Labs & Facilities

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NEW!!! software to book PSCM equipment here

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The Soft Matter Facility is intended as a structure where samples to be used on soft matter instruments can be prepared and characterised before use with neutron and synchrotron radiation techniques. Once the laboratories will be transferred in the new Science Building (spring 2013) the facility will also represent a place for meetings and exchange for the Soft Matter Communities of ILL & ESRF (including both members of staff and users). Besides a number of laboratories it will comprise space for a seminar room, offices for students, post-docs and scientists on sabbatical (see plan below).

At the moment, laboratories are being set-up both at the ILL and ESRF to host pieces of equipment that will eventually move to the new building.

List of pieces of equipment already available in the Soft Matter Laboratories (up-dated in may 2011):

Quartz Crystal Microbalance
Portable Raman Spectrometer
Kruss Contact Angle
ALV Static and Dynamic Light scattering
Beaglehole Ellipsometer for liquids
Ellipsometer for solids
Nanofilm Brewster Angle Microscope
Light microscopes
Polarizing microscope
Rheometers
Micro Differential Scanning Calorimeter
Optical Tweezers
AFM (@ESRF)
Spin-coater
Freeze-dryer
Tensiometer
Langmuir troughs
Tip sonicator

Users who wish to use these pieces of equipment in conjunction with a neutron or synchrotron radiation experiment related to Soft Matter, should contact Giovanna Fragneto: fragneto(at)ill.eu

ALV CGS-3 STATIC & DYNAMIC LIGHT SCATTERING

The ALV CGS-3 Compact Goniometer System (ALV GmbH, Langen, FRG) allows for a simultaneous measurement of static and dynamic light scattering. The temperature can be set between 5°C and 50°C.

Static light scattering (SLS) measures the form factor in the angular range of 17° and 152° (equivalent to Qmax ≈ 0.00255 Ǻ-1, depending on solvent index of refraction) and provides the following parameters:

A2 in mol L/g²   Second osmotic virial coefficient (solvent – solute interaction parameter)
RG in nm         Radius of gyration
MW in g/mol      Mass averaged molecular weight

Dynamic light scattering (DLS) measures the fluctuation in the scattered light with an ALV7004/FAST real time multiple tau digital Correlator with 3.125 ns as initial and shortest sampling time, thus allowing sub-nm particle characterization. Parameters obtained are:

D in m/s²   Translational diffusion coefficient
RH in nm      Hydrodynamic effective radius, acc. To Stokes – Einstein equation
PDI   Polydispersity index MW/MN, from cumulant analysis acc. To Koppel
kD in cm³/g Analogouos to A2 of SLS

Combining these techniques yields a supplementary information, the structure sensitive parameter ρ (ρ = RG/RH). It allows for an (overall) shape characterization of particles (e. g. sphere, rod, coil etc.).

Responsible: Ralf Schweins

: Fig. 1: ALV CGS-3 SLS / DLS instrument. The instrument is fully encapsulated and falls in laser class 1.

: Fig. 2: View on the laser beam illuminating a sample (cf. arrow) in the thermostatted toluene bath.

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BEAGLEHOLE PICOMETER LIGHT ELLIPSOMETER

Ellipsometry is an optical technique that measures the change in polarisation of light reflected at an interface. The complex ratio of the reflectivities for p- and s-polarised waves may be related to the dielectric structure of the interface through optical modelling. A simple relationship exists between the optical parameters for isotropic films at the air/liquid interface, and any deviations to the predicted behaviour can highlight the existence of a more complex interfacial structure or the presence of surface aggregates.

A Beaglehole Picometer Light ellipsometer is available in the PSCM, and is optimised for interfacial characterisation at the air/liquid and air/solid interfaces. The interfacial excess can be determined to a precision and sensitivity of < 5% of a surfactant monolayer, and with complementary information or optical modelling the data can be used to quantify the adsorbed amount of material at an interface. Data can be acquired at a rate of up to 200 Hz, hence the instrument provides access to the study of fast adsorption kinetics.

The ellipsometer offers two principal benefits to ILL users. First, it can be used as a pre-screening tool to characterise the kinetics and homogeneity of samples before neutron reflectometry (NR) beam time on FIGARO. Also, the interfacial excess of surface-active material may be compared precisely with respect to a changing variable such as solution composition or temperature. Second, the technique has greater sensitivity to species with a similar scattering length density to that of air (e.g. hydrogenated polymers). Therefore the acquisition of an ‘optical contrast’ during NR measurements can reduce the need for as many NR isotopic contrasts thus saving beam time and deuterated chemicals. Kinetic information may be quantified to complement further the neutron reflectometry data, and inhomogeneity in free liquid surfaces can be identified prior to the modelling of NR data.

Responsible: Richard Campbell

QUARTZ CRYSTAL MICROBALANCE

The QCM is a mass sensing device with the ability to measure very small masses changes on a quartz crystal resonator in real time. It is possible to measure mass changes as small as a fraction of monolayer or single layer of atoms. As the second generation of Quartz Crystal Microbalance with Dissipation monitoring (QCM-D) from Q-Sense, the E4 offers the opportunity to study molecular interactions and molecular adsorption to many different types of surfaces. Applications include proteins, lipids, polyelectrolytes, polymers and cells/bacteria interacting with surfaces or with previously bound molecular layers.

The instrument determines the mass of very thin surface bound layers and simultaneously gives information about their structural (viscoelastic) properties. It is based on the patented QCM-D technique, an extremely sensitive and fast technique providing multi-frequency and dissipation data that are needed to fully understand the state of molecular layers bound to the sensor surface.

- Software name Q-Tools

- Number of sensors 4, also possible to measure using only 1, 2 or 3 sensors

- Volume above each sensor ~ 40 μl using Q-Sense Flow Module for 5 MHz crystals

- Minimum sample volume ~ 200 μl

- Working temperature 18 to 45 °C, controlled via the software, stability ± 0.02 K

- Flow rates 0-1 ml/min

- Sensor crystals* 5 MHz, 14 mm diameter, polished, AT-cut, gold electrodes

Responsible: Yuri Gerelli

NANOFILM BREWSTER ANGLE MICROSCOPE

The BAM utilizes the fact that when p-polarized light is guided towards an air-water interface, no reflection occurs at a certain incident angle. This angle, the Brewster angle, is determined by Snell´s law and depends on the refractive indices of the materials in the system. The Brewster angle for the air-water interface is 53°, and under this condition the image of a pure water surface appears black. Addition of material to the air-water interface modifies the local refractive index (RI), and hence, a small amount of light is reflected and displayed within the image. The image displayed contains areas of varying brightness determined by the particular molecules and packing densities across the sampling area.

• The water surface is irradiated with p-polarised light. The refraction of the beam is determined by Snell's law.

• Reflected light occurs at an angle equal to the incident angle.

• At a certain angle of incidence, the Brewster Angle, the transmitted and expected reflected paths are perpendicular. Under this condition reflection is not possible. The image of the water surface appears black.

• Addition of material to the surface modifies the local refractive index and hence the angle of refraction such that the transmitted and reflected beams are no longer perpendicular.

• A small amount of light is reflected and displayed within the image. An image is built up from pixels of varying brightness determined by the particular molecules and packing densities across the sampling area.

Lateral resolution ≥1μm

Responsible: Robert Barker

LANGMUIR TROUGHS

Langmuir troughs used for the preparation of layers on solid substrates from insoluble amphiphilic molecules, typically lipids but also polymers and proteins.

LANGMUIR TROUGH NIMA 611

Trough surface 300x200 mm²

1 barrier

Dipper and well at one end

Dimensions well: 63x180 mm² 70mm deep

Temperature control

Pressure sensor uses a Wilhelmy plate (chromatography paper of wet perimeter 20.6mm weight 80mg/m²)

Manual and automatic system for Langmuir-Schaefer deposition optimized for 50mm wide squared substrates

LANGMUIR TROUGH NIMA 1212D

Trough surface 680x200 mm²

2 barriers (can move independently)

Dipper and well at center

Dimensions well: 90x110 mm² 85mm deep

Temperature control

Pressure sensor uses a Wilhelmy plate (chromatography paper of wet perimeter 20.6mm weight 80mg/m²)

Manual and automatic system for Langmuir-Schaefer deposition optimized for 50mm wide squared substrates

The trough is enclosed in a laminar flow fume-hood

Responsible: Giovanna Fragneto

DIFFERENTIAL SCANNING CALORIMETERS

The Micro DSCIII has a very low detection limit: calorimetric signals of less than one Microwatt can be detected. The cells are made of Hastelloy C, have a volume of approximately 1 cm3 and are readily removed and easily cleaned.

T range = 5 to 90°C, atmospheric pressure

Programmable temperature scanning rate (heating and cooling): 0.001 to 1.2°C/min

DSC 131

Crucibles designed to ensure good thermal transfer between the sample and the sensor – Alumina, Aluminum (30 and 100 μl).

T range = -120 to 700°C, atmospheric pressure, air or inert gas

Programmable temperature scanning rate (heating and cooling): 0.1 to 100°C/min

Responsible: Isabelle Grillo

TENSIOMETER

KRÜSS K11 TENSIOMETER

Fully automatic determination of surface and interfacial tension for routine measurements in laboratory and quality control applications

Measuring methods:

- Ring method (Du Noüy; correction acc. To Huh&Mason, Harkins&Jordan; Zuidema&Waters)

- Plate method (Wilhelmy)

Temperature range: 5 to 90°C

Measuring range: SFT / IFT 1 to 999 mN/m, Density: 1 to 2200 kg/m3

Responsibles: Isabelle Grillo and Richard Campbell

KRUSS CONTACT ANGLE

MODEL DSA14, KRÜSS:

The drops are generated with a reproducibility of 0.3 microliter and placed on the sample at the touch of a finger. Software-controlled contact angle measurement can start immediately after drop placement – without any further actions being required. With image recording rates of up to 61fps even rapid changes in the contact angle can be recorded.

Measuring range : 1 – 180°

Angle resolution : 0.1°C

Camera: Monochrome interline CCD, 780 x 580 pxl, 61fps

Environmental chamber : -10 - 90°C

Responsible: Marco MaccarinI

SPIN COATER

Delta6 RC Spin Coater from SUSS MicroTec used to coat solid substrates with polymer or lipid films.

Adaptors available for squared and round substrates of 50mm diameter (or 50x50mm² surface) or rectangular (80x50mm² surface).

Chuck rotation 0-10,000 rpm depending on size (please, check instructions before use).