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采用自制异丙醇铝,通过溶胶—凝胶法制备了氧化铝凝胶,在低温下烧成Al2O3透明多晶薄膜。用XPS技术探究了加热过程中桥氧的变化及铝氧基团中Al3+配位状态的变化规律。用英国VG公司产ESCALABMarkⅡ型XPS仪,MgKα射线作激发源(1253.6eV),计算机自动录谱、分峰拟合。将干凝胶及其300℃、400℃、600℃、800℃、1000℃的热处理产物依次编号为G1、G2、G3、G4、G5及G6。对上述试样进行XPS测试。对各试样的O1sXPS特征峰的分峰拟合发现,可将其分为两个峰,高能峰表征桥氧Ob,低能峰表征非桥氧Onb。在氧化铝凝胶及其热处理产物中,桥氧以Al—O—的形式存在,非桥氧以—H—O—Al的形式存在,故各试样中Al、O、H可能结合成分子量不等的一系列无机大分子,在这些无机大分子中,桥氧与非桥氧的相对含量及其变化呈现一定的规律性。在低温下获得的干凝胶中,Ob/Onb=1,桥氧与非桥氧的含量近乎于相等,随着热处理温度的升高,桥氧相对减少,非桥氧相对增加,表明无机大分子的Al—O键在加热状态下发生断裂,分子量降低。但1000℃热处理产物中,桥氧又呈上升趋势,表明Al、O的结合状态,即Al的配?
Alumina gel was prepared by sol-gel method and self-made aluminum isopropoxide was used to prepare Al2O3 transparent polycrystalline thin films at low temperature. The XPS technique was used to investigate the changes of bridging oxygen and the Al3 + coordination state in the aluminum-oxygen groups. With the British VG company ESCALABMark Ⅱ type XPS instrument, MgKα rays as the excitation source (1253.6eV), the computer automatically recorded spectrum, sub-peak fitting. The xerogels and their heat-treated products at 300, 400, 600, 800 and 1000 ° C were numbered G1, G2, G3, G4, G5 and G6 in order. XPS test on the above sample. The peak fitting of the O1sXPS characteristic peak of each sample shows that it can be divided into two peaks, the high energy peak characterizes the bridging oxygen Ob and the low energy peak characterizes the non-bridging oxygen Onb. In the alumina gel and its heat treatment products, the bridging oxygen exists in the form of Al-O-, and the non-bridging oxygen exists in the form of -H-O-Al. Therefore, Al, O and H in each sample may be combined into the molecular weight Ranging from a series of inorganic macromolecules, in these inorganic macromolecules, the relative content of bridge oxygen and non-bridging oxygen and its changes showed a certain regularity. In the dry gel obtained at low temperature, Ob / Onb = 1, the content of bridging oxygen and non-bridging oxygen is almost equal, with the heat treatment temperature, the relative reduction of bridging oxygen, non-bridging oxygen relative increase, indicating that inorganic large Molecular Al-O bond in the heating state fracture, molecular weight decreases. However, at 1000 ℃ heat treatment products, the bridge oxygen is on the rise, indicating that the bonding state of Al, O, that Al with?