Polymer/drug films as a model system for a drug eluting coronary stent coating layer

Size: px
Start display at page:

Download "Polymer/drug films as a model system for a drug eluting coronary stent coating layer"

Transcription

1 Polymer/drug films as a model system for a drug eluting coronary stent coating layer Valeria Ciarnelli Prof. Clive Roberts Prof. Morgan Alexander, Prof. Martyn Davies School of Pharmacy The University of Nottingham 14 September 212 PharmSci_APS

2 Introduction: what is a coronary stent? The coronary artery stent is a tubular device, in the form of a coil or mesh, that is inserted at the site of arterial obstruction via a catheter. This device widens the coronary artery improving blood flow to the ischemic heart muscle. 2 types: Bare metal stent (BMS) Drug eluting stent (DES) A Obstruction: plaque. The stent is placed via catheter B Balloon inflated The artery is expanded C Scaffolding action The blood flow is re-established

3 Targets Drug eluting stent + Drug/Polymer coating layer Characterization of films as models for drug eluting coronary stent coating layer Characterization of the actual drug eluting coronary stent coating layer This work is a part of analytical support to develop a medical device Optimization of manufactoring process

4 Methods. Spun cast film preparation and equipments used Spin casting Spray coating AFM (XPS) 3 (ToF-SIMS) Spun cast or spray coated film Sample ID Casting Procedure Drying Step Series 1* Spun cast Room condition Series 2* Spun cast Bake in oven (5 C for 45 min) Series 3* Spray coated Warm air (5 C for 15 sec each 2 nd spray cycle) Series 4* Spun cast in argon atmosphere Bake in oven (5 C for 45 min under vacuum) *The films were made from solutions at different drug polymer weigh ratio precisely at 1:3; 1:1 and 3:1. Pure polymer and drug films were also made as references models.

5 Methods. Atomic Force Microscopy (AFM) A) Ball and stick model of pentacene B) STM images, C) and D) NC-AFM image of pentacene A B 1.3 Å C 5 Å 5 Å -2 Hz D Å + 1 Hz 5 Å 2 Å -7 Hz Leo Gross et al, Science, 29 Leo Gross et al, Science, 29, 324, Hz

6 Methods. Time of flight Secondary Ion Mass Spectroscopy (ToF-SIMS) Analysis Ion Beam Sputter Ion Beam 1 µm 3 µm y x Intensity Depth z Anna Belu et al. Chemical imaging of drug eluting coatings: Combining surface analysis and confocal Raman microscopy

7 Methods. X-Ray Photo-electron Spectroscopy (XPS) Photoemission peak Photo emission X-rays Inelastic scattering tail Free electron X-Ray Valence electrons ev Core electrons Nucleus X-Ray Coronene Molecule (C 24 H 12 )

8 Results. AFM characterization. Series 1 and 2 Series 1. Spun cast film without heating step. Tapping mode. 22nm Phase 63 15nm Phase nm Phase 6 2 µm Increasing drug loading :3 d:p wr 1: 1 d:p wr 3: 1 d:p wr Film at 1:3 wr shows circular pit features (diameter approximately 1-25). Clear evidence of phase separation Film at 3:1 drug polymer weight ratio shows globular surface features - 9 Series 2. Spun cast film with heating step (5 C for 45 min). QNM mode. 33nm DMT modulus 25 MPa DMT modulus DMT modulus MPa 145 nm 3 GPa c 2 µm MPa 1:3 d:p wr 1: 1 d:p wr 3: 1 d:p wr Film at 1:1 shows network structure surrounding deeper areas, globular features with a diameter of approximately 1 MPa GPa

9 Results. AFM characterization. Series 2 and 3 Series 3. Spray coated film on silicon wafer with heating step. (QNM mode) 167 nm DMT modulus 5.8 GPa 551 nm DMT modulus 2.6 GPa 216 nm DMT modulus 1 GPa 2.4 GPa GPa 1:3 d:p wr 1: 1 d:p wr 3: 1 d:p wr 75 MPa Increasing drug loading Presence of globular features (diameter 1) showing mechanical heterogeneity Features organized in globular domains also observed in the spun cast films. These features occur at a higher incidence with increasing drug concentration Series 4. Spun cast film on silicon prepared in argon atmosphere with heating step (5 C for 45 min) under vacuum. ( tapping mode RH = 5%) 2nm Phase 12 8 nm Phase nm Phase -15 2µm :3 d:p wr 1: 1 d:p wr 3: 1 d:p wr Different morphology although still presence of globular domains with diameter ranging from 1 to 35-21

10 Results. ToF-SIMS characterization. Depth profiling of spun cast films series 1 Series 1. Spun cast film on silicon wafer 1:3 d:p weight ratio 1:1 d:p weight ratio 3:1 d:p weight ratio Film at 1:3 drug polymer weight ratio without heating step Bulk Polymer PLA Interface Drug Everolimus Silicon x Film at 1:1 drug polymer weight ratio without heating step Polymer PLA Drug Everolimus Silicon x Film at 3:1 drug polymer weight ratio without heating step Polymer PLA Drug Everolimus Silicon x Surface Depht (nm) Depht (nm) Polymer Drug Silicon x n (n= 5,1 and 5 for 1:3, 1:1 and 3:1 respectively) This indicates that the drug migrates to the surface and to an extent at the substrate interface leaving the polymer relatively concentrated in the bulk. Overall relative ion peak intensities for drug and polymer markers are consistent with the respective concentration Sample ID Thickness (nm) Sputter time Sputter rate (sec) (nm/sec) 1:3 d:p wr :1 d:p wr :1 d:p wr Depht (nm)

11 Results. ToF-SIMS characterization. Depth profiling of spun cast films series 2 Series 2. Spun cast film on glass slide. The films underwent a drying step in the oven at 5 C for 45 min 1:3 d:p weight ratio 1:1 d:p weight ratio 3:1 d:p weight ratio Intensity Counts (ion (ions) count) Film at 1:3 drug polymer weight ratio with heating step Silicon Polymer PLA Drug Everolimus Count (ions) Film at 1:1 drug polymer weight ratio with heating step Silicon Polymer PLA Drug Everolimus Intensity Counts (ion (ions) count) Film at 3:1 drug polymer weight ratio with heating step Silicon Polymer PLA Drug Everolimus Polymer Drug Silicon The polymer is concentrated in the bulk region of the film The drug migrates to the surface forming a surface-enriched drug region for all the films at different loadings Polymer Drug 1:1 d:p wr

12 Results. ToF-SIMS characterization. Depth profiling of spun cast films series 3 Series 3. Spray coated film on silicon. The films underwent a drying step (warm air 5 C) 1:3 d:p weight ratio 1:1 d:p weight ratio 7 Spray coated film at 1:3 drug polymer wr Spray coated film at 1:1drug polymer wr Silicon 1 Polymer Drug Silicon Polymer 4 Drug Silicon x Drug Polymer Polymer The drug surface enrichment is less pronounced than the one observed for the spun cast films 1:1 d:p wr Polymer 25 Drug Spray coated film at 3:1 drug polymer wr :1 d:p weight ratio Drug Silicon 2 3 4

13 Results. XPS characterization. Surface analysis of spun cast films series 2 and spray coated films series 3 XPS spectra of drug powder XPS spectra of polymer powder x 1 2 x O 1s C 1s 25 O 1s CPS 4 CPS C 1s 2 N 1s Bi ndi ng E nergy (ev) Bi ndi ng E nergy (ev) C S( hi i b di d i C S / i ) Spun cast films (series 2) Spray coated films (series 3) Spun cast films (series 4) Drug/polymer wr (Drug loading) 1:3 (25%) 1:1 (5%) 3:1 (75%) 1:3 (25%) 1:1 (5%) 3:1 (75%) 1:3 (25%) 1:1 (5%) 3:1 (75%) N % (theoretical) N % (experimental) ± SD 1.3 ± ± ±.1.4 ±.4 1. ± ± ± ± ±.3 Experimental Drug % (w/w) ± SD 85.4 ± ± ± ± ± ± ± ± ± 1.7 Drug enrichment Less pronounced drug enrichment

14 Results. XPS characterization. Depth profiling of spun cast films: series 4 Series 4. Spun cast film on silicon. 5ºC for 45 min, Ar atmosphere and controlled humidity 1:3 d:p weight ratio 1:1 d:p weight ratio 3:1 d:p weight ratio C1s, O1s & Si2p % N1s % C1s, O1s & Si2p % N1s % C1s, O1s & Si2p % Etching time (sec) N1s % C 1s O 1s N 1s Si 2p Drug enrichment at the surface and interface (film/silicon). The same is observed for the other drug polymer concentrations. The drug profiles obtained from XPS and ToF-SIMS depth profiling are consistent.

15 Conclusions We are able to characterize this particular drug polymer coating layer using complementary surface analysis techniques. AFM shows the presence of globular features (diameter 1-15) occurring at higher incidence with increased drug loading ToF-SIMS depth profiling on the model films showed the drug and polymer distribution as a function of depth, with the drug preferentially located at the surface The XPS analysis confirmed the existence of an enrichment of drug on the surface of the model films (series 2 and 3) at higher percentage compared to the bulk drug loading. In the case of the spray coated films the drug at the surface increased with the drug loading The drug enrichment is more pronounced in the spun cast films than the spray coated films. We have gained an understanding of the distribution of the drug

16 Acknowledgements Supervisors Thanks to: Prof Clive J Roberts Prof Morgan R Alexander Prof Martyn C Davies Prof Chen Xinyong Dr David J Scurr Mrs Emily Smith From Kratos Analytical Chris Blomfield Simon Hutton THANKS FOR LISTENING

17 Results. ToF-SIMS Depth profiling of spun cast films: series 4 Series 4. Spun cast film on silicon wafer. Silicon substrate, 5 ºC for 45 min, Ar atmosphere and controlled humidity 1:3 d:p weight ratio 1:1 d:p weight ratio 3:1 d:p weight ratio Silicon Polymer Drug Silicon Polymer Drug Silicon Polymer Drug The drug migrates to both the surface and the interface (film/silicon) The polymer is concentrated in the bulk region. Relative ion peak intensities for drug and polymer markers are consistent with the respective concentration Sample ID Thickness (nm) Sputter time Sputter rate (sec) (nm/sec) 1:3 d:p wr :1 d:p wr :1 d:p wr

18 Results. AFM characterization Globular features Peak force QNM mode Series 3. 1:1 drug polymer wr Series 2. 1:1 drug polymer wr Deformation a 185 nm DMT modulus 3.5 GPa 1 a Diameters: 1 2 x 2 µm 1µm 1.5 x 1.5 µm 1 23 MPa b b 2 x 2 µm Diameters: 2 Series 3. 1:3 drug polymer wr 216 nm 1µm 1 GPa 1.5 x 1.5 µm Series 2. 2 areas of spun cast film at 1:1 drug polymer weight ratio. Globular features with a diameters of approximately 1-2 can be observed. Their formations is probably due to the dry step at 5 C for 45 min. 2 DMT modulus 75 MPa 2 Series 3. Granular structure of the domain. The size of the globular structure varies between 1 and 2 nm.

Applications of XPS, AES, and TOF-SIMS

Applications of XPS, AES, and TOF-SIMS Applications of XPS, AES, and TOF-SIMS Scott R. Bryan Physical Electronics 1 Materials Characterization Techniques Microscopy Optical Microscope SEM TEM STM SPM AFM Spectroscopy Energy Dispersive X-ray

More information

ToF-SIMS or XPS? Xinqi Chen Keck-II

ToF-SIMS or XPS? Xinqi Chen Keck-II ToF-SIMS or XPS? Xinqi Chen Keck-II 1 Time of Flight Secondary Ion Mass Spectrometry (ToF-SIMS) Not ToF MS (laser, solution) X-ray Photoelectron Spectroscopy (XPS) 2 3 Modes of SIMS 4 Secondary Ion Sputtering

More information

Surface and Interface Characterization of Polymer Films

Surface and Interface Characterization of Polymer Films Surface and Interface Characterization of Polymer Films Jeff Shallenberger, Evans Analytical Group 104 Windsor Center Dr., East Windsor NJ Copyright 2013 Evans Analytical Group Outline Introduction to

More information

S. Ichikawa*, R. Kuze, T. Shimizu and H. Shimaoka INTRODUCTION

S. Ichikawa*, R. Kuze, T. Shimizu and H. Shimaoka INTRODUCTION Journal of Surface Analysis,Vol.12 No.2 (2005); S.Ichikawa, et al., Coverage Estimation of Silane. Coverage Estimation of Silane Functionalized Perfluoropolyether Layer by using Time of Flight Secondary

More information

Paper presentation. M S Bootha Raju Date: 28/11/09

Paper presentation. M S Bootha Raju Date: 28/11/09 Paper presentation M S Bootha Raju Date: 28/11/09 Photoemission Spectroscopy and Atomic Force Microscopy Investigation of Vapor-Phase Codeposited Silver/Poly(3-hexylthiophene) Composites L. Scudiero, Haoyan

More information

PHI Model 06-C60 Sputter Ion Gun

PHI Model 06-C60 Sputter Ion Gun PHI Model 6-C6 Sputter Ion Gun Introduction: Physical Electronics introduced the model 6-C6 C 6 sputter ion gun and its unique capabilities for surface cleaning and depth profiling of soft materials (figure

More information

Introduction to X-ray Photoelectron Spectroscopy (XPS) XPS which makes use of the photoelectric effect, was developed in the mid-1960

Introduction to X-ray Photoelectron Spectroscopy (XPS) XPS which makes use of the photoelectric effect, was developed in the mid-1960 Introduction to X-ray Photoelectron Spectroscopy (XPS) X-ray Photoelectron Spectroscopy (XPS), also known as Electron Spectroscopy for Chemical Analysis (ESCA) is a widely used technique to investigate

More information

X-Ray Photoelectron Spectroscopy (XPS) Prof. Paul K. Chu

X-Ray Photoelectron Spectroscopy (XPS) Prof. Paul K. Chu X-Ray Photoelectron Spectroscopy (XPS) Prof. Paul K. Chu X-ray Photoelectron Spectroscopy Introduction Qualitative analysis Quantitative analysis Charging compensation Small area analysis and XPS imaging

More information

Interfacial Chemistry and Adhesion Phenomena: How to Analyse and How to Optimise

Interfacial Chemistry and Adhesion Phenomena: How to Analyse and How to Optimise Interfacial Chemistry and Adhesion Phenomena: How to Analyse and How to Optimise John F Watts Department of Mechanical Engineering Sciences The Role of Surface Analysis in Adhesion Studies Assessing surface

More information

MS482 Materials Characterization ( 재료분석 ) Lecture Note 12: Summary. Byungha Shin Dept. of MSE, KAIST

MS482 Materials Characterization ( 재료분석 ) Lecture Note 12: Summary. Byungha Shin Dept. of MSE, KAIST 2015 Fall Semester MS482 Materials Characterization ( 재료분석 ) Lecture Note 12: Summary Byungha Shin Dept. of MSE, KAIST 1 Course Information Syllabus 1. Overview of various characterization techniques (1

More information

Secondary Ion Mass Spectrometry (SIMS)

Secondary Ion Mass Spectrometry (SIMS) CHEM53200: Lecture 10 Secondary Ion Mass Spectrometry (SIMS) Major reference: Surface Analysis Edited by J. C. Vickerman (1997). 1 Primary particles may be: Secondary particles can be e s, neutral species

More information

PLASMA-POLYMER MODIFICATION OF BASAL PLANE GRAPHITE SURFACES FOR IMPROVED BIOCOMPATIBILITY

PLASMA-POLYMER MODIFICATION OF BASAL PLANE GRAPHITE SURFACES FOR IMPROVED BIOCOMPATIBILITY PLASMA-POLYMER MODIFICATION OF BASAL PLANE GRAPHITE SURFACES FOR IMPROVED BIOCOMPATIBILITY Anca Orăşanu, Marcus R. Davidson, Robert H. Bradley Advanced Materials & Biomaterials Research Centre, School

More information

Lecture 11 Surface Characterization of Biomaterials in Vacuum

Lecture 11 Surface Characterization of Biomaterials in Vacuum 1 Lecture 11 Surface Characterization of Biomaterials in Vacuum The structure and chemistry of a biomaterial surface greatly dictates the degree of biocompatibility of an implant. Surface characterization

More information

EE 527 MICROFABRICATION. Lecture 5 Tai-Chang Chen University of Washington

EE 527 MICROFABRICATION. Lecture 5 Tai-Chang Chen University of Washington EE 527 MICROFABRICATION Lecture 5 Tai-Chang Chen University of Washington MICROSCOPY AND VISUALIZATION Electron microscope, transmission electron microscope Resolution: atomic imaging Use: lattice spacing.

More information

Electronic Supplementary Information. Molecular Antenna Tailored Organic Thin-film Transistor for. Sensing Application

Electronic Supplementary Information. Molecular Antenna Tailored Organic Thin-film Transistor for. Sensing Application Electronic Supplementary Material (ESI) for Materials Horizons. This journal is The Royal Society of Chemistry 2017 Electronic Supplementary Information Molecular Antenna Tailored Organic Thin-film Transistor

More information

Application of Surface Analysis for Root Cause Failure Analysis

Application of Surface Analysis for Root Cause Failure Analysis Application of Surface Analysis for Root Cause Failure Analysis David A. Cole Evans Analytical Group East Windsor, NJ Specialists in Materials Characterization Outline Introduction X-Ray Photoelectron

More information

1 Introduction COPYRIGHTED MATERIAL. 1.1 HowdoweDefinetheSurface?

1 Introduction COPYRIGHTED MATERIAL. 1.1 HowdoweDefinetheSurface? 1 Introduction JOHN C. VICKERMAN Manchester Interdisciplinary Biocentre, School of Chemical Engineering and Analytical Science, The University of Manchester, Manchester, UK The surface behaviour of materials

More information

SUPPLEMENTARY INFORMATION

SUPPLEMENTARY INFORMATION SUPPLEMENTARY INFORMATION Facile Synthesis of High Quality Graphene Nanoribbons Liying Jiao, Xinran Wang, Georgi Diankov, Hailiang Wang & Hongjie Dai* Supplementary Information 1. Photograph of graphene

More information

Lecture 22 Ion Beam Techniques

Lecture 22 Ion Beam Techniques Lecture 22 Ion Beam Techniques Schroder: Chapter 11.3 1/44 Announcements Homework 6/6: Will be online on later today. Due Wednesday June 6th at 10:00am. I will return it at the final exam (14 th June).

More information

Secondaryionmassspectrometry

Secondaryionmassspectrometry Secondaryionmassspectrometry (SIMS) 1 Incident Ion Techniques for Surface Composition Analysis Mass spectrometric technique 1. Ionization -Electron ionization (EI) -Chemical ionization (CI) -Field ionization

More information

Electrochemical Deposition of Iron Nanoparticles on PPY and H terminated Si substrates. Karan Sukhija Co-op Term # 1 April 28 th, 2005

Electrochemical Deposition of Iron Nanoparticles on PPY and H terminated Si substrates. Karan Sukhija Co-op Term # 1 April 28 th, 2005 Electrochemical Deposition of Iron Nanoparticles on PPY and H terminated Si substrates Karan Sukhija Co-op Term # 1 April 28 th, 2005 Future Suggested Experiments Acknowledgments Presentation Outline Background

More information

IV. Surface analysis for chemical state, chemical composition

IV. Surface analysis for chemical state, chemical composition IV. Surface analysis for chemical state, chemical composition Probe beam Detect XPS Photon (X-ray) Photoelectron(core level electron) UPS Photon (UV) Photoelectron(valence level electron) AES electron

More information

XPS & Scanning Auger Principles & Examples

XPS & Scanning Auger Principles & Examples XPS & Scanning Auger Principles & Examples Shared Research Facilities Lunch Talk Contact info: dhu Pujari & Han Zuilhof Lab of rganic Chemistry Wageningen University E-mail: dharam.pujari@wur.nl Han.Zuilhof@wur.nl

More information

MICROCHIP MANUFACTURING by S. Wolf

MICROCHIP MANUFACTURING by S. Wolf by S. Wolf Chapter 15 ALUMINUM THIN-FILMS and SPUTTER-DEPOSITION 2004 by LATTICE PRESS CHAPTER 15 - CONTENTS Aluminum Thin-Films Sputter-Deposition Process Steps Physics of Sputter-Deposition Magnetron-Sputtering

More information

Auger Electron Spectroscopy

Auger Electron Spectroscopy Auger Electron Spectroscopy Auger Electron Spectroscopy is an analytical technique that provides compositional information on the top few monolayers of material. Detect all elements above He Detection

More information

Supplementary Figure 1 Detailed illustration on the fabrication process of templatestripped

Supplementary Figure 1 Detailed illustration on the fabrication process of templatestripped Supplementary Figure 1 Detailed illustration on the fabrication process of templatestripped gold substrate. (a) Spin coating of hydrogen silsesquioxane (HSQ) resist onto the silicon substrate with a thickness

More information

MSE 321 Structural Characterization

MSE 321 Structural Characterization Auger Spectroscopy Auger Electron Spectroscopy (AES) Scanning Auger Microscopy (SAM) Incident Electron Ejected Electron Auger Electron Initial State Intermediate State Final State Physical Electronics

More information

The design of an integrated XPS/Raman spectroscopy instrument for co-incident analysis

The design of an integrated XPS/Raman spectroscopy instrument for co-incident analysis The design of an integrated XPS/Raman spectroscopy instrument for co-incident analysis Tim Nunney The world leader in serving science 2 XPS Surface Analysis XPS +... UV Photoelectron Spectroscopy UPS He(I)

More information

Supplementary Information for. Silver Nanoparticles Embedded Anti-microbial Paints Based on Vegetable Oil

Supplementary Information for. Silver Nanoparticles Embedded Anti-microbial Paints Based on Vegetable Oil Supplementary Information for Silver Nanoparticles Embedded Anti-microbial Paints Based on Vegetable Oil Ashavani Kumar #, Praveen Kumar Vemula #, Pulickel M. Ajayan, George John * Department of Chemistry,

More information

raw materials C V Mn Mg S Al Ca Ti Cr Si G H Nb Na Zn Ni K Co A B C D E F

raw materials C V Mn Mg S Al Ca Ti Cr Si G H Nb Na Zn Ni K Co A B C D E F Today s advanced batteries require a range of specialized analytical tools to better understand the electrochemical processes that occur during battery cycling. Evans Analytical Group (EAG) offers a wide-range

More information

Segregated chemistry and structure on (001) and (100) surfaces of

Segregated chemistry and structure on (001) and (100) surfaces of Supporting Information Segregated chemistry and structure on (001) and (100) surfaces of (La 1-x Sr x ) 2 CoO 4 override the crystal anisotropy in oxygen exchange kinetics Yan Chen a, Helena Téllez b,c,

More information

A Sustainable Synthesis of Nitrogen-Doped Carbon Aerogels

A Sustainable Synthesis of Nitrogen-Doped Carbon Aerogels A Sustainable Synthesis of Nitrogen-Doped Carbon Aerogels Supporting Information By Robin J. White, a, * Noriko Yoshizawa, b Markus Antonietti, a and Maria-Magdalena Titirici. a * e-mail: robin.white@mpikg.mpg.de

More information

Auger Electron Spectroscopy Overview

Auger Electron Spectroscopy Overview Auger Electron Spectroscopy Overview Also known as: AES, Auger, SAM 1 Auger Electron Spectroscopy E KLL = E K - E L - E L AES Spectra of Cu EdN(E)/dE Auger Electron E N(E) x 5 E KLL Cu MNN Cu LMM E f E

More information

Surface Analysis - The Principal Techniques

Surface Analysis - The Principal Techniques Surface Analysis - The Principal Techniques 2nd Edition Editors johnc.vickerman Manchester Interdisciplinary Biocentre, University of Manchester, UK IAN S. GILMORE National Physical Laboratory, Teddington,

More information

Methods of surface analysis

Methods of surface analysis Methods of surface analysis Nanomaterials characterisation I RNDr. Věra Vodičková, PhD. Surface of solid matter: last monoatomic layer + absorbed monolayer physical properties are effected (crystal lattice

More information

PHI 5000 Versaprobe-II Focus X-ray Photo-electron Spectroscopy

PHI 5000 Versaprobe-II Focus X-ray Photo-electron Spectroscopy PHI 5000 Versaprobe-II Focus X-ray Photo-electron Spectroscopy The very basic theory of XPS XPS theroy Surface Analysis Ultra High Vacuum (UHV) XPS Theory XPS = X-ray Photo-electron Spectroscopy X-ray

More information

ECE Semiconductor Device and Material Characterization

ECE Semiconductor Device and Material Characterization ECE 4813 Semiconductor Device and Material Characterization Dr. Alan Doolittle School of Electrical and Computer Engineering Georgia Institute of Technology As with all of these lecture slides, I am indebted

More information

Surface Analysis - The Principal Techniques

Surface Analysis - The Principal Techniques Surface Analysis - The Principal Techniques Edited by John C. Vickerman Surface Analysis Research Centre, Department of Chemistry UMIST, Manchester, UK JOHN WILEY & SONS Chichester New York Weinheim Brisbane

More information

Nanoscale Chemical Characterization: Moving to 3 Dimensions

Nanoscale Chemical Characterization: Moving to 3 Dimensions Nanoscale Chemical Characterization: Moving to 3 Dimensions Eric B. Steel Chemical Science & Technology Laboratory National Institute of Standards & Technology Outline What is and why do we need chemical

More information

MS482 Materials Characterization ( 재료분석 ) Lecture Note 4: XRF

MS482 Materials Characterization ( 재료분석 ) Lecture Note 4: XRF 2016 Fall Semester MS482 Materials Characterization ( 재료분석 ) Lecture Note 4: XRF Byungha Shin Dept. of MSE, KAIST 1 Course Information Syllabus 1. Overview of various characterization techniques (1 lecture)

More information

Characterization of Secondary Emission Materials for Micro-Channel Plates. S. Jokela, I. Veryovkin, A. Zinovev

Characterization of Secondary Emission Materials for Micro-Channel Plates. S. Jokela, I. Veryovkin, A. Zinovev Characterization of Secondary Emission Materials for Micro-Channel Plates S. Jokela, I. Veryovkin, A. Zinovev Secondary Electron Yield Testing Technique We have incorporated XPS, UPS, Ar-ion sputtering,

More information

Imaging Methods: Scanning Force Microscopy (SFM / AFM)

Imaging Methods: Scanning Force Microscopy (SFM / AFM) Imaging Methods: Scanning Force Microscopy (SFM / AFM) The atomic force microscope (AFM) probes the surface of a sample with a sharp tip, a couple of microns long and often less than 100 Å in diameter.

More information

Correlative Raman Imaging of Polymeric Materials

Correlative Raman Imaging of Polymeric Materials APPLICATION NOTE Correlative Raman Imaging of Polymeric Materials WITec GmbH, Lise-Meitner-Str. 6, 89081 Ulm, Germany phone+49 (0) 731 140 700, fax +49 (0) 731 140 70 200 info@witec.de, www.witec.de Characterization

More information

Reduced preferential sputtering of TiO 2 (and Ta 2 O 5 ) thin films through argon cluster ion bombardment.

Reduced preferential sputtering of TiO 2 (and Ta 2 O 5 ) thin films through argon cluster ion bombardment. NATIOMEM Reduced preferential sputtering of TiO 2 (and Ta 2 O 5 ) thin films through argon cluster ion bombardment. R. Grilli *, P. Mack, M.A. Baker * * University of Surrey, UK ThermoFisher Scientific

More information

Supporting Online Material for

Supporting Online Material for www.sciencemag.org/cgi/content/full/321/5894/1331/dc1 Supporting Online Material for Identification of Active Gold Nanoclusters on Iron Oxide Supports for CO Oxidation Andrew A. Herzing, Christopher J.

More information

Solutions for Assignment-6

Solutions for Assignment-6 Solutions for Assignment-6 Q1. What is the aim of thin film deposition? [1] (a) To maintain surface uniformity (b) To reduce the amount (or mass) of light absorbing materials (c) To decrease the weight

More information

Technical description of photoelectron spectrometer Escalab 250Xi

Technical description of photoelectron spectrometer Escalab 250Xi Technical description of photoelectron spectrometer Escalab 250Xi Resource center Physical Methods of Surface Investigations 2014 Table of contents Common description 3 Analytical chamber 8 Preparation

More information

Analysis of Poly(dimethylsiloxane) on Solid Surfaces Using Silver Deposition/TOF-SIMS

Analysis of Poly(dimethylsiloxane) on Solid Surfaces Using Silver Deposition/TOF-SIMS Special Issue Surface and Micro-Analysis of Organic Materials 21 Research Report Analysis of Poly(dimethylsiloxane) on Solid Surfaces Using Silver Deposition/TOF-SIMS Masae Inoue, Atsushi Murase Abstract

More information

MS482 Materials Characterization ( 재료분석 ) Lecture Note 5: RBS

MS482 Materials Characterization ( 재료분석 ) Lecture Note 5: RBS 2016 Fall Semester MS482 Materials Characterization ( 재료분석 ) Lecture Note 5: RBS Byungha Shin Dept. of MSE, KAIST 1 Course Information Syllabus 1. Overview of various characterization techniques (1 lecture)

More information

Biomaterial Scaffolds

Biomaterial Scaffolds Biomaterial Scaffolds Biomaterial Properties Surface properties Bulk properties Biological properties Types of Biomaterials Biological materials Synthetic materials Surface Properties The body reads the

More information

Electronic Supplementary Information

Electronic Supplementary Information Electronic Supplementary Information High Electrocatalytic Activity of Self-standing Hollow NiCo 2 S 4 Single Crystalline Nanorod Arrays towards Sulfide Redox Shuttles in Quantum Dot-sensitized Solar Cells

More information

EE 527 MICROFABRICATION. Lecture 25 Tai-Chang Chen University of Washington

EE 527 MICROFABRICATION. Lecture 25 Tai-Chang Chen University of Washington EE 527 MICROFABRICATION Lecture 25 Tai-Chang Chen University of Washington ION MILLING SYSTEM Kaufmann source Use e-beam to strike plasma A magnetic field applied to increase ion density Drawback Low etch

More information

Electronic Supplementary Information. inverted organic solar cells, towards mass production

Electronic Supplementary Information. inverted organic solar cells, towards mass production Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A. This journal is The Royal Society of Chemistry 2018 Electronic Supplementary Information Polyelectrolyte interlayers with a

More information

5) Surface photoelectron spectroscopy. For MChem, Spring, Dr. Qiao Chen (room 3R506) University of Sussex.

5) Surface photoelectron spectroscopy. For MChem, Spring, Dr. Qiao Chen (room 3R506) University of Sussex. For MChem, Spring, 2009 5) Surface photoelectron spectroscopy Dr. Qiao Chen (room 3R506) http://www.sussex.ac.uk/users/qc25/ University of Sussex Today s topics 1. Element analysis with XPS Binding energy,

More information

Fig. S1 The Structure of RuCE(Left) and RuCA (Right)

Fig. S1 The Structure of RuCE(Left) and RuCA (Right) Supporting information Fabrication of CZTS and CZTSSe photocathode CZTS photocathode was fabricated by sulfurization of a stacked film containing Cu, Zn and Sn. The stacked film was fabricated on Mo coated

More information

Film Characterization Tutorial G.J. Mankey, 01/23/04. Center for Materials for Information Technology an NSF Materials Science and Engineering Center

Film Characterization Tutorial G.J. Mankey, 01/23/04. Center for Materials for Information Technology an NSF Materials Science and Engineering Center Film Characterization Tutorial G.J. Mankey, 01/23/04 Theory vs. Experiment A theory is something nobody believes, except the person who made it. An experiment is something everybody believes, except the

More information

Secondary ion mass spectrometry (SIMS)

Secondary ion mass spectrometry (SIMS) Secondary ion mass spectrometry (SIMS) ELEC-L3211 Postgraduate Course in Micro and Nanosciences Department of Micro and Nanosciences Personal motivation and experience on SIMS Offers the possibility to

More information

The Controlled Evolution of a Polymer Single Crystal

The Controlled Evolution of a Polymer Single Crystal Supporting Online Material The Controlled Evolution of a Polymer Single Crystal Xiaogang Liu, 1 Yi Zhang, 1 Dipak K. Goswami, 2 John S. Okasinski, 2 Khalid Salaita, 1 Peng Sun, 1 Michael J. Bedzyk, 2 Chad

More information

Supporting Information

Supporting Information Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A. This journal is The Royal Society of Chemistry 2018 Supporting Information A minimal non-radiative recombination loss for efficient

More information

Predicting the Lifetime of Flexible Permeation Barrier Layers for OLED Displays

Predicting the Lifetime of Flexible Permeation Barrier Layers for OLED Displays Predicting the Lifetime of Flexible Permeation Barrier Layers for OLED Displays Bhadri Visweswaran, Siddharth Harikrishna Mohan, William Quinn, Ruiqing (Ray) Ma, Jeff Silvernail, James Sturm, Sigurd Wagner

More information

Supplementary Information

Supplementary Information Supplementary Information Experimental Section Hybrid Nanoparticle Synthesis The hafnium nanoparticles surface-modified with methacrylic acid (MAA, Sigma Aldrich, 99%), trans 2, 3-dimethylacrylic acid

More information

Supporting Information s for

Supporting Information s for Supporting Information s for # Self-assembling of DNA-templated Au Nanoparticles into Nanowires and their enhanced SERS and Catalytic Applications Subrata Kundu* and M. Jayachandran Electrochemical Materials

More information

IONTOF. Latest Developments in 2D and 3D TOF-SIMS Analysis. Surface Analysis Innovations and Solutions for Industry 2017 Coventry

IONTOF. Latest Developments in 2D and 3D TOF-SIMS Analysis. Surface Analysis Innovations and Solutions for Industry 2017 Coventry Latest Developments in 2D and 3D TOF-SIMS Analysis Surface Analysis Innovations and Solutions for Industry 2017 Coventry 12.10.2017 Matthias Kleine-Boymann Regional Sales Manager matthias.kleine-boymann@iontof.com

More information

SUPPLEMENTARY INFORMATION

SUPPLEMENTARY INFORMATION SUPPLEMENTARY INFORMATION Towards wafer-size graphene layers by atmospheric pressure graphitization of silicon carbide Supporting online material Konstantin V. Emtsev 1, Aaron Bostwick 2, Karsten Horn

More information

Supporting Information

Supporting Information Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A. This journal is The Royal Society of Chemistry 017 Supporting Information Reduced Bimolecular Recombination in Blade-Coated,

More information

High Yield Synthesis of Aspect Ratio Controlled. Graphenic Materials from Anthracite Coal in

High Yield Synthesis of Aspect Ratio Controlled. Graphenic Materials from Anthracite Coal in Supporting Information High Yield Synthesis of Aspect Ratio Controlled Graphenic Materials from Anthracite Coal in Supercritical Fluids Suchithra Padmajan Sasikala 1, Lucile Henry 1, Gulen Yesilbag Tonga

More information

All-Inorganic Perovskite Solar Cells

All-Inorganic Perovskite Solar Cells Supporting Information for: All-Inorganic Perovskite Solar Cells Jia Liang, Caixing Wang, Yanrong Wang, Zhaoran Xu, Zhipeng Lu, Yue Ma, Hongfei Zhu, Yi Hu, Chengcan Xiao, Xu Yi, Guoyin Zhu, Hongling Lv,

More information

Supplementary Information. Large Scale Graphene Production by RF-cCVD Method

Supplementary Information. Large Scale Graphene Production by RF-cCVD Method Supplementary Information Large Scale Graphene Production by RF-cCVD Method Enkeleda Dervishi, *a,b Zhongrui Li, b Fumiya Watanabe, b Abhijit Biswas, c Yang Xu, b Alexandru R. Biris, d Viney Saini, a,b

More information

MSE 321 Structural Characterization

MSE 321 Structural Characterization Auger Spectroscopy Auger Electron Spectroscopy (AES) Scanning Auger Microscopy (SAM) Incident Electron Ejected Electron Auger Electron Initial State Intermediate State Final State Physical Electronics

More information

Supporting Information

Supporting Information Electronic Supplementary Material (ESI) for ChemComm. This journal is The Royal Society of Chemistry 2014 Supporting Information Controllable Atmospheric Pressure Growth of Mono-layer, Bi-layer and Tri-layer

More information

Direct-writing on monolayer GO with Pt-free AFM tips in the

Direct-writing on monolayer GO with Pt-free AFM tips in the Supplementary Figure S1 Direct-writing on monolayer GO with Pt-free AFM tips in the presence of hydrogen. We replaced the Pt-coated tip with a gold-coated tip or an untreated fresh silicon tip, and kept

More information

Large Scale Direct Synthesis of Graphene on Sapphire and Transfer-free Device Fabrication

Large Scale Direct Synthesis of Graphene on Sapphire and Transfer-free Device Fabrication Supplementary Information Large Scale Direct Synthesis of Graphene on Sapphire and Transfer-free Device Fabrication Hyun Jae Song a, Minhyeok Son a, Chibeom Park a, Hyunseob Lim a, Mark P. Levendorf b,

More information

The Effect of Water and Confinement on Self-Assembly of

The Effect of Water and Confinement on Self-Assembly of Supporting Information: The Effect of Water and Confinement on Self-Assembly of Imidazolium Based Ionic Liquids at Mica Interface H.-W. Cheng, J.-N. Dienemann, P. Stock, C. Merola, Y.-J. Chen and M. Valtiner*

More information

Characterization of Materials with a Combined AFM/Raman Microscope

Characterization of Materials with a Combined AFM/Raman Microscope Application Note 089 short Characterization of Materials with a Combined AFM/Raman Microscope Marko Surtchev 1, Sergei Magonov 1 and Mark Wall 2 1 NT-MDT America, Tempe, AZ U.S.A. 2 Thermo Fisher Scientific,

More information

Graphene: Plane and Simple Electrical Metrology?

Graphene: Plane and Simple Electrical Metrology? Graphene: Plane and Simple Electrical Metrology? R. E. Elmquist, F. L. Hernandez-Marquez, M. Real, T. Shen, D. B. Newell, C. J. Jacob, and G. R. Jones, Jr. National Institute of Standards and Technology,

More information

Team Captain: Ben Jones Design and Modeling: Elizabeth Ashley Modeling: Kerry Toole Prototyping and Secretary: Rachel Stein Treasurer: Mari Hagemeyer

Team Captain: Ben Jones Design and Modeling: Elizabeth Ashley Modeling: Kerry Toole Prototyping and Secretary: Rachel Stein Treasurer: Mari Hagemeyer Team Captain: Ben Jones Design and Modeling: Elizabeth Ashley Modeling: Kerry Toole Prototyping and Secretary: Rachel Stein Treasurer: Mari Hagemeyer 1 Background and Motivation Project Design Goals Technical

More information

Thermally Functional Liquid Crystal Networks by Magnetic Field Driven Molecular Orientation

Thermally Functional Liquid Crystal Networks by Magnetic Field Driven Molecular Orientation Supporting information Thermally Functional Liquid Crystal Networks by Magnetic Field Driven Molecular Orientation Jungwoo Shin, Minjee Kang, Tsunghan Tsai, Cecilia Leal, Paul V. Braun and David G. Cahill*,

More information

Understanding electron energy loss mechanisms in EUV resists using EELS and first-principles calculations

Understanding electron energy loss mechanisms in EUV resists using EELS and first-principles calculations Understanding electron energy loss mechanisms in EUV resists using EELS and first-principles calculations Robert Bartynski Sylvie Rangan Department of Physics & Astronomy and Laboratory for Surface Modification

More information

X-ray Photoelectron Spectroscopy/ Electron spectroscopy for chemical analysis (ESCA), By Francis Chindeka

X-ray Photoelectron Spectroscopy/ Electron spectroscopy for chemical analysis (ESCA), By Francis Chindeka X-ray Photoelectron Spectroscopy/ Electron spectroscopy for chemical analysis (ESCA), By Francis Chindeka X-ray photoelectron spectroscopy (XPS) or Electron spectroscopy for chemical analysis (ESCA), Surface

More information

Atomic Layer Deposition of Hafnium Oxide at Temperatures below 100ºC. K. C. Kragh

Atomic Layer Deposition of Hafnium Oxide at Temperatures below 100ºC. K. C. Kragh Atomic Layer Deposition of Hafnium Oxide at Temperatures below 100ºC K. C. Kragh Dept. of Physics and Optical Engineering, Rose-Hulman Institute of Technology REU Student in the Advanced Materials Research

More information

SUPPORTING INFORMATION

SUPPORTING INFORMATION Electronic Supplementary Material (ESI) for Nanoscale. This journal is The Royal Society of Chemistry 2014 SUPPORTING INFORMATION Materials Graphite powder (SP-1 graphite) was obtained from Bay carbon.

More information

Supplementary Information

Supplementary Information Electronic Supplementary Material (ESI) for Nanoscale. This journal is The Royal Society of Chemistry 2015 Supplementary Information Visualization of equilibrium position of colloidal particles at fluid-water

More information

Spectroscopy at nanometer scale

Spectroscopy at nanometer scale Spectroscopy at nanometer scale 1. Physics of the spectroscopies 2. Spectroscopies for the bulk materials 3. Experimental setups for the spectroscopies 4. Physics and Chemistry of nanomaterials Various

More information

Surface and Electronic Structure Study of Substrate-dependent Pyrite Thin Films

Surface and Electronic Structure Study of Substrate-dependent Pyrite Thin Films Surface and Electronic Structure Study of Substrate-dependent Pyrite Thin Films Talk Outline Stoichiometry and sodium study of pyrite thin films: Quick Review Surface structure of pyrite thin films Electronic

More information

Supplementary information. Derivatization and Interlaminar Debonding of Graphite-Iron Nanoparticles Hybrid

Supplementary information. Derivatization and Interlaminar Debonding of Graphite-Iron Nanoparticles Hybrid Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics. This journal is the Owner Societies 2017 Supplementary information Derivatization and Interlaminar Debonding of Graphite-Iron

More information

Graphene films on silicon carbide (SiC) wafers supplied by Nitride Crystals, Inc.

Graphene films on silicon carbide (SiC) wafers supplied by Nitride Crystals, Inc. 9702 Gayton Road, Suite 320, Richmond, VA 23238, USA Phone: +1 (804) 709-6696 info@nitride-crystals.com www.nitride-crystals.com Graphene films on silicon carbide (SiC) wafers supplied by Nitride Crystals,

More information

GEM-based gaseous Photomultipliers for UV and visible photon imaging. Dirk Mörmann Amos Breskin Rachel Chechik Marcin Balcerzyk Bhartendu Singh

GEM-based gaseous Photomultipliers for UV and visible photon imaging. Dirk Mörmann Amos Breskin Rachel Chechik Marcin Balcerzyk Bhartendu Singh GEM-based gaseous Photomultipliers for UV and visible photon imaging Dirk Mörmann Amos Breskin Rachel Chechik Marcin Balcerzyk Bhartendu Singh Gaseous Photomultiplier State of the art: Advantages: large

More information

Electronic Supplementary Information

Electronic Supplementary Information Electronic Supplementary Information Selective Diels-Alder cycloaddition on semiconducting single-walled carbon nanotubes for potential separation application Jiao-Tong Sun, Lu-Yang Zhao, Chun-Yan Hong,

More information

ARGON RF PLASMA TREATMENT OF PET FILMS FOR SILICON FILMS ADHESION IMPROVEMENT

ARGON RF PLASMA TREATMENT OF PET FILMS FOR SILICON FILMS ADHESION IMPROVEMENT Journal of Optoelectronics and Advanced Materials Vol. 7, No. 5, October 2005, p. 2529-2534 ARGON RF PLASMA TREATMENT OF FILMS FOR SILICON FILMS ADHESION IMPROVEMENT I. A. Rusu *, G. Popa, S. O. Saied

More information

Surface Analysis. Dr. Lynn Fuller Dr. Fuller s Webpage:

Surface Analysis. Dr. Lynn Fuller Dr. Fuller s Webpage: ROCHESTER INSTITUTE OF TECHNOLOGY MICROELECTRONIC ENGINEERING Surface Analysis Dr. Lynn Fuller Dr. Fuller s Webpage: http://people.rit.edu/lffeee 82 Lomb Memorial Drive Rochester, NY 14623-5604 Tel (585)

More information

Effects of plasma treatment on the precipitation of fluorine-doped silicon oxide

Effects of plasma treatment on the precipitation of fluorine-doped silicon oxide ARTICLE IN PRESS Journal of Physics and Chemistry of Solids 69 (2008) 555 560 www.elsevier.com/locate/jpcs Effects of plasma treatment on the precipitation of fluorine-doped silicon oxide Jun Wu a,, Ying-Lang

More information

MODERN TECHNIQUES OF SURFACE SCIENCE

MODERN TECHNIQUES OF SURFACE SCIENCE MODERN TECHNIQUES OF SURFACE SCIENCE Second edition D. P. WOODRUFF & T. A. DELCHAR Department ofphysics, University of Warwick CAMBRIDGE UNIVERSITY PRESS Contents Preface to first edition Preface to second

More information

Supplementary Figure S1. AFM images of GraNRs grown with standard growth process. Each of these pictures show GraNRs prepared independently,

Supplementary Figure S1. AFM images of GraNRs grown with standard growth process. Each of these pictures show GraNRs prepared independently, Supplementary Figure S1. AFM images of GraNRs grown with standard growth process. Each of these pictures show GraNRs prepared independently, suggesting that the results is reproducible. Supplementary Figure

More information

Supporting Information

Supporting Information Electronic Supplementary Material (ESI) for ChemComm. This journal is The Royal Society of Chemistry 2014 Supporting Information High-k Polymer/Graphene Oxide Dielectrics for Low-Voltage Flexible Nonvolatile

More information

Birck Nanotechnology Center XPS: X-ray Photoelectron Spectroscopy ESCA: Electron Spectrometer for Chemical Analysis

Birck Nanotechnology Center XPS: X-ray Photoelectron Spectroscopy ESCA: Electron Spectrometer for Chemical Analysis Birck Nanotechnology Center XPS: X-ray Photoelectron Spectroscopy ESCA: Electron Spectrometer for Chemical Analysis Dmitry Zemlyanov Birck Nanotechnology Center, Purdue University Outline Introduction

More information

PHYSICAL AND CHEMICAL PROPERTIES OF ATMOSPHERIC PRESSURE PLASMA POLYMER FILMS

PHYSICAL AND CHEMICAL PROPERTIES OF ATMOSPHERIC PRESSURE PLASMA POLYMER FILMS PHYSICAL AND CHEMICAL PROPERTIES OF ATMOSPHERIC PRESSURE PLASMA POLYMER FILMS O. Goossens, D. Vangeneugden, S. Paulussen and E. Dekempeneer VITO Flemish Institute for Technological Research, Boeretang

More information

( 1+ A) 2 cos2 θ Incident Ion Techniques for Surface Composition Analysis Ion Scattering Spectroscopy (ISS)

( 1+ A) 2 cos2 θ Incident Ion Techniques for Surface Composition Analysis Ion Scattering Spectroscopy (ISS) 5.16 Incident Ion Techniques for Surface Composition Analysis 5.16.1 Ion Scattering Spectroscopy (ISS) At moderate kinetic energies (few hundred ev to few kev) ion scattered from a surface in simple kinematic

More information

Supporting Information: Poly(dimethylsiloxane) Stamp Coated with a. Low-Surface-Energy, Diffusion-Blocking,

Supporting Information: Poly(dimethylsiloxane) Stamp Coated with a. Low-Surface-Energy, Diffusion-Blocking, Supporting Information: Poly(dimethylsiloxane) Stamp Coated with a Low-Surface-Energy, Diffusion-Blocking, Covalently Bonded Perfluoropolyether Layer and Its Application to the Fabrication of Organic Electronic

More information

Secondary Ion Mass Spectroscopy (SIMS)

Secondary Ion Mass Spectroscopy (SIMS) Secondary Ion Mass Spectroscopy (SIMS) Analyzing Inorganic Solids * = under special conditions ** = semiconductors only + = limited number of elements or groups Analyzing Organic Solids * = under special

More information

Supporting Information. Re-Investigation of the Alleged Formation of CoSi Nanoparticles on Silica. Van An Du, Silvia Gross and Ulrich Schubert

Supporting Information. Re-Investigation of the Alleged Formation of CoSi Nanoparticles on Silica. Van An Du, Silvia Gross and Ulrich Schubert Supporting Information Re-Investigation of the Alleged Formation of CoSi Nanoparticles on Silica Van An Du, Silvia Gross and Ulrich Schubert Experimental All manipulations were carried out under an atmosphere

More information