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electron spectroscopy for chemical analysis

under environmental conditions

Key Features
• Fast Quality Control
• High Throughput Analysis
• Controllable Atmosphere
• Revolutionary Technology
• Ergonomic all-in-one Design
• Fully Software Controlled
Innovation in surface Spectroscopy
and microscopy systems

SPECS leads the way in developing


cutting-edge components and systems for
groundbreaking new surface analysis tools.

SPECS Surface Nano Analysis GmbH


SPECS Surface Nano Analysis GmbH headquarters
is situated in the center of Germany’s capital
Berlin with subsidiaries in Switzerland, USA and
Mounting of EnviroESCA
component for final testing China. SPECS has attracted a talented team of
scientists and engineers who have dedicated their
knowledge and experience to the development,
design, and production of instruments for surface
science, materials research, and nanotechnology
for almost 30 years.

In order to continuously improve performance


and keep abreast of the latest developments,
we are in contact with numerous scientists,
SPECS engineer during users and customers from all over the world.
system assembly Reliable quality control (ISO 9001 certified) and
excellent fast service, both remote and on-
site, ensures maximum uptime and long-term
operation and reliability of SPECS instruments
over many years.

EnviroESCA
EnviroESCA
Electron Spectroscopy for Chemical Analysis
under Environmental Conditions

A new dimension in chemical surface


analysis

Electron Spectroscopy for Chemical


Analysis – Past to Present
In 1905 Albert Einstein received the Nobel The global success of X-ray Photoelectron
Prize in Physics for his quantum mechanical Spectroscopy (XPS) is a result of the development
interpretation of the photoelectric effect. of methods for reliable and precise quantification
Based on the results of Heinrich Hertz and of ESCA data with an elemental detection limit of
Max Planck about the nature of light being <1% in the uppermost surface layers. Already in
an electromagnetic wave and about the the early 1970s Kai Siegbahn realized, that the
general existence of discrete energy portions, Ultra-High Vacuum (UHV) environment necessary
nowadays named “quantum”, this has been a in conventional ESCA machines is limiting the
big step for basic science. At this time nobody applications of this method to solid sample
knew, that this will evolve into the most surfaces. So he suggested applying ESCA to
important method for non-destructive surface liquids, using a differential pumping setup for the
chemical analysis. To reach this understanding analyzer and X-ray source. He was able to reach
the development of energy dispersive electron a maximum pressure of 10-2 mbar at that time.
analyzers had been necessary.
Again it took almost three decades in experi-
Thus it took several decades until Kai Siegbahn mental development to reach pressures of up
developed and experimentally realized the first to 1 mbar in synchrotron experiments. (Near)
experiment of this kind in the late 1960s, again Ambient Pressure XPS ((N)AP-XPS) was born,
resulting in a Nobel Prize in Physics. By excitation yielding fundamental insight in the operation of
of electrons from solid samples using characte- catalysts and the analysis of liquids and liquid-
ristic X-rays and detecting the number of solid interfaces. State-of-the-art instrumentation
photoelectrons in dependence of their kinetic for NAP-XPS allows for purely laboratory-based
energies it became possible to use the element- NAP-XPS systems as the use of synchrotron
specific electron energies to derive the chemical radiation is not mandatory anymore.
composition of sample surfaces without destroying
them. He named the method Electron Spectro- It is time for the next step in evolution.
scopy for Chemical Analysis, or in short ESCA.
EnviroESCA
electron spectroscopy for chemical analysis
under environmental conditions

The Beginning of a New Era


Building on our pioneering developments of
recent years SPECS proudly presents EnviroESCA.
This novel and smart analysis tool overcomes
the barriers of standard XPS systems by enabling
analyses at pressures far above UHV. EnviroESCA
is designed for high-throughput analysis and
opens up new applications in the fields of medical
technology, biotechnology and the life sciences.
It offers the shortest loading-to-measurement
time on samples of all types including liquids,
tissue, plastics and foils, powders, soil, zeolites,
rocks, minerals and ceramics.

Environmental Integrated
• Controllable atmosphere from sample • Ergonomic all-in-one design
loading to analysis • Quick installation and setup
• Adaptable process gas dosing systems • Minimized downtime
• Specialized sample environments • Cost and time efficient servicing
• Compatible with all kinds of samples and • Easy consumable replacement
sizes up to Ø 120 mm and 40 mm in height

Networking Reliable
• SampleExplorer • Reproducible analysis recipes
• SmartDock • Comprehensive system parameter logging
• AutoLoader • Uptime focused user support
• GloveBox
Optimized
Versatile
• Application oriented software package
• Revolutionary analyzer technology • Fully remote operation
• μ-Focus X-ray source • Automated vacuum system
• High resolution XPS • Easy to use sample loading
• Environmental Charge Compensation • Optical sample navigation
• Sputter depth profiling

EnviroESCA
Environmental
Enviroesca - chemical surface analysis under
environmental conditions

Key Applications for EnviroESCA


XPS is established as a powerful and wide-ranging non-destructive analytical method. In
particular, the precise and reproducible quantification of trace signals which it affords, has
helped to answer important questions in fundamental and applied science. EnviroESCA enhances
the significance of the results in many conventional applications and expands the technique’s
horizons. Feel free to browse the growing application note catalogue on the EnviroESCA website
www.EnviroESCA.com

Liquids Gaseous and Liquid


Environments
Water and aqueous reagents
are essential in any biologi- The interaction of gases
cal process or system. But and liquids with surfaces
apart from a few special low plays a key role in many
vapor-pressure cases, liquids different fields ranging
have not been accessible to any technique requir- from biological and catalytic systems to
ing UHV conditions. EnviroESCA opens up this construction materials. EnviroESCA offers the
exciting field of applications. possibility of investigating surfaces in contact
with gases and liquids, such as salt water, acidic
rain, wastewater, or gaseous atmospheres
Astrochemistry and with high humidity.
Astrobiology
The interaction of organic
Biological Materials
molecules with water and
ice surfaces in atmospheres With the capability of oper-
that can be found on ating in the near ambient
distant planets is a vital field of research. pressure regime EnviroES-
EnviroESCA can create sample environments CA offers an entirely new
that realistically simulate conditions in planetary opportunity to investigate
atmospheres such as on Mars, where the biological materials and processes, making ESCA
pressure ranges from 10-6 mbar to 7 mbar. more versatile than ever before.
Food Science Archaeology and
The outer surfaces of
Archaeometry
food from organic and The analysis of priceless
industrial production ancient artifacts with
processes are in contact surface science techniques
with the atmosphere that like XPS and NAP-XPS allows
surrounds them, already on the field or later in to deliver results about the
the production hall, in the fridge or in its sales surface composition of metallic and non-metallic
packaging. Therefore the investigation of the specimens without damaging or destroying
interaction between different atmospheres and them. EnviroESCA offers the possibility to load
the food is essential to understand what are large and uneven samples and to perform the
the parameters for optimizing the packaging or analysis in environmental conditions which will
pretreatment of eatables to avoid contamination preserve the delicate relics.
and to keep them fresh for a longer time.

Cosmetics
Pharmaceutical
Cosmetics in contact with
Research
skin and hair interact on the
Pharmaceutical drugs molecular level. Therefore
interact with different tuning and optimization of
atmospheres on their way the interface plays a key
from the production line to role for the character of the interaction between
the patient. Their surfaces interact for example the ingredients and the tissue.
with the press were they are brought into
their shape over to the sales packaging where
they are stored and finaly to the contact
Soils and Minerals
with the hand of the patient and the acidic
atmosphere of the body. EnviroESCA helps XPS analysis is widely used
to understand these interactions on the in soil and mineral research
molecular level of their surfaces and to optimize for characterizing surface
production or storage processes. organic films, mineral de-
composition and redox
transformations. Until now these studies were
limited to UHV compatible samples. EnviroESCA
overcomes this constraint and offers new exciting
possibilities.

EnviroESCA
Fabrics Medical and 7
Biomaterials
The performance of highly
sophisticated fabrics is Medical implants are
governed by the interac- devices or tissues that
tion of the interface with are placed inside or on
the surrounding atmos- the surface of the body.
phere. By studying the surface properties of A widely used material for surgical implants is
the fibers in wet air, deeper insights into rele- Titanium. It is important to be able to analyze the
vant processes under more realistic conditions Ti surface to achieve optimized interactions with
can be gained. the surrounding tissue.

Energy Materials Catalysts


and Devices
The function and efficiency
Batteries and fuel cells are of a catalyst is principally
devices that use chemical determined by its surface
reactions to store and properties. XPS and NAP-
convert energy. Fuel cells XPS are proven and
for instance consume fuel and oxidants during powerful tools for investigating catalytic
operation so that their investigation is not behaviour in studies ranging from model systems
possible in traditional XPS spectrometers. With to real world materials.
EnviroESCA the funda-mental steps in such
devices can be investigated in operando.
Coatings and Thin
Films
Polymers and Coatings and platings
Plastics are widely used in optics
Polymers and plastics are manufacturing and metal
used in many fields such refinement as they
as food grade packaging optimize the surface
and medical technology. properties of materials to make them harder,
Their composition is stronger and more durable. The coatings are
especially important when the polymers get thin films which interact with the substrate
in direct contact with food or humans. With on one side and the gaseous or liquid
EnviroESCA the concentration of hazardous environment on the other.
contaminations can be quantified regardless
of their vacuum compatibility.
Nanomaterials Metals
Nanomaterials have Metallic parts can rapidly
attracted a lot of attention be analyzed without
from research and industry pre-cleaning or surface
in the past decades. preparation. With the
Questions about the unrivaled short sample
influence of the surrounding atmos-phere on the loading time and the robotic AutoLoader
chemical composition and potential core-shell they can be taken directly from the production
structure are ideally addressed by EnviroESCA. line for quality control.

Corrosion Microelectronics and


The reliability of
Semiconductors
mechanical or electrical The quality of conductive
connections depends platings on printed
strongly on their chemical circuit boards is crucial
composition and degree for the operation of any
of corrosion. EnviroESCA facilitates the microelectronic device. With the AutoLoader
investigation of the metal surface in interaction this high performance tool is ideally suited
with its surrounding gas or liquid phase for unattended and automated analysis
environment to gain a detailed understanding of microelectronic devices.
of processes governing corrosion.

EnviroESCA
Networking
Enviroesca - chemical surface analysis under
environmental conditions

SampleExplorer
Measurement time can be saved by planning
experiments in advance with the stand-alone
SampleExplorer. An unlimited number of
measurement positions and tasks can be defined
for batch processing before inserting the sample
into EnviroESCA. A high precision sample stage
is embedded in a geometrical mockup of the
analysis setting. Equipped with three high
resolution cameras it enables documentation
of the analysis area. For each measurement
position a “through the lens” view with an optical
resolution well below 10 µm and a wide angle
view of the analysis position are recorded in
conjunction with a survey view of the platter.

SmartDock
All samples are introduced to the sample
environment modules via SmartDock. It consists
of a sliding door mechanism for manual sample
loading with a connection system for easy docking
of sample containers. The sample containers
allow transportation of samples prepared
ex situ under vacuum or gas atmospheres.
While docked, sample containers are supplied
with power, gases and pressurized air for valves
or actuators. The containers are fully integrated
into the EnviroESCA device network for remote
control or automation. The SmartDock can also
be exchanged with a glove box docking system.
Versatile
Enviroesca - chemical surface analysis under
environmental conditions

EnviroESCA features a unique modular approach in pressure ranges from ultra-high vacuum
to the system design, combining the advantages to hundreds of mbar are now possible. This
of several specialized ESCA systems in a single combination enables the user to investigate even
entity. It is adaptable to suit different experimental the most challenging samples of a class that was
conditions through the use of dedicated incompatible with traditional ESCA equipment.
interchangeable sample environment modules. As Furthermore the ionized gas atmosphere provides
in any conventional ESCA instrument the electron low energy ions and electrons, that lead to a self-
energy analyzer and the X-ray source are the key compensating process named environmental
components of EnviroESCA. But combined with charge compensation. Thus nearly every insulating
SPECS advanced, automated vacuum and gas- sample can be characterized without additional
handling systems, reliable working conditions components.

Electron Energy Analyzer Ion Source


• Hemispherical analyzer • Scannable small spot ion source
• Specialized for environmental applications or gas cluster ion source as
• Delayline electron detector with up to optional components
400 channels

Charge Compensation
Microscopes
• Environmental Charge
Compensation by X-ray • Digital microscopes for
photoionization of the gas easy sample positioning
molecules above the and documentation
sample surface

X-ray Source
Analysis Compartment
• Al Kα micro-focused
• Minimized chamber
monochromator
volume
• Variable spot sizes
tailored to experimental
• Stainless steel
requirements

EnviroESCA
11
The unique sample environment in EnviroESCA as smart units for different classes of samples
makes it ideally suited for characterization of and applications. The modules are equipped
materials that may not be UHV compatible: with all relevant components such as sample
The stringent UHV requirement of conventional stage, plasma cleaning and gas handling. Their
XPS is dispensed with in EnviroESCA. Dedicated exchange can be readily accomplished in just
sample environment modules are provided a few minutes.

Digital Microscope
• Video recordings and still photos of the sample
during pump down or pretreatment cycles
Quick Connector
• Gas tight seal between
sample environment and
analysis compartment Pumping System
• Fully computer controlled
Gauges integrated pumping stages

• Full range gauges from


ambient to ultra high
vacuum conditions
• Gas type independent SmartDock
capicitance gauges
• Sliding door mechanism for
manual sample introduction
Plasma Cleaner • Allows mounting of sample
containers under vacuum or
• RF plasma cleaner
with inert gas filling
for sample and
equipment cleaning

Sample Stage Sample Connections


• Fully motorized sample • Spare ports for electrical, gas or
stage for precise positioning liquid feedthroughs to connect the
of the sample in front of the sample with the outside
analyzer and X-ray source • Examples are thermocouple
• Samples can be of any shape contacts, multipin feedthroughs for
within a volume of Ø 120 mm Peltier cooling or heating stages,
and 40 mm in height USB, fiber optics and many more
Integrated
Enviroesca - chemical surface analysis under
environmental conditions

The compact all-in-one design of EnviroESCA Located centrally on the front face is the sample
includes all the necessary equipment, loading bay where samples are introduced into
from power supplies to closed-cycle water the Sample Environment.
cooling, within a single small-footprint unit.

Analysis Module
• Excitation sources Status Indicator
• Electron analyzer
• Gas dosing • Integrated design

Service Accesses Sample Loading Bay


• Ergonomically positioned • Quick access door
• Monitored access • SmartDock
• Safety glass

Sample Environment
Dimensions • Precision sample stage
• RF plasma cleaner
• Footprint 2.1 m x 1.7 m
• Height 2.7 m
• Weight 1800 kg

EnviroESCA
13
Compact dimensions and vibration isolation of access facilitates fast and simple maintenance
the backing pumps ensure that EnviroESCA can and consumable replacement. All connections
be installed with ease in sensitive and space- to the laboratory infrastructure are located at
constrained laboratories. Convenient service a central position.

Thermal Management
• Forced air and convection cooling

Vacuum System
• Integrated design
• F ully computer Electronics
controlled
• 
Integrated pumping • Integrated cabinets
stages • M
 easurement and
automation PC

Gas Handling
• S pecialized gas
dosing units

Cooling System
• C
 losed-cycle water
cooling

Connectivity
• Mains
• Purge and venting gas
• Process gases
Service Access
• Pressurized air
• Accessible machine interior
• Monitored access
Reliable & Optimized
Enviroesca - chemical surface analysis under
environmental conditions

Automation Experiment Recipes


The advanced software control system enables Customized measurement recipes simplify the
fully automated sample analysis to be carried workflow of complex experimental procedures.
out. It controls the vacuum system, the gas The SampleExplorer is a fully integrated but
handling system and all analysis components. stand-alone tool to define experiments in advance
Even operation from mobile devices is possible. for most efficient use of the measurement time.
Software tools such as a periodic library are
of course included to assist less experienced
operators.

XPS survey spectrum


shown in experiment Data Processing
recipes editor
Advanced curve-fitting routines used for
automated peak identification and quantification
are just one example of the feature-packed
In addition, the optional robotic AutoLoader can software package. Specific data sets are easily
be used for completely unattended introduction retrieved from the central database by using
and processing of sample batches. Thus high- advanced search routines. Each entry can be
throughput analysis of stored samples or parts tagged and grouped for batch data analysis.
taken from production lines can be realized in a
unique way. Manual access to all procedures is
nevertheless available to experienced users.

Data Logging
All system parameters including temperature of
system components, pressure readings, and
equipment health status are permanently
recorded. Availability of this database makes for
time-efficient service and maintenance. Service
All system components were designed or selected
for extended lifetime operation and highest
reliability ensuring low cost-of-ownership.
EnviroESCA offers the possibility of full remote
Vacuum control control of the entire system. Rapid and easy
expert view maintenance reduces down-time and service
costs to a minimum.

EnviroESCA
Technical Data
15
Summary

EnviroESCA Sample Environment


(standard, others on request)

• Hemispherical electron analyzer with Sample • High precision 3-axis


Electron 150 mm mean radius Stage stage
Spectrometer • Differentially pumped lens system • Up to 120 mm in
• Delayline detector with up to 400 channels diameter and 40 mm
• Al Kα micro-focused monochromator in height
Sample Size
• Rowland circle diameter of 600 mm • 50 mm inner
X-ray Source
• Spot sizes of 200 µm – 1 mm optimized diameter
to analysis area addressable

Charge • Environmental Charge Compensation • Mass flow controlled


Neutralization Gas Dosing process and purge
• Scannable small spot ion source gas
Ion Source
(200 eV – 5 keV) • Downstream RF
(optional) Cleaning
• Gas cluster ion source plasma cleaner
• Turbomolecular pumps • Digital microscope
Pumping System
• Oil-free backing pumps for sample
Camera
• Defined by analyzer aperture observation and
Pressure Range (up to 100 mbar with an aperture of 300 µm; documentation
other aperture sizes on request)
• Two separated gas dosers at analysis position
Gas Dosing System
• Mass flow controllers
• 3 digital microscopes for sample
Cameras
navigation and documentation
• Fully automated vacuum and gas
Automation and
dosing system
Software
• Advanced software package

Dimensions
2100 mm
1700 mm
2700 mm

2000 mm
SPECS Surface Nano Analysis GmbH
Voltastrasse 5
13355 Berlin / Germany
www.EnviroESCA.com

T +49 30 46 78 24-0
F +49 30 46 42 083
E info@specs.com

Version 02.03

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