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The “GANESHA”

A next-generation SAXS instrument

by

JJ X-Ray Systems Aps Aka SAXSLAB

White Paper

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SAXSLAB’s GANESHA

SAXLAB’s GANESHA is a next-generation SAXS instrument making extensive use of synchrotron-type tried and trusted motorization, neutron-type experimental approaches, as well as the latest technology in networked instrument control and data analysis. Thus fully automated and remotely controllable, it represents a true leap in SAXS instrument user-friendliness and functionality,

The most striking feature of the GANESHA is that the detector is situated inside a large continuous vacuum chamber, where it can be controlled to adjust the distance between sample and detector. This allows for access to an unprecedented q-range, spanning both the very low q-range to standard WAXS range. In addition, the GANESHA has a large spacious sample area allowing for a variety of sample environments and specialized measurement techniques. In all versions, the GANESHA makes use of recently developed detectors with an unprecedented combination of low-noise, high dynamic range, high spatial resolution, high detection efficiency and extremely high resistance to radiation damage and deterioration. In the high-end versions use is also made of the recently developed micro-focus sources providing up to a factor of 40 increase intensity over systems based on conventional sealed tube sources.

Even in the low-end versions of the GANESHA, the full functionality is maintained, including capability of performing SAXS, MAXS, WAXS, GISAXS and Reflectometry on both isotropic and oriented samples.

Introduction 1

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Justification for yet another SAXS instrument

With experience in constructing gas-detectors and lab-based SAXS systems since the 1980’s, as well as commercially supplying such systems since 2004, it has long been a dream of ours to develop the ideal lab-based SAXS instrument, providing this to the growing group of SAXS users. In our opinion, the ideal SAXS instrument is able to probe samples over a large range of length scales (SAXS/MAXS/WAXS), is able to perform many experimental techniques, while handling many types of samples and employing various sample-manipulation methods. Also, the ideal SAXS instrument for the 21st century needs to do these things in a way that allows the non-expert to be able to easily carry out these wide range of measurements, without damaging the instrument and jeopardizing the quality of data. The GANESHA is exactly such an instrument, and to the best of our knowledge the only commercial system living up to the ideal criteria.

Why GANESHA?

Shri Ganesha is a Hindu god symbolizing Intellect, Wisdom, and Education as well as the god of good fortune in new endeavours. He is often depicted in the form of a four-armed being with an elephant head. Ganesha’s traits thus fit extremely well with the actual SAXS instrument functionality and appearance. As examples, we can mention Ganesha’s large ears for listening, elephant head and trunk, and large body with a potbelly full of infinite universes.

SAXSLAB and JJ X-Ray Systems History

SAXSLAB is the name under which JJ X-Ray Systems ApS., a small Danish company, presently markets its SAXS product portfolio. Until August 2009 these products were marketed under the JJ X-Ray name. But in order to accurately reflect the company’s increasing commitment to SAXS instrumentation, the gradual transition to SAXSLAB has begun. Since 2004 the company has provided over 14 mostly high-end SAXS systems to European and Middle Eastern customers. These have often been highly customized in terms of their application scope and constituent components, but have in most cases been based on the 1st generation platform developed by Molecular Metrology, (a company later acquired by Rigaku US), with customization and integration performed by JJ X-Ray Systems ApS. JJ X-Ray Systems ApS’s technical expertise derives from more than 20 years of experience in the construction and optimization of X-Ray equipment for a number of experimental techniques in both synchrotron and home-laboratory application. In addition JJ X-Ray Systems ApS, draws strongly on the local manufacturing and scattering expertise in the Copenhagen area.

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Experimental techniques easily obtainable with the GANESHA

The GANESHA can be easily configured to perform any of the following measurement techniques:

• SAXS • GISAXS1 • Reflectometry- with 2D detector1 • MAXS • WAXS

Basic Elements of the GANESHA

All versions of the GANESHA consist of the following elements (many elements having a number of options)

• X-ray source (3 options - all with multilayer monochromators) • X-ray filter (motorized ) • Collimation/Pinhole System - (2 Options – all Evacuated and Motorized) • Sample Chamber (3 Options: In air, Large and Evacuated, Small and Evacuated ) • Sample Stage (many options- all Internal and Motorized) • Sample Viewer (Internet-enabled consisting of 2 cameras for avoiding parallax effects) • Detector Positioning Stage (3 axis: Distance from sample, Vertical and Horizontal) • Pilatus Solid State 2D photon counting Detector (many possible sizes – size determined by budget) • Multiple Interchangeable Beam stops in front of the detector • Insertable Pin-diode detector for recording beam intensity and transmission • Motor Controller • Vacuum Pumping System • Instrument server (controlling all components and the measurements) • Instrument control client (for controlling the instrument server remotely) • Data reduction software • Date analysis software • Sample standards for instrument calibration • Instrument Support Table, with instrument server and electronics integrated

Description of Optional elements for the GANESHA

Additional available options for the GANESHA

• Various Sample Stages • Micro-beam option requiring additional collimator unit

1 Requires Rotary Sample Stage

The GANESHA 2

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A leap in functionality

We consider the GANESHA to be a next generation SAXS system for the home laboratory due to the incorporation of significant leaps in functionality and user friendliness, compared to prior commercial systems. We consider particularly the following functionality leaps to be most significant

• The possibility for the detector to be moved automatically inside the vacuum-tank to cover a

wide range of scattering angles from low-q SAXS to true WAXS.

• The motorization of collimator, sample positioning, and the detector means that user alignment can be completely automated, and the instrument can make intelligent use of the various achievable intensity and resolution combinations, specifically:

o The motorization of the pinholes allows the system to automatically change between different pinhole configurations optimize the intensity in the beam without user interaction

o The motorization of the detector and associated beam stop allows for both automated alignment of the beam stop in the beam automatically shifting the position of the detector to acquire additional data in a

different q-range (a total q-range of 2E-3 Å-1 to ~3Å-1 is possible)2

• The use of the Pilatus detector3 provides the following advantages over existing SAXS detectors (gas, image plate, and CCD)

o Low background on par with (or better than) gas-detectors due to individual Photon counting capability with rejection of noise and cosmic radiation

o No parallax o A very fine detector resolution (172 microns) o A high detection efficiency at 8 keV o A very high maximum pixel count rate (2 million counts per second per pixel) o No damage to the detector if hit by the primary beam in the laboratory

• Changing between SAXS, WAXS, GISAXS, and Reflectometry configuration is only a software

issue, not requiring any alteration to the instrument hardware.4

• The possibility to control and monitor the measurement process remotely

2 Limits will depend on actual detector size and sample environment 3 The Pilatus detector is a revolutionary imaging solid state detector, developed at the Swiss Light Source, and now sold by the Swiss company Dectris 4 Requires a sample stage with a rotation and a GISAXS/Reflectometry beam stop

Why Next Generation? 3

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Table of Components and Options

Component Options/Description Original

Manufacturer Comment

X-ray Source Sealed Tube (Cu or Mo) GE Inspection Sturdy, Reliable, Lowest Intensity (Intensity ~1) Genix 3D (Cu or Mo) Xenocs 2nd Generation Microfocus Source Micromax 002+ (Cu) Rigaku US 2nd Generation Microfocus Source (~12X intensity) 007HFM (Cu or Mo) Rigaku Japan Microfocus Rotating Anode (~35X intensity)

Filter Several filter thicknesses JJ X-Ray Provides at least 5 different filter Configurations Collimation 4 Round Pinholes JJ X-Ray Provides 3 Resolution/Intensity Configurations

Square Slit-formed Apertures JJ X-Ray Provides Infinite number of Resolution/Intensity Configurations Sample Chamber In Air

Large, Evacuated Small, Evacuated

JJ X-Ray JJ X-Ray JJ X-Ray

For users wanting to work with samples only in air. Allows for a wide variety of sample environments For users primarily doing liquid work, wanting easy access or easy flow-thru.

Sample Stage X-Z JJ X-Ray Standard Stage (80 mm x 80 mm), room for large cells X-Z-theta JJ X-Ray Standard Stage + 360 degree rotation 3-,4-,5- or 6-axis JJ X-Ray Custom Stages

Sample Viewer Double Camera JJ X-Ray Allows viewing the sample from the side and above Det. Positioning Stage 3 axis linear - Long travel JJ X-Ray Sample-Detector Distance 50-1550 mm for Qmin=2E-3 Å-1

3 axis linear - Medium travel JJ X-Ray Sample-Detector Distance 50-650 mm for Qmin=8E-3Å-1 Detector Pilatus 100K Dectris Size 83.8 x 33.5 x mm2

Pilatus 200K Dectris Size 83.8 x 70.0 x mm2 Pilatus 200K Dectris Size 83.8 x 106.5 x mm2

Beam stops near detector

Round (any size). Insertable JJ X-Ray For Pinhole collimation, exchangeable by motor Square, Insertable JJ X-Ray For Square aperture collimation, exchangeable by motor

Vacuum Pump System High Volume Rotary Vane Pump with booster

Edwards

Good Rapid Vacuum achievement

Instrument Server High end multicore server JJ X-Ray Handles both instrument control, data reduction and real-time data analysis

Instrument Control Client Any PC (Windows or Linux) JJ X-Ray Data Reduction Software SAXSGUI JJ X-Ray/Rigaku Data Analysis Software SAXSGUI and others JJ X-Ray Sample Standards Silver Behenate, Glassy Carbon JJ X-Ray For SAXS

Turkey Tendon JJ X-Ray For low-q SAXS Corundum JJ X-Ray For WAXS

Instrument table Also holds all electronics JJ X-Ray/Bosch Component Description Original

Manufacturer Comment

Optional Sample stages Ambient Multiple Holder Plate JJ X-Ray Standard Plate Thermostated Capillary Holder JJ X-Ray -30 to 120 C, holder for 6 refillable capillaries Thermostated Sandwich Holder JJ X-Ray -30 to 120 C ; holds 15 Samples sandwiched between foils High Performance Thermal Linkam -190 C to 300 C Shear Cell Linkam Stress/Strain Cell Linkam Liquid Flow Cell JJ X-Ray DSC Liquid Autosampler Anton Paar

Optional Components 4th Pinhole/Apert. (micro-beam) JJ X-Ray Ideal for SAXS mapping with microbeams

Instrument Overview 4

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Table of Generic GANESHA Configurations

Component Options/Description Basic-

Teaching Basic

Research μbeam

Scanner Bio -

SAXS & solution

Seeding & Crystal-

lization

High-End Multi-

Application

X-ray Source Sealed Tube (Cu or Mo)

Genix 3D (Cu or Mo) ( ) ( ) ( ) ( ) Micromax 002+ (Cu) ( ) 007HF (Cu or Mo)

Absorption filter Several filter thicknesses Collimation 4 Round Pinholes

Square Slit-formed Apertures Sample Chamber In Air

Large, Evacuated Small, Evacuated

( )

( )

( )

( )

( )

Sample Stage X-Z

X-Z-theta

3-,4-,5- or 6-axis Sample Viewer Double Camera Det. Positioning Stage 3 axis linear - Long travel

3 axis linear - Medium travel Detector Pilatus 100K

Pilatus 200K Pilatus 300K

Beam stops near detector

Round (any size). Insertable

Square, Insertable Vacuum Pump System High Volume Rotary Vane Pump Instrument Server High end multicore server Instrument Control Client Any PC (Windows or Linux) Data Reduction Software SAXSGUI Data Analysis Software SAXSGUI and others Sample Standards Silver Behenate, Glassy Carbon

Turkey Tendon

Corundum Instrument table Also holds all electronics

Component Description Basic-

Teaching Basic

Research μbeam

Scanner Bio -

SAXS & solution

Seeding & Crystal-

lization

High-End Multi-

Application

Optional Sample stages Ambient Multiple Holder Plate

Thermostated Capillary Holder  

Thermostated Sandwich Holder

High Performance Thermal

Shear Cell

Stress/Strain Cell Liquid Flow Cell

Optional Components 4th Pinhole/Apert. (micro-beam)

Generic Configurations 5

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Instrument Server

The heart of instrument is the instrument server, which handles the execution of the sample measurement. Physically it is a powerful multicore server that is capable of:

• Communicating with the various instrument components such as o the hardware directly controlling the detector o the source and shutter hardware o the motion controller for

various pinholes stages and insertable items sample stage

• Broadcasting the images of the sample • Storing and retrieving data • Receiving instructions from a remote client

The control and communication is built on a SPEC backbone, drawing on years of synchrotron experience in instrument control.

The Instrument Control Client (ICC)

The Instrument Control Client (ICC) is the “remote” human interface to the Instrument server. It is a graphical user interface that runs on either a windows or linux computer different from the instrument server. The ICC requires only a good internet connection and a good graphics card. The ICC allows:

o Interactive Control of Instrument components, such as Shutter on/off Stages motion/sample alignment Measurement: Start/Stop/Save/Continue Setting measurement modes Providing background information on samples

o Script based control of Instrument components, such as All of the interactive commands Multiple Sample Measurements Sample parameter Scans (position, temperature etc)

o Results Display, such as Scan Plots 2D Detector Data Averages of 2D data (Radial, Azimuthal, Slice etc) Live image of sample

Instrument Control 6

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Given the almost complete automation of SAXSLAB’s GANESHA and the wide range of scattering angles that the detector can collect (at various distances from the detector), we have had the opportunity to rethink how we do SAXS experiments in the laboratory. As a result we have developed at least two new unique5 approaches to optimizing the performance of the SAXS system.

Automatic Multiconfigurational Measurements

Conventional SAXS systems all have the possibility of manually setting the instrument up in different configurations to obtain different combinations of q-range and intensity. Sometimes this is done by moving the detector closer or further away from the sample. And sometimes it even entails changing the aperture sizes. Some users will even combine the data from these different settings. All conventional systems have this possibility, but in practice research groups rarely make these changes regularly since in the long run they are considered troublesome. Being fully motorized, the act of changing configuration with the GANESHA is a simple instruction to the instrument server, both a simple single change or a schedule of measurements in multiple configurations without human intervention. Both the ICC and the data-reduction software handle the automated multi-configurational measurements

Asymmetric Beam stop positioning for low-q data taking

For very high end systems one can consider three rectangular apertures for collimation, where the aperture size can be set to from 0 to 7 mm in increments of ½ microns. The number of combinations of pinhole configurations therefore borders infinite. To each pinhole configuration, there is one ideal beam stop size. Unfortunately, we do not have an infinite number of beamstops automatically available to us…so at first glance we cannot make use of the vast number of aperture configurations. However, we have come up with a scheme that requires only a few beam stops, and still allows for an infinite number of aperture configurations. We have termed the scheme “Asymmetric Beamstop”

5 At least unique among commercially available SAXS cameras

Measurement Philosophy 7

Perfect match of direct beam (purple), parasitic scatter (textured) and beam stop (black)

Beam stop is too large for finer collimation (with smaller direct beam and scattering). Potential low-q region not accessible.

By placing the beam stop (black) asymmetrically, the low q region is accessible to the right and to the top.

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This white paper has described the essentials of SAXSLAB’s GANESHA system, both in terms of functionality, components and options. Due to the broad range of applications in SAXS as well as user’s continued developing needs and often limited resources, the GANESHA has been built on a platform concept, which allows users to construct the best possible instrument meeting both their needs, skills, and size of purse, by combining various components. Given the wide range of final configurations, it is therefore impossible to provide general “instrument” specifications for the SAXSLAB GANESHA in this document. Such specifications are very particular to the exact choice of components and will therefore be provided at the same time as a particular quotation is provided. Nevertheless given that all variants of the instrument have the following features:

o Large motion of the detector allowing the gathering of both SAXS and WAXS data o Complete motorization o Complete In-vacuum operations o High degree of user friendliness allowing non-specialist to operate the system as well as

reduce and analyze the data.

we look forward to providing this instrument to the ever-developing community of SAXS users.

Conclusion 8