ZEISS Индустриален качествен контрол

"Дни на безразрушителния контрол 2018"

Anton Tonchev 2018-06-07 Agenda

1 Светът на ZEISS 2 От суровина до краен продукт. Being sure. 3 ZEISS Microscopy: Поглед към портфолиото 4 Корелативна микроскопия. Нови хоризонти в науката

Carl Zeiss Bulgaria, Anton Tonchev 2017-03-07 2 Светът на ZEISS ZEISS Group

Пазари Компанията . Индустриални решения . Изследователска дейност ZEISS е водеща световна група от фирми в . Медицинска техника оптичната и в оптоелектронната индустрия. . Оптика за крайни потребители Carl Zeiss AG не публична компания, а е изцяло притежавана от фондация Carl Zeiss Основни направления

SMT / Полупроводникова индустрия Наука & контрол на качеството

Медицинска техника Оптика за крайни потребители Повече от 35 Нобелови лауреати са използвали ZEISS микроскопи, за да направят света по-добър

Alvar Gullstrand Manfred Eigen Sir Paul M. Nurse Andre Geim Eric Betzig (Chemistry) Stefan W. Hell (Physiology or Medicine) Leland H. Hartwell Konstantin Timothy Hunt Novoselov William E. (Physiology or Medicine) (Physics) Moerner (Chemistry) Eric A. Cornell Robert Koch Christiane (Physics) Sir John B. (Physiology or Nüsslein- Gurdon Medicine) Volhard Shinya John O'Keefe (Physiology or Craig C. Mello Yamanaka May-Britt Moser Medicine) Andrew Z. Fire (Physiology or Edvard I. Moser (Physiology or Medicine) (Physiology or Medicine) Medicine)

1905 1906 1911 1925 1952 1953 1967 1991 1995 1999 2001 2002 2006 2008 2010 2011 2012 2013 2014

Sidney Brenner H. Robert Horvitz Richard Adolf Bert Sakmann Dan Erwin Neher John E. Sulston Shechtman Zsigmondy (Physiology or (Physiology or (Chemistry) (Chemistry) Medicine) Medicine) Harald zur Hausen (Physiology or Medicine)

Günter Blobel Osamu Shimomura (Physiology or Medicine) Santiago Ramón y Martin Chalfie Cajal Camillo Golgi Frits Zernike Ahmed A. Zewail Roger Tsien (Physiology or Medicine) (Physics) (Chemistry) (Chemistry)

6 Предизвикателства с различен мащаб

Пълна информация от микро до нано… Being sure. От суровина до краен продукт Производство на метали Сложен процес с много неизвестни Единственият производител с пълно портфолио за всички приложения… Микроструктура на материали Как да свържем информация от обработка, структура и различни механизми

m cm mm μm nm Å ZEISS Microscopy

Широко портфолио…

Stereo Sub-micron Widefield Polarized Confocal Nanoscale Helium Ion C-SEM FE-SEM FIB-SEM LM XRM LM LM LM XRM Microscope

1 μm 700 nm 250 nm 200 nm 200 nm < 50 nm < 2 nm < 1 nm < 1 nm < 0.5 nm

…за многобройни предизвикателства в света на научните изследвания. Качествен контрол от марко до микро

…често се налага да се правят комплексни анализи на различни по големина обекти

cm mm μm nm

Fractured Chain Printed Circuit Board Fibers Cathode of a Lithium Atomized Iron Powder Ion Accumulator Портфолиото в детайл ZEISS Microscopy Системи за визуална инспекция

Greenough-type stereo microscope: - Stemi 305: 5:1 zoom - Stemi 508: 8:1 zoom

Automated Digital Microscope: - Максимална резолюция ~ 1 μm - Максимално увеличени 1,011x

CMO optics SteREO Discovery: - V8 8:1/ V12 12:1/ V20 20:1 - Моторизиран - FL/ POL ZEISS Microscopy Прави микроскопи

Primotech Axio Lab.A1 Materials

Axio Scope.A1 Materials Axio Imager Materials ZEISS Microscopy Инвертни микроскопи

Axio Vert.A1 Materials:

- 5x кодиран ревловер за обективи - Светло поле, тъмно поле, DIC, C-DIC, флуоресценция и поляризация - VisiLED/HAL 100 осветление

Axio Observer 3/5/7 Materials:

- 6x кодиран револвер за обективи - Моторизирана система - Светло поле, тъмно поле, DIC, C-DIC, флуоресценция, фазов контраст и поляризация - microLED/HAL 100/HBO - Корелативна микроскопия - Конфокална микроскопия ZEISS Microscopy Специализиран софтуер за анализ на материали Graphite in Cast Iron

CircularPolarization Differential with additionalPolarizationDarkfieldBrightfield Interference lambda Contrast compensator (C-DIC)

ZEISS Axio Imager 2

Specimen preparation and image interpretation: Dr. H.-L. Steyer, Kesselsdorf, Germany

Carl Zeiss Microscopy Grain Size in the Eye of the Beholder...

Eyepiece reticle with ASTM E112

Possible sources of human error • Estimations rely on operator • Vary by operator • Data entered manually

Carl Zeiss Microscopy Modern Digital Metallurgical Laboratory

Digital Stereo Upright Inverted Widefield Polarized

Confocal LIGHT MICROSCOPES LIGHT

• Comparative Diagrams to compare to standards, images, and custom views • Standards available: EN ISO 643, ASTM E 112, ASTM E 1382, BS 4990, SEP 151061, EN 10247, DIN 5060 Grain Structure Analysis Starts with an image with good contrast

Aluminum imaged with polarizer with lambda plate (full wave) Determine Grain Size Automatically or interactively with high precision and reproducibility Multiphase Alloy Analysis Quantification and reporting

Analyze distribution of different phases:

• Solid vs air/void • Mixture or metallic phase Brass, etched (bright field) Brass, segmented • Intermetallic compound

Report with multiphase analysis results Report with multiphase analysis results Non-metallic Inclusions (NMI) Automatic detection, measurement, and reporting

Sulfide inclusions in steel

• Large sample surface areas to be scanned automatically: inclusions are recorded in their entirety • Objectives for outstanding contrast and resolution • Fully motorized for reproducible system settings LSM конфокална микроскопия ZEISS LSM 800 за материали Конфокален микроскоп за изследване на материали и качествен контрол

Carl Zeiss Microscopy 8/4/2018 27 ZEISS LSM 800 за материали Възможни приложения

Surface Metrology Structural Analysis of Composite

Layer Thickness Measurement Find deposits of raw materials

Carl Zeiss Microscopy 8/4/2018 28 ZEISS LSM 800 за материали Възможни приложения

Aluminum structure in Printed graphite structure, color coded height map Paper surface with indent from pen, 3D-view of Circular Differential Contrast (C-DIC) C Epiplan-APOCHROMAT 20x/0.7 color coded height map EC Epiplan-NEOFLUAR 10×/0.25 C Epiplan-APOCHROMAT 20x/0.7

Surface texture of geometric standard (ISO 5436-1, type C) Fiber composite. Comparison of different Erosion on electrical switch. Evaluation of material 3D-view of color coded height map with profile view contrast methods erosion and accumulation. 7x1 tiles image to get the evaluation length of 4mm Left Brightfield, right Fluorescence 5x5 tiles image C Epiplan-APOCHROMAT 10x/0.4 C Epiplan-APOCHROMAT 20x/0.7

Carl Zeiss Microscopy 8/4/2018 29 Сканиращ електронен микроскоп за Материалознание ZEISS CSEM продуктово семейство. EVO Най-високо качество на изображението в всички режими на вакуум EVO High Definition Imaging in All Vacuum Modes

New Variable Pressure & Extended Pressure Detectors

. VPSE-G4 provides the improved VP imaging up to 400 Pa

. C2D provides an upgrade over VPSE-G4 for the best VP imaging up to 750 Pa

. C2DX provides the best EP imaging up to VPSE G4 Max: 400 Pa 3000 Pa

C2D Max: 750 Pa

C2DX Max: 3000 Pa

Min P = 10 Pa Q: What adds Electron Optics to Light Optics? A: Different and Complementary Contrast Methods

Light Microscopy Scanning Electron Microscopy

Industrial diamonds

Contrast from color and reflections Contrast from shades of grey and edges Three Contrast Methods unique to SEM

Surface Morphology Phase Contrast Elemental Chemistry

Secondary Electron Image (SE) Backscattered Electron Image (BSE) Mo Elemental Map Stainless Steel Fracture Dissimilar joint between low alloy steel and nickel alloy Secondary Electron Imaging Yields high detail Surface Morphology

Zinc-phosphate E-coating as applied to car body panels, delineated by “edginess” of SE contrast mechanism Backscattered Electron Imaging Yields a Snapshot of Compositional Differences

Tyre Cord steel threat in rubber, revealed by phase contrast scaling with the density of the materials Steel = high density = bright, Rubber = low density = dark Energy Dispersive Spectrometry (EDS) Major and minor element analysis

EDS analysis Information from EDS . Most common analytical method used in electron microscopy X-ray spectrum . Fast acquisition . Accurate to 0.1 wt.% for most elements . Single point, area and line scans . Elemental quantification . Element distribution maps

Quant Elemental maps Elem. Wt.% Ni 58.8 Co 12.4 Cr 19.0 Mo 4.2 Ti 3.1 Fe 0.8 Electron Back Scattered Diffraction (EBSD) Crystallography

EBSD Information from EBSD . Commonly used in Metals & Steel applications . Provides point analysis, phase discrimination, Fore-scatter Imaging Orientation Maps crystal orientation, texture & grains

Strain analysis Microstructural data

Elemental maps

Crystal Orientation Pole figures ZEISS Microscopy SEM images with measurement ZEISS Microscopy …and EDS element analysis Нов стандарт в изследването на Материали Корелативна микроскопия Защо корелативна микроскопия? Всичко на едно място – от микро до нано

Carl Zeiss Microscopy 42 Защо корелативна микроскопия? Функционална и структурна информация в едно

LM

LM EM EDX-overlay

EM

An alternative mode of correlative microscopy is to take th two images from the same sample at the same location and overlay them to generate a new level of information. Board (Electronics) Correlative Microscopy with Shuttle & Find

LM 5x SEM VPSE 200x Correlation

Application Challenge Solution

• Application Board failure • Searching for the root cause • The correlation of images analysis of a failure (root cause of a enables an assumption for the temperature impact) root cause • e.g. metallic particles, bores in • The particle is the reason for solder, corrosion, bad the failure / temperature impact interfaces, defect phases Li-ion Batteries Correlative Microscopy with Shuttle & Find

Brightfield Image LM Polarized light image LM Correlation with elemental composition

Application Challenge Solution

• microstructure characterization • analyze relations between cell • The correlation of images of Li-ion batteries to achieve design and battery enabled to workout qualitatively deeper understanding of the performance that the sharply edged grains battery performance within the cathode active material • extraction of quantitative are composed of LiMn O microstructure data to develop 2 4 whereas the roundly shaped physical models grains consist of LiNixCoyO2 ZEISS Microscopy Portfolio Multi-Scale Characterization for Multi-Scale Research

A complete microscopy portfolio…

Stereo Sub-micron Widefield Polarized Confocal Nanoscale Helium Ion C-SEM FE-SEM FIB-SEM LM XRM LM LM LM XRM Microscope

1 μm 700 nm 250 nm 200 nm 200 nm < 50 nm < 2 nm < 1 nm < 1 nm < 0.5 nm Versa Ultra …to address multi-scale research challenges. 520 Versa X-ray Microscope vs Conventional MicroCT

Conventional MicroCT 520 Versa X-ray Microscope

Source Source

(Dss + Dds) GeoMag = Dss

XRM is well suited for package FA - it maintains resolution regardless of package size

Carl Zeiss SMT PCS Tomography in 3D X-ray Microscopy: How it Works

Acquire 2D Projections While Rotating Sample

Reconstruct 3D Volume Obtain “Virtual Cross Sections” XRM is a high-resolution complementary technique to physical cross sectioning

Head in Pillow Defect (1”x1” package, 2hr scan)

XRM Image* Optical Microscope Image* non-destructive virtual cross-section physical cross-section (destructive)

Red arrows show polishing defects caused by physical cross-section *Source: IEEE/SEMI ASMC 2013

Изследване на материали

Polarized light image from a SubHydration-micronThaumasite20 nm of thick 3cement dimensional layerssulphate imaged of cementdataattack in cross-section of concrete takencapturedwith EVOaimaged concrete fromenvironmental with a samplecement Crossbeam. - imagedbasedSEM with with Axio Imager 2 for buildingby controllinga Sigma material theFESEM with humidity, a and Versa Materials Research. Xtemperature-rayMineralogic Microscope. and pressuresoftware. in the chamber.

Compound Confocal X-ray Scanning Field Emission Focussed Ion Helium Ion Electron Scanning Electron Beam

1um 200 nm <50 nm < 2 nm < 1 nm < 1nm < 0.5 nm

Carl Zeiss Microscopy 8/4/2018 51 Корелативна микроскопия за изследване на материали Аналитична информация

Particle chemistry

Inclusion standards

Failure inspection

Crystallography Nanotomography

Crack analysis

m cm mm μm nm Å Надежден партньор в науката Посетете нашата уеб страница!

www.zeiss.com/microscopy Carl Zeiss Microscopy GmbH, Global Marketing 08.08.2012 55