XPS에서 파이썬으로 구현한 Thickogram의 박막 두께 측정 웹 프로그램

이종완 한국물리학회 2021 새물리 Vol.71 No.12

One of the most important applications of XPS (X-ray photoelectron spectroscopy) is to measure the film thickness by using AR-XPS (angle-resolved XPS). The so-called thickogram, which is a nomogram, was developed as an alternative graphical solution to calculate the film thickness easily from the XPS data. It is, however, uncomfortable to photocopy the thickogram and to apply ruler and pencil for finding the graphical intersection. In this research, we developed a computer program with python to automate the thickogram, and published it as an open source on the web so that everyone can access it for the calculation of a film thickness. XPS (X-ray Photoelectron Spectroscopy: X-선 광전자 분광법)의 가장 중요한 응용분야 중의 하나는AR-XPS (Angle-resolved XPS) 를 이용한 박막의 두께 측정이다. XPS 데이터로부터 박막의 두께를쉽게 계산하기 위해서 nomogram인 소위 Thickogram이 개발되었다. 종이에 복사해서 자와 연필로직선을 그어 교차점을 읽어 사용하는 Thickogram은 이제는 불편할 수 밖에 없다. 본 논문에서는 파이썬언어를 이용하여 컴퓨터 프로그램으로 Thickogram을 자동화시켰으며 누구나 쉽게 박막의 두께를 계산할수 있도록 인터넷 상에 오픈소스로 웹사이트를 제공하였다.

Ultra-thin SiO₂ on Si VIII. Accuracy of method, linearity and attenuation lengths for XPS

Kim, Kyung Joong,Seah, M. P. Heyden & Son 2007 Surface and interface analysis Vol.39 No.6

<P>In the study of ultra-thin films (<10-nm thick), there is a range of methods that can provide accurate measurements of differences in thickness. However, in a pilot study under the auspices of the Consultative Committee for Amount of Substance (CCQM), results for the archetypal system of SiO<SUB>2</SUB> on Si show that the methods have different offsets such that, at all thicknesses, positive or negative amounts in the range up to 1 nm may be observed between methods. All the methods studied give thicknesses that are greater than those measured by X-ray photoelectron spectroscopy (XPS) by amounts between 0.2 nm and approximately 1 nm. Significant parts of these offsets, of other methods with respect to XPS, may be attributed to contaminations which increase the apparent thickness but that do not affect XPS. However, not all of these offsets can yet be explained at the 0.2 nm level. The remaining part of the offsets could be thought to have arisen either from the XPS or from the other methods. In this study, by measuring SiO<SUB>2</SUB> deposited in situ on amorphous Si by XPS it is shown that the XPS linearity is consistent with the previous estimate of ± 0.025 nm, down to fractions of a monolayer, with no significant offset and that, therefore, it is the offsets seen using other methods that need further study. Recent calculations of the film thickness dependence of the attenuation lengths (ALs) for this system, using NIST SESSA software, are not consistent with these data although earlier calculations are. This work shows that XPS, with the AL calibrated by one or more other methods that are valid for differences in thickness, can provide a traceable measurement of thickness in all laboratories. © Crown Copyright 2007. Reproduced with the permission of Her Majesty's Stationery Office. Published by John Wiley & Sons, Ltd.</P>

HCD 이온플레이팅 장치 제작 및 Stainless Steel 위에TiN 박막의 미세색상변화에 따른 XPS분석

박문찬,이종근,최광호,차정원,김응순,박진흥 한국안광학회 2010 한국안광학회지 Vol.15 No.4

Purpose: HCD ion plating apparatus by hollow cathod discharge method was fabricated and TiN films were deposited on stainless steel by this apparatus with increasing in N2 gas flow and the fine color changes of TiN films were analyzed. Methods: The spectroradiometer and spectrophotometer were used to observe optically the fine color changes of TiN thin films, and XPS was used to analyze the compositions of TiN thin films with increasing in N2 gas flow. Results: The color coordinate of TiN thin film with N2 120 sccm gas flow showed (0.382, 0.372) which had the mixed colors of gold and silver, and the color coordinate changed to the increasing value of (x,y) with increasing in N2 gas flow which indicated the deep gold color. It was found that the slopes of the reflectances at 550nm were increased with increasing in N2 gas flow. And from the Ti scans using XPS, it was found that the peak heights of 455 eV derived from TiN composition were increased with increasing in N2 gas flow, while the peak heights of 459 eV from TiO2 composition were decreased. Conclusions: The results obtained above were that the color of TiN film with 120 sccm N2 gas flow had been observed from the mixed color of silver and gold due to TiC, TiO2, TiN on the surface and TiN, TiO2 inside film, and the color of TiN films changed a deep gold color with increasing in N2 gas flow due to increasing TiN composition. 목적: Hollow Cathode Discharge방법을 이용한 HCD 이온플레이팅 장비를 제작하였고, 이 장비를 이용하여 stainless steel 위에 TiN 박막을 질소 가스양을 변화하면서 코팅하였으며, 이때 TiN 박막의 미세색상변화를 분석하 였다. 방법: 질소 가스에 대한 TiN박막의 미세색상변화를 광학적으로 관찰하기 위해 분광복사계와 분광광도계를 사 용하였고, 질소 가스에 대한 TiN 박막의 성분 변화를 알기위해 XPS로 분석하였다. 결과: 질소가스 120 sccm의 TiN 박막의 CIE 색좌표는 (0.382, 0.372)로 은색과 금색의 혼합색으로 나타나고 질소 가스양이 증가함에 따라 x, y값 둘 다 조금씩 커져 금색이 점점 진해지는 것을 알 수 있었다. 또한 분광광도계에 의한 TiN 박막의 반사율에 있어서 질 소 가스양이 증가함에 따라 550 nm 파장근처에서의 반사율의 기울기가 대체적으로 점점 커지는 것을 알 수 있었 다. 그리고 XPS를 사용하여 Ti scan 한 결과, TiO2 성분에서 유래된 458 eV의 조그마한 피크는 조금씩 더 들어가 며 TiN 성분에서 유래된 455 eV의 큰 피크는 약간씩 커지는 것을 볼 수 있었다. 결론: 질소 가스양이 120 sccm인 TiN 박막에서는 표면에 있는 TiC 성분과 표면과 내부에 존재하는 TiO2, TiN 성분으로 인해 은색과 금색의 혼합색 으로 나타났으나, 질소 가스양이 증가함에 따라 TiN 성분이 다른 성분에 비해 점점 많아져 금색이 점점 진해진 것 으로 유추할 수 있었다.

철도에서의 동상방지를 위한 모형시험에서 XPS 및 PE골재의 설치 효과

김동관(Donggwan Kim),윤여원(Yeowon Yoon),김영진(Youngchin Kim) 한국지반환경공학회 2014 한국지반환경공학회논문집 Vol.15 No.10

본 연구에서는 철도노반에서의 동결융해로 인한 피해를 줄이고자 뛰어난 단열효과와 강도를 가진 XPS(eXtruded PolyStyrene)와 PE골재(polyethylene aggregates)를 사용하여 동상을 억제하는 방법을 연구하고자 대형동토실에서 모형시험을 수행하였다. 이를 위해 노반과 PE골재의 혼입비율을 변화시켜 건조밀도와 함수비, 온도에 따른 열전도율을 측정하였다. 시험결과 노반에 혼입된 PE골재 비율에 비례하여 단열효과가 증가하였지만, 간극의 함수비와 온도변화에 민감하였다. 또한 철도노반을 모사한 모형시험에서 각 단열재의 두께와 설치순서를 다르게 한 후 단열효과를 비교 결과, XPS의 단열효과가 우수한 것으로 나타났으며 XPS판자가 상부, PE골재가 하부에 설치될 때 그 반대의 경우보다 단열효과가 뛰어난 것으로 나타났다. In this research, in order to study insulation effect of commercial XPS and recycled PE aggregates for prevention of frost heave in the roadbed of railroad track from the freezing temperature, model tests were carried out in the large freezing room. For this, thermal conductivities were measured for various dry densities, water contents, temperatures and mixing ratios of PE aggregates. From the tests, it can be seen that thermal conductivities of roadbed decrease with the increase of the ratio of mixed PE aggregates. However it was sensitive to the changes of temperature and water content due to the amount of water in the voids. From the model test of railroad track, it can be seen that the time to reach 0 ℃ was longer for XPS than that for the PE aggregates. Also the test shows best insulation effect can be achieved when XPS board was installed above the PE aggregate layer rather than the opposite order.

XPS를 이용한 Sb-doped $SnO_2$ 투명전도막의 특성 분석

임태영,김창열,심광보,오근호 한국결정성장학회 2003 한국결정성장학회지 Vol.13 No.5

Sol-gel dip coating법으로 soda lime glass 기판 위에 ATO(antimony-doped tin oxide) 투명전도막을 제조할 때, 기판 위에 형성된 $SiO_2$ barrier 층 및 $N_2$ gas annealing 에 따른 광투과율 및 전기적 특성에 대한 효과를 정량적으로 측정하고, XPS(X-ray photoelectron spectroscopy) 분석을 통해 고찰하였다. $SiO_2$ barrier층을 갖는 glass 기판 위에 코팅된400 nm 두께의 ATO 박막을 질소분위기에서 annealing한 결과, 광 투과율은 84%그리고 전기저항은 약 $5.0\times 10^{-3}\Omega \textrm{cm}$로 측정되었다 XPS 분석결과 이러한 우수한 전기전도성은 $SiO_2$ buffer층이 glass 기판으로부터 Na 이온의 확산을 막아 ATO막 내에 $Na_2SnO_3$ 및 SnO와 같은 2차상 불순물의 형성을 억제하여 막 내부의 Sb의 농도 및 $Sb^{5+}/Sb^{3+}$ 비를 증가시키고, $N_2$ annealing은 $Sb^{5+}$ 도 환원시키지만 $Sn^{4+}$를 환원시키는 효과가 크게 작용하였기 때문으로 사료된다. In the fabrication process of transparent conducting thin films of the ATO (antimony-doped tin oxide) on a soda lime glass substrate by a sol-gel dip coating method, the effects of the $SiO_2$ buffer layer formed on the substrate and $N_2$ annealing treatment were investigated by XPS (X-ray photoelectron spectroscopy) analysis. Optical transmittance and electrical resistivity of the 400 nm-thick ATO thin films which were deposited on $SiO_2$ buffer layer/soda lime glass and then annealed under nitrogen atmosphere were 84 % and $5.0\times 10^{-3}\Omega \textrm{cm}$ respectively. The XPS analysis confirmed that a $SiO_2$ buffer layer inhibited Na ion diffusion from the substrate, resulting in prohibiting the formation of a secondary phase such as $Na_2SnO_3$ and SnO and increasing Sb ion concentration and ratio of $Sb^{5+}/Sb^{3+}$ in the film. And it was also found that $N_2$ annealing treatment leads to the reduction of $Sn^{4+}$as well as $Sb^{5+}$ however the reduction of $Sn^{4+}$ is more effective and therefore consequently results in decrease in the electrical resistivity to produce an excellent electrical properties of the film.

XPS와 AFM에 의한 올리고펩타이드의 자기 집합화 단분자막 분석

송성훈,박진영,김우식,Nakamura, Chikashi,Miyake, Jun,장상목 한국화학공학회 2003 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.41 No.1

금속 기판 위에 유기 박막을 형성하는 방법 중에서 티올기와 Au와의 결합을 이용한 자기집합에 관한 연구가 활발히 진행되고 있다. 포르피린 유도체와 강하게 결합하는 타올기를 가지는 올리고펩타이드 PSP1과 PSP2를 합성하여 MOPS 완층용액에서 금표면에 자기집합화 단분자막(self-assembled monolayer, SAM)을 형성시켜 X-ray photoelection spectroscopy(XPS)와 atomic force microscopy(AFM)을 이용하여 분석하였다. 그 결과 PSP2의 경우와 PSP1의 경우보다 Au표면에서 SAM이 더욱 더 잘 형성되고 있음을 알 수 있었고 MOPS완충용액에 존재하는 황 이온의 영향도 알 수 있었다. 이 결과는 구성단위로부터 이론적으로 계산한 SAM막의 steric energy 값의 차이에서 유추한 결론과 일치하였다. Recently, the self-assembled monolayer(SAM) of thiols on nible metals has been studied intensively. Oligopeptides such as PSP1(Tyr-Ala-Gly-Tyr-Cys) and PSP2(His-Ala-Ser-Cys) with thiol group, which interact strongly with a typical cationic porphyrin derivative, are synthesized. Peptides adsorption from the liquid phase on Au has been studied using X-ray photoelection spectroscopy(XPS) and AFM image. XPS provides further evidence that the primary adsorbate species is bonded to Au through the sulfur atom. By the analysis of XPS spectra and AFM image, it is found that PSP2 is self-assembled better than PSP1 and the sulfur ion MOPS buffer solution has an effect on the self-assembling performance. This result is coincident with the calculation result of steric energies of Au-Peptide bonded SAM structure.

UBM Sputtering System에 의한 안경테용 TiN막 제작에 있어 Oxygen 영향 연구

박문찬,이종근,주경복,이화자,김응순,최광호 한국안광학회 2009 한국안광학회지 Vol.14 No.1

Purpose: TiN films were deposited on sus304 by unbalanced magnetron sputtering system which was designed and developed as unbalancing the strength of the magnets in the magnetron electrode. The effect of oxygen incorporation in the fabrication of deposited films was investigated. Methods: The cross sections of deposited films on Silicon wafer were observed by SEM to measure the thickness of the films, the components of the surface of the films were identified by XPS survey spectra, the compositional depth-profile of deposited films was examined by an XPS apparatus. Results: From the data of XPS depth profile of films, it could be seen that the element O as well as the elements Ti and N present in the surface of the film and the relative percentage of the element O was constant at 65 at.% with respect to the depth of film. Conclusions: The color change with thickness of the films had something to do with the change of Ti 2p3/2 peak intensity and shape mixed of TiO2, TiN, TiOxNy compound. 목적: Magnetron의 세기를 비대칭으로 한 unbalanced magnetron sputtering 장치를 설계· 제작하고, 이 장치를 사 용하여 sus304시편 위에 TiN을 코팅할 때 산소영향을 연구하고자 한다. 방법: 코팅막의 두께를 알기 위해 실리콘 웨이퍼 위의 코팅막을 SEM으로 단면을 관찰하였고, TiN 코팅박막표면의 성분을 분석하기 위하여 XPS를 사용하였 으며, 표면안쪽의 성분을 관찰하기 위해 depth profile을 하였다. 결과: XPS depth profile 데이터로부터 티타늄과 질 소 뿐만 아니라 산소가 일정한 양으로 존재하며, 산소의 양은 약 65at.%의 큰 양이 존재한다는 것을 알 수 있었다. 두께에 따른 색상변화는 세 개의 피크가 모여서 형성이 된 Ti 2p3/2 피크의 모양이 두께에 따라 약간 다르다는 것을 알 수 있었다. 결론: 코팅 중에 산소가 섞여 순수한 TiN보다는 TiO2, TiN, TiOxNy 세가지 조합에 의해 색이 결정되 는 것을 알 수 있었다.

졸-겔법으로 성장한 Mg<SUB>x</SUB>Zn<SUB>1−x</SUB>O:In 박막의 전구체 농도에 따른 물성 연구

최효진(Hyo Jin Choi),이민상(Min Sang Lee),김홍승(Hong Seung Kim),안형수(Hyung Soo Ahn),장낙원(Nak Won Jang) 한국물리학회 2022 새물리 Vol.72 No.6

본 논문에서는 졸-겔법에 의해 사파이어 기판에 성장된 MgZnO:In 박막의 In과 Mg 전구체의 농도에 따른 물성 변화를 연구하였다. 성장된 박막의 특성은 XRD, UV-vis, Hall effect, XPS를 이용하여 분석하였다. XRD 분석 결과에 따르면 시료는 모두 c-축 우선 배향성을 보였고, UV-vis 분석 결과 시료의 가시광 영역 투과율이 대체로 80% 이상인 것을 확인하였다. Hall 효과 측정을 통해 In이 많이 첨가될수록 비저항이 감소하는 것을 확인할 수 있었다. XPS 분석에 따르면 In을 5mol% 이상 첨가하면 Mg 함량이 감소하는 것으로 나타났다. O 1s 결합 에너지 역시 XPS로 조사하였고, O<SUB>I</SUB>/O<SUB>II</SUB> 비율을 비교하여 박막의 결합 상태를 관찰하였다. In을 5 mol% 이상 첨가했을 때는 In이 Mg의 산소 공공 합성을 방해하여 O<SUB>I</SUB>/O<SUB>II </SUB>비율이 감소함을 확인하였다. In this paper, changes in physical properties of MgZnO:In thin films grown on a sapphire substrate using the sol-gel method were investigated as per the concentrations of In and Mg precursors. The properties of the grown thin films were analyzed using XRD, UV-Vis, Hall effect, and XPS. According to the XRD results, all samples showed the c-axis preferential orientation growth. UV-Vis analysis confirmed that the samples exhibited a transmittance of >80% in the visible region. Through the Hall effect measurement, the resistance was found to decrease with the increasing In amount. According to the XPS analysis, when >5 mol% of In was added, the Mg content decreased. The O 1s binding energy was also investigated using XPS, and the bonding state of the thin film was observed by comparing the O<SUB>I</SUB>/O<SUB>II</SUB> ratio. When >5 mol% of In was added, it interfered with the generation of oxygen vacancy during the synthesis of Mg, thus decreasing the O<SUB>I</SUB>/O<SUB>II</SUB> ratio.<br/>

XPS 분석을 통한 CrMoN 코팅의 마찰마모 거동 연구

양영환 ( Young Hwan Yang ),여인웅 ( In Woong Lyo ),박상진 ( Sang Jin Park ),임대순 ( Dea Soon Lim ),오윤석 ( Yoon Suk Oh ) 대한금속재료학회 ( 구 대한금속학회 ) 2012 대한금속·재료학회지 Vol.50 No.8

The tribological behavior of CrMoN films with respect to surface chemistry was investigated by using X-ray photoelectron spectroscopy (XPS). All of the films were prepared from a hybrid PVD system consisting of DC unbalanced magnetron (UBM) sputtering and arc ion plating (AIP) sources. The tribological property of the films was evaluated by a friction coefficient using a Ball-on-disk type tribometer. The chemistry of wear track was analyzed by energy dispersive spectroscopy (EDS) and XPS. The friction coefficient was measured to be 0.4 for the CrMoN film, which is lower than that of a monolithic CrN film. EDS and XPS results imply the formation of an oxide layer on the coating surface, which was identified as molybdenum oxide phases, known to be a solid lubricant during the wear test.

Quantitative analysis of Si_1-xGe_x alloy films by SIMS and XPS depth profiling using a reference material

Oh, Won Jin,Jang, Jong Shik,Lee, Youn Seoung,Kim, Ansoon,Kim, Kyung Joong Elsevier 2018 APPLIED SURFACE SCIENCE - Vol.432 No.2

<P><B>Abstract</B></P> <P>Quantitative analysis methods of multi-element alloy films were compared. The atomic fractions of Si<SUB>1-x</SUB>Ge<SUB>x</SUB> alloy films were measured by depth profiling analysis with secondary ion mass spectrometry (SIMS) and X-ray Photoelectron Spectroscopy (XPS). Intensity-to-composition conversion factor (ICF) was used as a mean to convert the intensities to compositions instead of the relative sensitivity factors. The ICFs were determined from a reference Si<SUB>1-x</SUB>Ge<SUB>x</SUB> alloy film by the conventional method, average intensity (AI) method and total number counting (TNC) method. In the case of SIMS, although the atomic fractions measured by oxygen ion beams were not quantitative due to severe matrix effect, the results by cesium ion beam were very quantitative. The quantitative analysis results by SIMS using MCs<SUB>2</SUB> <SUP>+</SUP> ions are comparable to the results by XPS. In the case of XPS, the measurement uncertainty was highly improved by the AI method and TNC method.</P> <P><B>Highlights</B></P> <P> <UL> <LI> Quantitative analysis methods of multi-element alloy films were investigated. </LI> <LI> The RSFs were determined from a reference alloy film by the conventional method, average intensity method and total number counting method. </LI> <LI> In XPS analysis, the measurement uncertainty was highly improved by the AI method and TNC method. </LI> </UL> </P>