光谱学与光谱分析
光譜學與光譜分析
광보학여광보분석
SPECTROSCOPY AND SPECTRAL ANALYSIS
2015年
5期
1376-1382
,共7页
孙玉祥%钟石磊%卢渊%孙欣%马军艳%刘哲
孫玉祥%鐘石磊%盧淵%孫訢%馬軍豔%劉哲
손옥상%종석뢰%로연%손흔%마군염%류철
激光诱导击穿光谱%薄膜%等离子体图像
激光誘導擊穿光譜%薄膜%等離子體圖像
격광유도격천광보%박막%등리자체도상
Laser induced breakdow n spectroscopy%Film%Plasma imaging
为了发展一种实时、快速、非接触,能对金属氧化物纳米薄膜中元素成分进行分析的检测方法,搭建了一套基于L IBS技术的薄膜检测分析系统。该系统可同时实现样品平面的精确定位,样品烧蚀坑形貌实时观测,等离子体成像和光谱采集等功能。样品为在单晶硅基底上利用溶胶-凝胶法制备的约40 nm厚的氧化锆功能薄膜,实验中将其放置在一个位移精度为0.01 m m的三维平移台上。系统测试结果表明,在两束聚焦的连续激光辅助下,样品平面的定位精度达到了20μm ,LIBS单脉冲检测光谱信号的面积分强度的重复性的相对标准偏差(RSD )达到了1.6%。在室温和大气环境下,对等离子体空间分布、信号强度随激发能量、时间参数和LTSD(激光聚焦点到样品表面的距离)参数而变化的情况从光谱角度进行了实验研究,并优化了实验参数和探测参数。利用实验得到的光谱数据,用玻尔兹曼方计算了等离子体的电子温度,利用硅的原子线计算了电子密度,对定量检测所必须的局部热力学平衡(LTE)条件进行了评价。
為瞭髮展一種實時、快速、非接觸,能對金屬氧化物納米薄膜中元素成分進行分析的檢測方法,搭建瞭一套基于L IBS技術的薄膜檢測分析繫統。該繫統可同時實現樣品平麵的精確定位,樣品燒蝕坑形貌實時觀測,等離子體成像和光譜採集等功能。樣品為在單晶硅基底上利用溶膠-凝膠法製備的約40 nm厚的氧化鋯功能薄膜,實驗中將其放置在一箇位移精度為0.01 m m的三維平移檯上。繫統測試結果錶明,在兩束聚焦的連續激光輔助下,樣品平麵的定位精度達到瞭20μm ,LIBS單脈遲檢測光譜信號的麵積分彊度的重複性的相對標準偏差(RSD )達到瞭1.6%。在室溫和大氣環境下,對等離子體空間分佈、信號彊度隨激髮能量、時間參數和LTSD(激光聚焦點到樣品錶麵的距離)參數而變化的情況從光譜角度進行瞭實驗研究,併優化瞭實驗參數和探測參數。利用實驗得到的光譜數據,用玻爾玆曼方計算瞭等離子體的電子溫度,利用硅的原子線計算瞭電子密度,對定量檢測所必鬚的跼部熱力學平衡(LTE)條件進行瞭評價。
위료발전일충실시、쾌속、비접촉,능대금속양화물납미박막중원소성분진행분석적검측방법,탑건료일투기우L IBS기술적박막검측분석계통。해계통가동시실현양품평면적정학정위,양품소식갱형모실시관측,등리자체성상화광보채집등공능。양품위재단정규기저상이용용효-응효법제비적약40 nm후적양화고공능박막,실험중장기방치재일개위이정도위0.01 m m적삼유평이태상。계통측시결과표명,재량속취초적련속격광보조하,양품평면적정위정도체도료20μm ,LIBS단맥충검측광보신호적면적분강도적중복성적상대표준편차(RSD )체도료1.6%。재실온화대기배경하,대등리자체공간분포、신호강도수격발능량、시간삼수화LTSD(격광취초점도양품표면적거리)삼수이변화적정황종광보각도진행료실험연구,병우화료실험삼수화탐측삼수。이용실험득도적광보수거,용파이자만방계산료등리자체적전자온도,이용규적원자선계산료전자밀도,대정량검측소필수적국부열역학평형(LTE)조건진행료평개。
In order to develop a method to analyze the metal elements in the thin film samples rapidly ,directly and without sam-ple preparation ,a laboratory LIBS system was established recently for nanometer film analysis .This system could determine the position of sample plane ,observe the profiles of sample after pulse-material interaction and detect the plasma morphologyand spectral emission at the same time .Samplesused were ZrO2 films about 40 nm thickness prepared on Si by a sol-gel process ,and they were located on a manual X-Y-Z translational stage with theaccuracy of 0.01 mm .Final results showed that the positional accuracy is about 20μm with the help of two CW lasers ,and the RSD of repeatability of single-shot spectra could be to 1.6% . We investigated special morphology of plasma ,variation tendency of signal intensity as a function of pulse energy ,LTSD (laser focus to sample distance) and time ,which provide cornerstone for optimizing experimental parameters under the conditions of room temperature and atmospheric pressure .We calculated plasma temperature by way of Boltzmann curve and electron densi-tythrough the acquired data .We also appraised necessary LTE conditions for quantitativeanalysis .