Spectroscopies and Microscopies of Interfaces

 AFM Bruker Bioscope Resolve

The BioScope Resolve offers the highest resolution atomic force microscopy imaging and most comprehensive cell mechanics capabilities available for use with a Leica DMi8 inverted optical microscope. It incorporates Bruker’s proprietary PeakForce Tapping technology to enable the highest resolution biological imaging and picoNewton-level force and spectroscopy measurements at each pixel. Real-time synchronization of optical microscopy and atomic force microscopy data opens the door to previously inaccessible data, including physical structure, biochemical interactions, and mechanical and physicochemical properties. This AFM allows the analysis of samples (organic, inorganic, cellular, etc.) in air, in organic solvent (hexane, isopropanol, ether, etc.) or in an aqueous medium with temperature control.

Leica DMi8 inverted optical microscope:

Leica DMi8 motorized stand
EL 6000 metal halide light source
Transmitted light condenser (LED, 0.3NA, WD = 70 mm)
3 objectives (20x, 40x, 60x magnification) with fluorescence cubes (DAPI, FITC, RHO)
Hamamatsu ORCA Camera, Hamamatsu Flash CMOS
Top View Optics camera (10x magnification, Up to 5MP, max frame rate 9 FPS)
AFM-Raman coupling module:

IRIS pack for AFM-TERS
Matchbox iO laser (532nm, 50mW)
Accessories :

BioScope Resolve EasyAlign
Micro-Volume cell (< 60µL) sealed around the AFM probe
Air & Fluid Cantilever holders with injection system
BioScope Resolve Scan Stage (XY 10mm x 10mm, Z<15µm)
2 temperature control modules (20 to 60°C and 20 to 200°C)


AFM Asylum (Oxford instruments) : MFP3D-Bio model

The MFP3D-BIO is one of the only bio-AFMs that makes no compromises on AFM imaging resolution, force measurement performance, or application versatility while integrating seamlessly with a range comprehensive range of optical techniques. The stability of the MFP3D-BIO allows it to measure forces of the order of picoNewton and to analyze the smallest characteristics of samples. The technology and design of the optical head eliminates non-linearities, off-axis movements and interference fringes. This AFM is mounted on an Olympus IX71 inverted optical microscope. Its custom-designed condenser enables standard optical microscopy modes, including phase contrast and fluorescence.

Olympus IX71 inverted optical microscope:

Olympus manual stand
Olympus TH4-200 halogen lamp
X-Cite 120Q metal halide light source
3 objectives (4x, 20x and 60x magnification) with fluorescence cubes (DAPI, FITC, RHO)
Olympus E3 digital SLR camera
Top View Optics Camera (10x magnification)
Accessories :

Environmental controller (temperature -20 to +120°C, humidity 0 to 95%)
MFP3D Scan Stage semi-motorized (XY 20mm x 20mm, Z<40µm)

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Scanning electronic Microscopy JEOL JSM-IT500HR + EDS

 

SEM JEOL JSM-IT 500 HR :

– Resolution under high vacuum: 1.5 nm (30 kV), 4.0 nm (1.0 kV).

– Resolution under low vacuum: 3.0 nm (15 kV).

– Magnification: ×5 to ×600,000 (for 128 mm × 96 mm image size).

– MEB-FEG acceleration voltage: 0.5 kV to 30 kV.

– Probe current: 1 pA to 20 nA; peak current up to 200µA.

– Maximum sample size: 200 mm diameter × 75 mm height.

EDS OXFORD Ultim Max 170 :

– Analytical resolution (mapping): 50 nm at 5kV

– Mn Kα resolution 127 eV at 130 000 cps

– F Kα resolution 64 eV at 130 000 cps

– C Kα resolution 56 eV at 130 000 cps

  SECM

 

SECM-103

  • SECM-103

  • Maximum scan range: 25 mm in 3 axes

  • Resolution with motor : 0.1 µm

  • Resolution with piezo : 1.5 nm

  • Equipped with PalmSens 4, potential ±10 V, current 100 pA – 250 mA, 18-bit resolution, EIS 10 µHz – 1 MHz

  • Coupling with Keithley 6430 sub-femtoamp remote source meter, EQCM (QCA917 quartz crystal analyzer)

  • Detection of contact of the probes by shear force with 7280 Lock-in Amplifier

 

SECM-109

  • Maximum scan range : 25 mm in X and Z, 150 mm in Y

  • Resolution with motor : 0.1 µm

  • Resolution with piezo : 4 nm (only in Z)

  • Equipped with potentiostat PalmSens 3, potential ±5 V, current 100 pA – 250 mA, 16-bit resolution.

  • Detection of contact of the probes by shear force with 7270 Lock-in Amplifier

 

Accessories :

  • Laser puller P-2000 for the fabrication of capillaries and the microelectrodes Polisher of microelectrodes HEKA MHK 1A

 

Infrared Absorption FTIR Spectrometer Nicolet 8700

 

Measurement range 15000-15 cm-1

Resolution up to 0.09 cm-1

NIR / MIR / FIR beamsplitter

DLATGS KBR / DLATGS PE detector

Liquid Nitrogen cooled MCT detector

Nitrogen purged optical path / Nitrogen purged sample compartment


FTIR Spectrometer Bruker 70V coupled with Hyperion microscope

 

Measurement range 12000-10 cm-1

Resolution better than 0.4 cm-1

Beamsplitter for NIR 15,000-1,200 cm-1 / MIR 8,000-350 cm-1 / Wide range MIR+FIR 6,000-10 cm-1

Wide range DLATGS detector 12,000-20 cm-1

Liquid Nitrogen cooled MCT detector 12000-600 cm-1

Vacuum optical path / Vacuum or Nitrogen purged sample compartment

Coupled with a HYPERION 2000 INFRARED MICROSCOPE from near to mid infrared

Reflection or transmission X16 and x32 objectives

MIR MCT detector cooled with liquid Nitrogen 12000-600cm-1

NIR InGaAs detector cooled with Peltier 12800-4000 cm-1

FTIR Spectrometer Bruker Tensor 27

 

Spectral range 8,000 to 340 cm-1

Resolution better than 0.9 cm-1

DLATGS detector

Common accessories associated with spectrometers:

 

  • Transmission measurements

    Diamond ATR (powder and liquid) / Germanium / ZnSe

    DRIFT

    IRRAS

    Specular reflection variable or fixed angle Sample environment control through dedicated cells (commercial (LINKAM …) or special design at the laboratory) with temperature regulation (from 93 to 1073 K) and/or controlled atmospheres (vacuum, N2 – relative humidity…)
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Cary 6000i Spectrophotometer

 

Double beam UV-Visible Near infrared spectrophotometer from 175 to 1800 nm with automatic source and detector change

Liquid or solid transmission Resolution of 0.01 nm Linear up to an absorbance of 6 Specular reflection at variable or fixed angle DRIFT

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Renishaw inVia Qontor Raman Spectrometer

 

Renishaw inVia Qontor confocal Raman microprobe (532 nm, 785 nm).

Low frequency measurements down to 10 cm-1 at 532 nm.

Maintain real-time focus with LiveTrack to acquire accurate, reproducible spectra and topography in real time from samples with significant height variations.

Control of the sample environment via dedicated cells (commercial (LINKAM . . .) or special production in the laboratory) with temperature regulation (from 93 to 1073 K) and/or under controlled atmospheres (vacuum, N2 – humidity relative…)

Jobin Yvon T64000 Raman Spectrometer

Liquid nitrogen cooled CCD detector with very high sensitivity.

Triple monochromator system (additive or subtractive) with 1800 rpm gratings.

Simple monochomator with EDGE filter with 1800 / 600 / 300 rpm networks.

Confocal microspectrometry (Olympus BX41 microscope).

Analysis of liquids in a macro chamber.

Excitation laser sources 488 nm, 457 nm, 514 nm, 632 nm, 532 nm, 561 nm, 672 nm.

Resolution up to 1 cm-1

Control of the sample environment via dedicated cells (commercial (LINKAM . . .) or special production in the laboratory) with temperature regulation (from 93 to 1073 K) and/or under controlled atmospheres (vacuum, N2 – humidity relative…)

Mössbauer spectroscopy @ low temperature

 

Refrigeration of the cryostat is produced as a compressed helium gas is expanded in the expander (Cold head) which is the part of the closed cycle cryogenic refrigerator. The expender is supplied helium gas from a helium compressor through a flexible hose. Following expansion, refrigeration is created according to the Gifford-McMahon cycle (expansion-compression). Through a second hose, the returns to the compressor to complete the closed loop. No helium is consumed in this process. A soft bellows for vibration isolation from cryostat maintaining the exchange gas circulation between the cold finger to the sample holder. The vacuum shroud as a lower part of the cryostat is equipped with optical windows in Be allowing irradiation and transmission analysis of cooled samples. The system allows to reach temperatures of about 6K in 2h30 of cooling and a vacuum of 10-8 Torr. A 50 ohms heating resistor (Thermofoil) allows regulation between 6 and 340 K and two Si diodes allow temperature measurement on and near the sample. The spectrometer unit described elsewhere in the service section for Mössbauer spectrometry operates in transmission geometry from a 57Co source mounted on a velocity transducer and a detection system using NaI (Tl) and an electronic chain.

Cell

The Dural cell with a beryllium window is transparent to gamma radiations from the MIMOS spectrometer and operates in a controlled atmosphere with inert gases. This cell is ideally suited to the use of Mössbauer spectrometry in backscattering mode. A wide range of samples sensitive to oxidation by atmospheric oxygen can be analysed

MIMOS

 

MIMOS II, developed by G. Klingelhöfer’s group at the University of Mainz, started the MER (Mars Exploration Rover) missions from 2004 and is a miniaturised spectrometer. Because of the complexity of sample preparation on the Martian surface, the choice was immediately made to use the reflection geometry, which is also known as “backscattering”. In this case, no sample preparation is required, the spectrometer is simply presented in front of the sample, which becomes an emitter because the source and detector are on the same side and the spectrum is recorded. The signal detected in backscattering corresponds to gamma, X or conversion electrons depending on the detection mode chosen and the escape area corresponding to these radiations. As in conventional spectrometers, the source is mounted on a Mössbauer drive allowing Doppler modulation of the emitted energy. The detector has 4 cross-mounted counters using 4 Si-PIN diodes for very good resolution and excellent efficiency for radiation between 6.4 and 14.4 keV at the expense of the gas counters used in other systems.

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XPS / UPS Spectrometer KRATOS AXIS Ultra DLD

 

Sources :

  • XPS: monochromatised Al; dual anode Mg (1253.6 eV), Al (1486.6 eV).

    UPS: He(I) (21.2 eV) and He(II) (40.8 eV).

    Analysed area: 300×700µm (hybrid mode); spot size 15 to 110 µm.

Hemispheric analyser radius 165 mm (Passing energy 5 to 160 eV).

Ar ion guns for etching (5 keV).

Electron guns for charge compensation (analysis of insulators).

Energy resolution:

  • XPS: FWHM Ag3d5/2: 0.45 eV.

    UPS: Resolution at Fermi Ag level: 0.12 eV.

    Analysis in angular (ARXPS).

Temperature analysis -150 to +600°C.

Glove box connected to the introduction chamber.

Vacuum < 5 10-9 mbar.

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