Attachment 1 - SOW NB6460502501860 Raman microscope1.pdf

STATEMENT OF WORK

Raman Microscope

A. BACKGROUND INFORMATION

The Chemical Sciences Division is involved in a project seeking to deliver a testbed for heterogeneous catalysts based on emerging X-ray characterization methods as a key component of a current NIST Innovations in Measurement Science (IMS) project. IMS projects are competitively chosen for their potential for high impact on a scientific, engineering, and/or technological challenge that benefits society.

They impact stakeholders at NIST, industry, commercial labs, other federal agencies, or academia. The results promise to transform existing scientific, engineering, and/or technological knowledge to enable future capabilities for NIST and significantly advance NIST’s mission. In particular, these capabilities are being commissioned at NIST’s X-ray facilities at the National Synchrotron Light Source II in Upton, NY and involve the integration of a NIST-built detector to enable a first-of-kind measurement approach.

In support of these efforts, the Raman microscope will be used to validate the performance of custom reaction cells being development for use in the ultrahigh vacuum chamber. These cells are being tested in Gaithersburg using an ultrahigh vacuum chamber that is a replica of the equipment at the X-ray facility.

The Raman microscope will also provide complementary data on catalysts at industrially relevant reaction conditions. Moreover, as a benchtop technique, Raman microscopy will provide a key reference point relating data from NIST’s testbed to conventional techniques being applied to the materials under study at other internal and external facilities. In short, the Raman capabilities described below will play a key role in validating and benchmarking the capabilities under development as well as standardizing the reaction data that will be collected.

B. SCOPE OF WORK

The Contractor shall provide one (1) Raman microscope system that meets the following minimum technical requirements. Key attributes include an objective turret with a range of optics available for confocal measurements that reject certain background signals, portability requirements so that it can be used in the Gaithersburg laboratory or integrated into beamline measurements at the X-ray facility in NY, the ability to integrate with in situ reaction cells, and the ability to couple to an ultrahigh vacuum chamber. The Contractor shall deliver and install the instrument, demonstrate performance characteristics meeting requirements, and provide training.

C. SPECIFICATIONS

1. Performance Requirements:

a) Spectral resolution better than 2.5 cm-1 for the 405 nm and 532 nm wavelengths.

b) Include a solid state 405 nm laser with at least 30 mW power.

c) Include a solid state 532 nm laser with at least 50 mW power.

d) Enable at least 1 mW control over each laser power via software control.

e) Include at least one holographic grating with at least 1800 lines/mm and the spectrograph must possess a focal length of at least 200 mm.

f) Use appropriate Rayleigh filters for each laser. For the 405 nm laser, this will allow measurement of the Raman spectrum from at least 100 cm-1 to 3500 cm-1. For the 532 nm laser, this will allow measurement of the Raman spectrum from at least 50 cm-1 to 3500 cm-1.

g) Back-illuminated CCD array detector with at least 1024 x 256 pixels. This detector shall be Peltier-cooled to -70 °C without requiring water or liquid nitrogen. The CCD shall have a peak quantum efficiency over 90 % and a rapid readout capable of greater than 1000 spectra per second.

h) Allow for stepwise scanning of the grating synchronized to the CCD readout such that the Raman spectrum from the entire spectral range can be acquired without artefacts from stitching together large spectral regions collected back-to-back.

i) An objective turret which can include up to at least 5 objectives. The Contractor shall provide at least three objectives. One objective shall have a magnification of 5x and shall have a long working distance (greater than 15 mm) and an numerical aperture (NA) of at least

0.1. The second, shall be a 20x objective with working distance and NA of approximately

3.5 mm and 0.4, respectively. Third, a long-working distance objective at high magnification is needed. This shall have magnification, working distance, and NA of approximately 50x, 8 mm, and 0.5, respectively. Empty locations on the turret shall have blank caps.

j) The instrument shall include a calibration source such as a neon lamp and silicon.

2. Sample Integration Requirements:

a) The objective turret must permit scanning microscopy studies of a sample via motorized travel in the X, Y, and Z directions (with Z being the direction of the sample). This turret must be compatible with both the 405 nm laser and the 532 nm laser.

b) The range of motion in each direction shall be at least 50 mm with a minimum step size of 100 nm or less and the motors must use an encoder.

c) Flexibility is needed for sampling different catalyst environments in situ. As such, the microscope must be capable of incorporating at least a foot of free space underneath it and six inches to either side to accommodate different reaction cells. Similarly, the instrument must have capabilities for sampling cells from a vertical or horizontal orientation. In Section H, cell examples are provided to illustrate the required optical orientations.

d) In order to facilitate alignment, the system must also include white light illumination of the sample along with video imaging and a routine for auto-focusing.

3. Ultrahigh Vacuum Integration Requirements:

a) The Raman instrument shall also couple to an ultrahigh vacuum chamber.

b) The integration solution shall couple onto a 4.5” conflat flange.

c) The integration solution shall not compromise the 10-9 Torr base pressure of the chamber.

d) The integration solution shall be able to focus the laser to the center of the chamber, which is

6” from the flange. See Section H for an illustration of the vacuum chamber and an example cell the Raman microscope must probe.

e) The 532 nm laser shall be coupled to the integration solution with a fiber optic cable at least 5 m in length. Appropriate Rayleigh filters as described above shall be implemented.

f) In order to provide confocal measurements, the fiber optic cable shall be integrated to an objective with a magnification of at least 20x and a working distance sufficient to allow at least 0.5” of vacuum in between any component of the integration solution and the reaction cell at the center of the vacuum chamber.

g) The fiber optic system shall include capabilities for white light illumination and video imaging.

h) If a window is used for the 532 nm laser to enter into the vacuum chamber, it shall be made of fused silica or similar material that does not interfere with the Raman signal and it shall have a sufficiently large aperture as to not obstruct the beam during motor motion as described below.

i) Motors shall be integrated with the integration solution that allows for movement of the laser with respect the reaction cell. The range of motion on these motors shall be at least 10 mm in the X and Y directions (parallel to the face of the cell) and at least 100 mm in the direction of the cell.

j) If a bellows is needed to achieve the above requirements, it shall be welded to the integration solution and the motors shall have sufficient torque to achieve the desired motion while the chamber is under vacuum.

4. Portability Requirements:

Given the need to synthesize information across multiple techniques and to collaborate across multiple geographical locations, it is necessary that the instrument facilitate some degree of portability. This means that travel-proof containers with foam or otherwise protective inserts must be provided to facilitate packing and relocation of the Raman microscope, including the spectrometer, at least one laser, motors, objective turret, and any fiber optic cables necessary for operation via government vehicle. Reassembly of the instrument at the end destination must be achievable within a few hours based on the training referenced later in this document.

5. Software Requirements:

a) The contractor will provide software for instrument control and data acquisition.

b) Software must allow for data analysis of spectra and display of images from the Raman microscope as well as white light images.

c) Software must automate the collection of line, depth, and area scans in XYZ direction.

d) In order to facilitate the rapid acquisition of spectra at high spatial resolution, the software must be able to perform encoded steps less than or equal to 100 nm in size.

e) The software must automate tracking of the surface to maintain focus of the sample through extended sampling or sampling across uneven surfaces.

f) The software must include a data analysis package including statistical tools such as least squares, principal component, and multivariate curve resolution analysis.

g) The software must allow for automated switching between between measurements involving the objective turret coupled to the XYZ stage and the laser coupled to the ultrahigh vacuum without any manual changes to the system performed by the user.

h) The software must allow for visualization of the measured Raman image such that physical viewing through an eyepiece is not required.

i) The software must facilitate the change from one laser to the other with no manual changes to the system performed by the user.

j) The software must also control the XYZ motors used to steer the laser in the ultrahigh vacuum chamber.

6. Installation:

The Contractor shall install the instrument in Building 221, Room B153, at NIST Gaithersburg, MD.

Installation shall include, at a minimum, uncrating/unpacking of all equipment, set-up and hook-up of all equipment, start-up, demonstration of specifications, and removal of all trash. Instrument will operate to manufacturer’s specifications upon installation. Installation will take place during normal business hours, between 8:30 am and 5:00 pm Eastern Time, Monday through Friday except Federal Holidays, and will be coordinated with the NIST Technical Point of Contact (TPOC). Installation is to occur within 180 days of award.

7. Warranty:

The Contractor shall provide, at a minimum, a one year warranty for the equipment. The warranty shall cover all parts, labor and travel. The warranty shall commence upon Government acceptance.

8. Training:

Include training at NIST for at least 2 NIST personnel covering normal operation, troubleshooting, and routine maintenance. Training must also cover breakdown/assembly using portability containers.

Training will be provided during normal business hours, between 8:30am and 5:00pm Eastern Time, Monday through Friday, except Federal Holidays, and will be coordinated with the NIST Technical Point of Contact (TPOC) to ensure maximum availability of NIST personnel. Training is to occur within 30 days of installation. The training may be completed on-site at NIST immediately after installation and demonstration of specifications.

D. DESIGN REVIEW

NIST requires a design review and government acceptance of the design before manufacturing/customization may commence. The Contractor shall provide design documents showing relevant interface and design elements required in the specifications to the Contracting Officer Representative (COR) and Technical Point of Contact (TPOC) within 45 calendar days from receipt of award. NIST will review to verify that the design appears workable and consistent with requirements.

NIST will provide comments or acceptance within 10 days of receipt. Iterations on the design may be required if the design is not acceptable. The NIST COR will notify the Contractor of government acceptance. Acceptance of the design does not make the government liable if any aspect does not function as expected or required; the Contractor retains full liability for the performance of the design and equipment provided.

E. DELIVERABLES:

Description Quantity Due Date Deliver to Format Design Review Documents

One (1) Within 45 calendar days from receipt of award

COR and TPOC Electronic

Raman microscope One (1) Within 180 calendar days from receipt of order

COR in NIST- Gaithersburg

Delivered on-site

Installation of instrument

Once Within 30 calendar days of delivery

Coordinate install with TPOC

Performed on-site

Training on the instrument

Once Within 30 calendar days of delivery

Coordinate training with TPOC

Performed on-site with NIST personnel

F. ACCEPTANCE CRITERIA

After installation, the Contractor shall demonstrate that all performance specifications are met and that the instrument is able to couple to the ultrahigh vacuum chamber in Gaithersburg.

G. GENERAL INFORMATION

1. Safety: The Contractor employee shall be responsible for knowing and complying with commercial installation safety regulations. Such regulations include, but are not limited to, general safety, fire prevention, and waste disposal.

2. Security: NIST is a restricted campus. An identification badge is required for access for entry into buildings and also is shown to the armed Security Police when entering the campus.

3. Identification Badges: Contractor employees shall comply with NIST identification and access requirements. The Contractor shall provide the name and citizenship information of employees for on-site visits to the NIST COR prior to arrival. The COR will submit the name(s) and citizenship information to the NIST Office of Security in order for a given Contractor employee to enter the NIST campus. The Contractor employee is responsible for absences due to missing or expired identification and access documents. Each Contractor employee shall wear a visible identification badge provided by the NIST Security Office.

4. Vehicle Registration: All Contractor employees must register their vehicles with the NIST

Security Office to gain access to the campus. A valid driver’s license, Government-furnished civilian ID (which in most cases can be a valid driver's license), proof of insurance and current registration must be presented to the NIST Security Office.

H. Sample Integration Requirements:

It is necessary to be able to measure samples from a “vertical” or “horizontal” orientation in air.

An example of each orientation is shown below.

Vertical Orientation

Fig. 1: (A) The Linkam CCR1000 reaction cell is shown on the left with the image taken from:

https://www.linkam.co.uk/ccr1000. (B) The Raman high temperature reaction chamber is shown on the right with the image taken from: https://harricksci.com/raman-high-temperature-reaction-chamber/.

Commentary: It is common for commercial cells to fill a bed with a catalyst in powder form. For in situ measurements with a Raman microscope, it is then necessary to make the measurement in a vertical orientation with the objective directly above the window.

Horizontal Orientation

Fig. 2: A tubular reactor is shown with the catalyst, a powder, loaded inside a thin-walled capillary. The cell is turned 45 degrees with respect to an incoming X-ray beam, which typically has dimensions of one millimiter in the vertical and a few millimeters in the horizontal, this beam is parallel to the ground. The X-rays hit the powder and either transmit through the sample or stimulate fluorescence which is measured by a detector to the left (at a 90 degree angle with respect to the incoming beam). The cell is approximately five inches tall and four inches wide (eight inches wide including gas connections – not shown).

Commentary: For a tubular reactor such as this one, it is convenient to perform measurements in a horizontal orientation. For example, by bringing the objective in from the back of the cell directly toward the viewer and using a long working distance to avoid blocking X-ray beam transmitted through the sample.

Ultrahigh Vacuum Integration Requirements:

Fig. 3: (A) The ultrahigh vacuum chamber in Gaithersburg is shown on the left. The CF flanges mentioned in the statement of work are on the upper level of flanges. (B) A picture inside the chamber at the NIST X-ray beamline is shown on the right. Note that the cells are positioned along the cylindical axis at the center of the chamber. Cells typically use a silicon nitride window with a 1 mm x 1 mm membrane.

Commentary: As many of the X-ray experiements are performed under ultrahigh vacuum, it is important that the Raman instrumentation also be capable of integrating with the vacuum chamber. The idea is that this would be accomplished with the 4.5” CF flanges around the top level. Note that the chamber itself stands roughly five feet above the ground, so a fiber optic cable needs some length to facilitate the experiment, as stated in the statement of work. Also, there are several detectors around the chamber on different ports, so it is useful for the integration strategy to bolt directly onto the CF flange in a compact manner. From there, it is a matter of steering the Raman system’s laser onto the membrane of the silicon nitride window which is typically 1 mm by 1 mm and at the center of the chamber. The catalyst is then just inside that window.