Identification of relaxation maxima of internal friction in the Zr – Nb alloy after nitriding, oxidation in air, and in situ carburization

V. Anan’in, B. Kalin, V. Novikov, A. V. Sumarokova
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Abstract

The internal friction method was used to study the behavior of the Zr – 1 wt. % Nb alloy after oxidation in air, nitriding in an atmosphere of technical nitrogen, and in situ carburization during measurements. In this case, carbon was deposited on the samples during measurements due to thermal decomposition of vapors of diffusion oil. The pressure in the system was about 10–2 Pa. The temperature dependence of the logarithmic decrement of damped bending vibrations with a frequency of 2.2 – 2.4  Hz was measured on specimens in the form of a rectangular plate 22 × 8 × 0.3 mm in size. The measurements were carried out at a constant heating rate of about 4 K/min from room temperature to 700 – 750 °C. The obtained temperature dependences of internal friction were divided into partial maxima using a special program. The program determines the temperatures of the relaxation maxima and calculates the effective activation energy using the Werth — Marx formula. The internal friction spectra in successive measurements on one sample changed due to the diffusion redistribution of the alloy components. The parameters of the relaxation maxima for carbon (153 – 159 kJ/mol), oxygen (203 – 207 kJ/mol) and nitrogen (235 – 238 kJ/mol) in the alloy under study, depending on the experimental conditions, have been established. Grain-boundary (Gb) impurity maxima due to these impurities were also found. The following activation energies were obtained: 173 – 179 kJ/mol for C-Gb, 216 – 219  kJ/mol for O-Gb and 222 – 229 kJ/mol for N-Gb. Impurity grain-boundary maxima associated with carbon, oxygen, and nitrogen were observed in each series of measurements. The activation energy of the grain-boundary maxima proper decreases monotonically from 202.4 to 194.5 kJ/mol in a series with oxidation in air (experiments 711 – 715), and remains about 200 kJ/mol in nitrided samples.
氮化、空气氧化和原位渗碳后Zr - Nb合金内摩擦弛豫最大值的确定
采用内摩擦法研究了Zr - 1wt . % Nb合金在空气中氧化、在工业氮气气氛中渗氮和测量时的原位渗碳行为。在这种情况下,由于扩散油蒸气的热分解,碳在测量期间沉积在样品上。系统的压强大约是10 - 2pa。在尺寸为22 × 8 × 0.3 mm的矩形板上测量了频率为2.2 - 2.4 Hz的阻尼弯曲振动对数衰减的温度依赖性。测量在恒定的加热速率下进行,从室温到700 - 750℃,加热速率约为4 K/min。利用特殊的程序将得到的内摩擦温度依赖关系划分为局部最大值。该程序确定了松弛最大值的温度,并使用沃斯-马克思公式计算有效活化能。由于合金成分的扩散再分布,在同一样品上连续测量的内摩擦谱发生了变化。根据不同的实验条件,确定了合金中碳(153 ~ 159 kJ/mol)、氧(203 ~ 207 kJ/mol)和氮(235 ~ 238 kJ/mol)的弛豫最大值参数。还发现了由这些杂质引起的晶界(Gb)杂质最大值。得到的活化能分别为:C-Gb为173 ~ 179 kJ/mol, O-Gb为216 ~ 219 kJ/mol, N-Gb为222 ~ 229 kJ/mol。在每一系列测量中都观察到与碳、氧和氮有关的杂质晶界最大值。在空气氧化过程中(实验711 ~ 715),晶界活化能最大值从202.4 ~ 194.5 kJ/mol单调降低,氮化样品的晶界活化能最大值保持在200 kJ/mol左右。
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