68-1045-22_1301025629 Specifications.pdf

Specifications for correlative micro-spectroscopy system

The Naval Research Laboratory has a requirement for a Visible to Far-infrared Fourier Transform Infrared Spectromicroscopy System (FTIRSm) that will be replacing a less capable Fourier Transform Infrared (FTIR) spectrometer (Bruker Tensor 37) that is coupled to an infrared microscope and already exists at NRL.

The system must consist of the following components and shall meet or exceed the following minimum specifications.

Visible to Far-infrared Fourier Transform Infrared Spectromicroscopy System S1. The FTIRSm System shall consist of all mechanical, optical, data-acquisition, data-analysis, and data-visualization components necessary to perform Reflection, transmission and emission measurements over the spectral range of 15-25000 cm-1 with a spectral resolution equal to or better than 0.9 cm-1 on samples with lateral dimensions of 3mm x 3mm within an environment purged with dry nitrogen gas. To cover the specified spectral range, the FTIRSm System shall include the following components

a. The FTIRSm system shall simultaneously hold three room-temperature detectors and one liquid-nitrogen-cooled detector, and have the ability to optically and electronically switch between them via software control and motorized actuators (see S4). The FTIRSm shall include the following detectors

i. The FTIRSm shall include a wide-range DLaTGS detector capable of covering the spectral range of 20 – 12000 cm-1

ii. The FTIRSm shall include a liquid-Nitrogen-cooled mercury cadmium telluride (MCT) detector covering the spectral range of 600 – 12000 cm-1 with a detectivity (D*) greater than 2 x 1010 cm Hz1/2/W and liquid nitrogen hold time greater than 8 hours

iii. The FTIRSm shall include a liquid-Nitrogen-cooled indium antimonide (InSb) detector covering the spectral range of 1850 – 10000 cm-1 with a detectivity (D*) greater than 1.5 x 1011 cm Hz1/2/W, and liquid nitrogen hold time greater than 8 hours

iv. The FTIRSm shall include a room temperature Indium Gallium Arsenide (InGaAs) detector covering the spectral range of 4000 – 12800 cm-1 with a noise equivalent power of less than 5 x 1012 W/Hz1/2

v. The FTIRSm shall include a room temperature silicon detector covering the spectral range of 9000 – 25000 cm-1 with a noise equivalent power less than 1 x 1014 W/Hz1/2

vi. External transfer optics and electronics (coupled in through BNC)

b. The FTIRSm shall include beamsplitters to fully cover the spectral range of 15 – 25000 cm-1 and shall include a storage compartment for these beamsplitters. The FTIRSm shall include the following beamsplitters:

i. The FTIRSm shall include a quartz beamsplitter covering the spectral range of 3500 – 28,000 cm-1

ii. The FTIRSm shall include a KBr beamsplitter covering the spectral range of 350 – 8000 cm-1

iii. The FTIRSm shall include a wide range beamsplitter covering the spectral range of 6000 – 10 cm-1

c. The FTIRSm shall include the following light sources to cover the spectral range of 40 – 25000 cm-1:

i. The FTIRSm shall include a visible/NIR tungsten lamp light source with an output power of at least 150 W, covering the spectral range of 4000-25000 cm-1. The source shall include the required power supply to power the lamp.

ii. The FTIRSm shall include a mid-infrared source covering the spectral range of 40-4000 cm-1

iii. The FTIRSm shall include an optical input port allowing the user to use a user-specified light source with the system. The input port shall direct the light into the interferometer for modulation and then either into the sample compartment or microscope to interact with a user-supplied sample – as selected by the user within the software interface.

d. The FTIRSm shall also include the following characteristics

i. The spectrometer shall use aluminum-coated mirrors to allow spectral coverage throughout the infrared, visible, and ultraviolet spectral regimes of 15 – 25000 cm-1

ii. The spectrometer shall include a software-controlled aperture wheel with at least 12 different aperture sizes that will serve to reduce the intensity of both internal and external light sources.

iii. The spectrometer shall consist of mounted CaF2, KBr, and CsI windows that are interchangeable and can be installed within the output and input ports of the spectrometer.

S2. The FTIRSm shall include a dry-nitrogen-gas-purged compartment for measuring sample transmission and reflection. The sample compartment shall include the following components:

a. The Sample compartment shall contain a quick-release mounting mechanism that allows different measurement accessories to be placed, latched, and automatically aligned with the optical beam path in the system. This quick-release mechanism shall accept the following accessories that will be included with the FTIRSm:

i. The FTIRSm shall include a removable mount for holding samples vertically to perform transmission measurements on samples. This holder shall be automatically aligned with the optical beam path when it is mounted within the spectrometer sample compartment

ii. The FTIRSm shall include a removable jig for measuring sample reflectance with a 10-degree angle of incidence. This holder shall be automatically aligned with the optical beam path when it is mounted within the spectrometer sample compartment. The jig shall include sample masks that will limit the sample measurement area to 3/8”, 1/2”, and 2” diameter areas. This jig shall also include a reference mirror calibrated for the infrared spectral regime.

S3. The FTIRSm shall include an all-reflective, broadband microscope capable of carrying out infrared transmission, reflection, and emission measurements on microscale samples with lateral dimensions in the range of 5x5 microns to 300 x 300 microns. The microscope system shall be docked on a reconfigurable output (for reflection/transmission) and input (for emission) port of the main spectrometer such that it can utilize the light sources, transfer optics, and optical interferometer/beamsplitters outlined in specifications S1c, S1d, S1b. In addition, the microscope system shall include the following items/characteristics:

a. The FTIRSm microscope shall include the following optical elements

i. The microscope shall include binoculars with an adjustable eyepiece to view the sample and inspect the sample focus

ii. The microscope shall include a visible camera viewport that includes a high-resolution visible camera with a resolution of at least 5 Megapixels

iii. The microscope shall include reflective optical elements to route infrared light through the microscopes. The mirrors employed within this system shall be aluminum coated, allowing reflection, transmission, or emission measurements to be performed over the spectral range of 15 – 25000 cm-1. The position of these mirrors shall be user selectable within the software outlined in specification S4.

iv. The microscope shall contain optics necessary to perform IR measurements while simultaneously observing the sample in reflection mode

v. The microscope shall contain a pair of transparent apertures within the image plane that will allow spectral measurements of regions within a subarea of the microscope's visible field of view. The size and angular orientation of these apertures shall be continuously variable from over the range of 5-300 microns and 0-360 degrees.

vi. The microscope shall contain filter slots that allow for the insertion of a visible and/or infrared polarizer and analyzer to be inserted within the infrared optical path before the sample and after the sample, respectively.

vii. The microscope system shall include the following polarization filters that will be used with the filter slot specified in S3a.vi:

1. Visible polarizing filter covering the spectral range of 440 – 800 nm with transmission greater than 32% and a polarization contrast greater than 1000:1

2. ZnSe Mid-infrared, wire-grid polarizing filter covering the spectral range of 600 – 4000 cm-1 with an extinction ratio greater than 300 at the frequency 1000 cm-1

viii. The microscope system shall include the following polarization filters that will be used with the analyzer slot specified in S3a.vi:

1. Visible polarizing filter covering the spectral range of 440 – 800 nm with transmission greater than 32% and a polarization contrast greater than 1000:1

2. ZnSe Mid-infrared, wire-grid polarizing filter covering the spectral range of 600 – 4000 cm-1 with an extinction ratio greater than 300 at the frequency 1000 cm-1

b. Detectors

i. The microscope shall simultaneously hold two liquid-nitrogen-cooled detectors, and the detector used in the optical path shall be selectable via a motorized, computer-controlled mirror that the user can control within the instrument software, as specified in specification S4.

ii. The microscope shall include a liquid-nitrogen-cooled mercury cadmium telluride (MCT) detector covering the spectral range of 600 – 10000 cm-1 and shall have an 8-hour liquid nitrogen hold time. The detector shall be mounted in a mechanism that allows the user to easily remove and reinstall the detector with the detector department of the microscope.

iii. The microscope shall include a liquid-nitrogen-cooled mercury cadmium telluride (MCT) detector covering the spectral range of 450 – 10000 cm-1 with a detectivity (D*) greater than 5 x 109 cm Hz1/2/W and shall have an 8-hour liquid nitrogen hold time. The detector shall be mounted in a mechanism that allows the user to easily remove and reinstall the detector with the detector department of the microscope.

iv. The microscope shall include a silicon detector covering the spectral range of 9500-25000 cm-1 with a noise equivalent power less than 1x1014 W/Hz1/2.

v. The microscope shall include an electronic interface for the microscope detector analog to digital converter that is accessible to user such that the user can supply their own external detector for the microscope when the detector compartment covers and detectors are removed.

c. Microscope objectives

i. The microscope shall include a microscope objective turret capable of holding at least 4 objectives.

ii. The microscope shall include a low-magnification (less than 5x) visible-glass objective that can be used for visualizing the sample through either the binoculars or microscope camera

iii. The microscope shall include a 15x magnification, all-reflective, Cassegrain objective for both visualizing the sample through the binoculars/camera and collecting reflectance, transmission, or emission spectra from the sample.

iv. The microscope shall include a 15x magnification, all-reflective, Cassegrain objective as the condenser for illuminating the sample on the microscope stage in transmission mode.

v. The microscope shall include an infrared 3.5x objective for infrared imaging and spectra collection with a spectral range of 770 – 5000 cm-1, working distance of greater than 30 mm, and a numerical aperture of less than or equal to 0.15.

d. Mapping stage with automated focus assembly

i. The microscope shall include a motorized XYZ mapping and imaging stage that allows for automating reflectance, transmission and emission measurements with the microscope.

ii. The XY motorized stage shall have a lateral movement range of at least 75 mm x 50 mm with a step size less than or equal to 0.1 microns and a repeatability of less than 1 micron.

iii. The Z motorized stage shall allow automated focus control with an adjustment accuracy of 0.1 microns.

iv. The motorized stage shall be controlled by an XYZ joystick controller S4. The FTIRSm shall include software that allows the user control the instrumentation and perform measurements. More specifically, the software shall contain the following characteristics:

a. The software shall allow the user to configure the measurement mode and system settings - automatically adjusting the systems’ optical path depending on the mode selected and settings selected.

b. The software shall include a command entry mode that allows the user to specify the state of an each mirror actuator within the microscope.

c. The software shall acquire reflection, transmission, and emission spectra. The software acquisition shall be capable of acquiring and averaging up to 1000 spectra within a single measurement. In addition, the acquisition software shall allow the user to performed timed, repeated measurements where the user specifies the delay between measurements and the total number of measurements to be performed.

d. The software shall visualize acquired reflection transmission and emission spectra and provide user with the abilities to zoom, pan, filter, and normalize spectra.

e. The software shall include diagnostic tools that notify the user of lifetime limits for consumables such as light sources and the interferometer laser. The software shall also include validation tools that will allow the user to track the system performance over time.

f. The software shall include the ability to run, create, and edit macros and Visual Basic scripts for automating measurements .

g. The software shall include Labview Virtual Instruments for controlling the software. The LabView Virtual Instruments shall allow the user to configure the measurement mode and settings of the FTIRSm system and shall allow the user to execute measurements from within the LabView programming environment. The LabView Virtual Instruments shall be compatible with existing LabView 2018 codes that have already been written at NRL to automate measurements performed with a Bruker Tensor 37 spectrometer and microscope.

h. The software shall provide tools for processing reflection, transmission and emission spectra, including abilities to perform averaging, normalization, baseline correction, and derivative calculations on reflection, transmission, and emission spectra.

i. The software shall include the ability to perform automated line, area, and irregular mapping of sample transmission, reflection, and emission.

S5. The FTIRSm system shall include a step scan mode that allows spectra to be obtained by running the interferometer in a step-wise fashion. The step scan system shall include an electronic trigger box with BNC electrical connections that allows the user to provide external electronics to control and monitor the interferometer stepping and trigger measurements.

S6. The FTIRSm system shall include a computer system and monitor for running the software specified in S4. The computer system shall have the following characteristics

a. The computer shall have an Intel i7 processor with a clock rate of 3 GHz or better

b. The computer shall have at least 16 GB of RAM

c. The computer shall have a solid state drive with at least 256 GB of storage for storing the operating system and software

d. The computer shall have a secondary hard drive with at least 1 TB of storage for storing data

e. The computer shall have the Windows 10 Enterprise Operating System Installed.

Installation and Training The price of the Visible to Far-infrared Fourier Transform Infrared Spectromicroscopy (FTIRSm) system must include delivery of the instrument to the U.S. Naval Research Laboratory in Washington, DC; installation; demonstration; and training.

The on-site installation should be carried out by a qualified engineer. The installation should include an on-site validation of specified performance and training of the final users at the Naval Research Laboratory.

Training shall include a hands-on tutorial for that ensures NRL personnel are proficient in operating the all modes of operation of the FTIRSm system.

Documentation and Warranty

a. A full set of all written documentation customarily provided to the public with a commercial item shall be provided. This shall include user manual(s) or equivalent as well as copies of any software, and any manuals for the software included with the system, if customarily provided. This documentation should be received by NRL with the system hardware unless other arrangements are agreed to by the authorized Government representative. In addition to the above documentation, which is customarily provided.

b. The contractor shall offer the Government at least the same warranty terms, including offers of extended warranties, offered to the general public in customary commercial practice. These warranty terms must be included in the system price. The period of the warranty shall begin upon acceptance.