热门关键词: 2025 è¾å ¥å ³é®è¯ 2023
钛合金具有比强度高、耐蚀性好、抗蠕变性好等显著优点,目前已经在航空航天、石油炼化、交通、医疗器械等领域实现了广泛应用。至今已发展出多种不同牌号的钛合金,添加元素的种类和含量严重影响钛合金的性能,因此,杂质含量要严格控制,一般来说,单元素杂质含量不超过0.1%,总杂质含量不超过0.4%。为了准确测试合金中的元素含量,国内外已开发出众多化学分析方法,如电感耦合等离子体原子发射光谱法(ICP-OES)、火焰原子吸收光谱法、X射线荧光光谱分析法、分光光度法、电位滴定法等。但是这些方法操作繁琐、耗时长、存在一定的干扰,且需要几种方法联合测定才能完成对多种元素的含量测定,样品用量较多。全谱直读光谱法作为一种快速测试方法,无须溶解样品,只需要对样品表面进行处理后,便可以进行直接测定。本实验采用全谱直读光谱法进行测试,通过筛选分析谱线以避免干扰、选择合适的通道及调整仪器的工作参数,建立了一种快速、准确的分析方法,同时测定了钛合金中铝、硅、铁、钒、钼、铌、锆7种元素的含量。
Q4型全谱直读光谱仪(德国布鲁克公司生产);普通车床;高纯氩气(纯度为99.999%);分析纯无水乙醇;钛合金标准物质。工作温度为15~30℃;工作湿度为20%~80%;光谱测量范围为130~800 nm;分析间隙为4 mm;火花室控制气氛为氩气,其纯度不低于99.999%;氩气流量:分析时2~4 L/min,载气压力0.4 MPa;冲洗5秒,样品激发时间11 s,积分时间10 s;曝光2次,放电时间:10μs~2 ms;总分析时间23 s。
将钛合金样品用车床车制,并控制转速为800 r/min,然后用细砂纸打磨,酒精擦拭。保证样品直径大于20 mm,厚度大于5 mm,试样大小能完全覆盖激发孔的直径,分析面平整、光洁、干燥、无油污、电解液和水渍;标准样品制备同样品。用钛合金块状光谱标准物质在Ti100通道下进行类型标准化,即绘制工作曲线,工作曲线的相关系数满足要求后,用钛合金标准物质作为控制样品进行验证。
在样品分析过程中,多次激发样品的目的是驱逐气路中的空气及上次试验的元素残留,冲洗时间即高纯氩气冲洗仪器工作回路的时间。氩气的冲洗时间由激发室容积的大小、氩气流量及其纯度等因素决定。积分时间(曝光时间)主要取决于样品中各元素的分析谱线和含量范围。为确定上述分析条件,对同一块钛合金标准样品进行光强度试验。结果表明当冲洗时间5 s,激发时间11 s,积分时间10 s,曝光2次,放电时间10μs~2 ms的条件下,各元素的光强度基本稳定。选择的各元素分析谱线波长见表1。
元素 | Ti(内标) | A1 | Si | Fe | Mo | V | Nb | Zr |
波长λ/nm | 301.7 | 394.4 | 288.1 | 275.5 | 287.2 | 311.2 | 410.0 | 357.2 |
元素 | 分析谱线/nm | 线性方程 | 相关系数r | 检出限/% |
Al | 394.4 | y=274257x-41926 | 0.9982 | 0.0009 |
Si | 288.1 | y=1,531,974x-10,971 | 0.9992 | 0.0020 |
Fe | 275.5 | y=269208x+4503.9 | 0.9980 | 0.0008 |
V | 311.2 | y=82159x-23272 | 0.9970 | 0.0010 |
Mo | 287.2 | y=33775x+78312 | 0.9987 | 0.0030 |
Nb | 410.0 | y=61033x+721639 | 0.9999 | 0.0010 |
Zr | 357.2 | y=163253x+15795 | 0.9979 | 0.0010 |
元素 | 标准样品 | 标准值/% | 测定值/% | 平均值/% | RSD/% |
Al | BS T-22 | 0.004 | 0.004,0.005,0.004,0.005,0.005,0.005,0.004,0.005,0.004,0.004 | 0.0051 | 4.89 |
Ti1023-18 | 3.31 | 3.45,3.33,3.32,3.35,3.55,3.45,3.35,3.35,3.47,3.40 | 3.40 | 2.21 | |
GBW(E)010072 | 7.78 | 7.81,7.85,7.79,7.82,7.75,7.72,7.90,7.86,7.82,7.82 | 7.81 | 0.67 | |
Si | TC21 | 0.024 | 0.025,0.026,0.027,0.027,0.028,0.027,0.027,0.028,0.027,0.028 | 0.027 | 3.49 |
101X Ti2 | 0.110 | 0.112,0.113,0.113,0.109,0.113,0.108,0.113,0.110,0.113,0.114 | 0.112 | 1.83 | |
GBW(E)020178 | 0.261 | 0.263,0.270,0.265,0.258,0.260,0.265,0.261,0.271,0.260,0.260 | 0.263 | 1.68 | |
Fe | TC21 | 0.047 | 0.045,0.045,0.047,0.050,0.045,0.045,0.046,0.045,0.047,0.048 | 0.046 | 3.67 |
Ti 6-2-178D | 0.66 | 0.63,0.65,0.64,0.66,0.67,0.64,0.68,0.68,0.67,0.67 | 0.659 | 2.72 | |
Ti1023-18 | 1.98 | 2.00,2.02,1.95,1.94,2.06,2.05,2.02,2.02,2.02,2.02 | 2.01 | 1.91 | |
V | BS T-22 | 0.500 | 0.507,0.503,0.514,0.520,0.489,0.511,0.507,0.507,0.497,0.497 | 0.505 | 1.80 |
Ti 6-2-178D | 5.41 | 5.45,5.36,5.45,5.35,5.45,5.45,5.45,5.55,5.45,5.45 | 5.44 | 1.01 | |
Ti1023-18 | 9.75 | 9.77,9.70,9.68,9.71,9.67,9.75,9.70,9.75,9.74,9.72 | 9.72 | 0.34 | |
Mo | Ti1023-18 | 0.0030 | 0.0033,0.0034,0.0032,0.0033,0.0033,0.0035,0.0033,0.0033,0.0034,0.0033 | 0.0033 | 2.47 |
GBW(E)010072 | 1.76 | 1.78,1.76,1.80,1.75,1.77,1.80,1.74,1.74,1.72,1.72 | 1.76 | 1.67 | |
101P 205 | 15.3 | 15.5,15.5,15.6,15.4,15.5,15.6,15.5,15.6,15.5,15.5 | 15.5 | 0.41 | |
Nb | 101X Ti6 | 0.0639 | 0.0624,0.0655,0.0596,0.0622,0.0633,0.0600,0.0650,0.0598,0.0653,0.0637 | 0.0631 | 3.34 |
101X Ti1 | 2.75 | 2.80,2.82,2.78,2.85,2.78,2.66,2.75,2.80,2.80,2.76 | 2.78 | 1.83 | |
GBW02521 | 3.94 | 3.94,4.02,3.94,3.92,3.98,3.93,3.88,3.90,3.87,3.99 | 3.94 | 1.23 | |
Zr | BS T-22 | 0.010 | 0.013,0.011,0.009,0.012,0.015,0.009,0.011,0.012,0.013,0.01 | 0.012 | 3.34 |
TC21 | 1.99 | 2.05,2.02,2.05,2.05,2.05,1.95,2.00,2.02,2.00,1.99 | 2.01 | 1.95 | |
GBW(E)010069 | 5.35 | 5.38,5.45,5.38,5.42,5.33,5.42,5.38,5.38,5.43,5.41 | 5.40 | 0.64 |
元素 | 标准样品 | 标准值/% | 测定值/% | 测定平均值/% | 准确度/% | RSD/% |
Al | GBW(E)020034 | 5.80 | 6.05, 6.04, 6.05 | 6.03 | 100.22 | 0.096 |
Si | GBW(E)020034 | 0.33 | 0.23, 0.25, 0.23 | 0.24 | 98.61 | 4.87 |
Fe | GBW(E)020034 | 0.485 | 0.047, 0.048, 0.051 | 0.049 | 101.38 | 4.28 |
V | GBW(E)020035a | 3.61 | 3.60, 3.65, 3.76 | 3.67 | 101.66 | 2.23 |
Mo | GBW(E)020034 | 2.02 | 2.82, 2.90, 2.78 | 2.83 | 98.60 | 2.16 |
Nb | GBW(E)020034 | 1.97 | 2.00, 2.02, 2.02 | 2.01 | 102.20 | 0.57 |
Zr | GBW(E)020034 | 1.53 | 2.00, 1.97, 1.95 | 1.97 | 99.16 | 1.27 |