氯化鋯濃度5 mM,制備得到非晶態(tài)氧化鋯納米顆粒,顆粒間存在一定的團聚,平均顆粒尺寸為17 nm。在均勻沉淀法中,以硫酸鋯、硝酸鋯為鋯源,以甲酰胺(CH3NO)為沉淀劑,制備了團聚輕、粒徑分布較窄的氧化鋯前驅(qū)體。使用聚乙二醇(PEG)為表面活性劑,通過調(diào)整鋯離子濃度、硝酸根與硫酸根的比例,對樣品顆粒尺寸進行控制。結(jié)果表明,當(dāng)硝酸鋯與硫酸鋯的摩爾比為8:1,鋯離子濃度在1mM時,產(chǎn)物為非晶態(tài)氧化鋯納米顆粒,顆粒形貌近似球形,分散性良好,且顆粒尺寸分布在5~25 nm之間,平均顆粒尺寸14 nm。
[Abstract]:Zirconia has good mechanical, thermal, chemical and biocompatibility properties. The properties of nanocrystalline zirconia have changed and some new properties have appeared. Nanocrystalline glasses may have new properties different from nanocrystalline because of their new atomic structure. Amorphous Zr02 has promising applications in semiconductor, catalyst and optical devices due to its short range ordered long range disordered amorphous structure, thermodynamics metastable state and high dielectric constant. In this paper, the preparation of amorphous zirconia nanocrystals by pressing amorphous zirconia nanoparticles is envisaged. Therefore, the preparation of nanometer-sized, spherical, narrow particle size and less agglomeration amorphous zirconia particles becomes the basis of the study of nanocrystalline glasses. Amorphous zirconia nanoparticles can be prepared by calcined zirconia precursors with small size, regular morphology, narrow particle size distribution and less agglomeration at low temperature. It is reported that the preparation method has the disadvantages of serious agglomeration, high cost and complicated operation. Therefore, it is urgent to explore the method of preparing high quality zirconia nanoparticles at low cost. In this paper, zirconia precursor nanoparticles were prepared by sol-gel method and homogeneous precipitation method. The zirconia precursor was calcined in air at 300 鈩，

本文編號：2321949