10

Applied Chemicals and Materials

INTRODUCTION

The Material Measurement Laboratory’s (MML’s) Applied Chemicals and Materials Division (ACMD), located in Boulder, Colorado, “characterizes the properties and structures of industrially important fluids and materials.” Its work “provides a diverse stakeholder community with innovative measurements and models and critically evaluated data, leading to improved processes and better products, as well as new and improved standards.” ¹ The ACMD is organized into the following five groups:

• Fatigue and Fracture Group
• Fluid Characterization Group
• Nanoscale Reliability Group
• Thermodynamics Research Center Group
• Thermophysical Properties of Fluids Group

The division chief and four of the five group leaders are new in their positions with the same group structure as in 2017, so it is presumed that the organization is in a state of flux.

Many of the individual projects in these groups are organized for either historical or administrative convenience, in contrast with unifying technical or methodological themes based on the MML mission statement. The division covers a number of long-standing “curator” functions such as the Charpy Verification Program and the REFPROP (Reference Fluid Thermodynamic and Transport Properties) database, which are central to the NIST mission but which dilute the scientific resources needed to maintain leadership in new areas of measurement science.

The ACMD covers all states of matter (gases, liquids, and solids, excepting only plasmas), crosscutting with many industries. As such, the programs are extremely broad. Nearly every project reviewed would fit well into another of the MML divisions, if the Boulder personnel were co-located with the Gaithersburg personnel. Even the title of ACMD covers everything from the applied (curator or legacy) programs through all states of matter be it chemical, biological, or materials. This was also evident in the organization of the presentations, which did not follow the group structure of the division.

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¹ John Perkins, NIST, 2020, “Applied Chemicals and Materials Division: Overview and Introduction,” presentation to the panel, September 9.

ASSESSMENT OF TECHNICAL PROGRAMS

Accomplishments

One third of the projects are of excellent quality with high-risk/high-impact potential following the recommendations of the 2017 review of the MML.² Two notable examples include improved measurement strategies to obtain more accurate thermophysical material properties and cannabis vapor detection.

Other programs are of excellent or good quality but might maintain focus more on the mission statement of the MML. Database (standard reference data or “SRD”) and standard reference material (SRM) activities are mission critical but use resources that limit activities in high risk programs. ACMD must extract full value from clients using these SRMs and databases to free up scientific resources for new projects.

The ACMD has a long history of excellence in thermodynamics of fluids and thermophysical properties. This tradition is maintained in several very strong programs. These seek to use advanced computational and laboratory measurement techniques to make major advances in the accuracy of thermodynamic data. The calculation and measurement of enthalpies of formation are fundamental to nearly all fields of chemistry and materials, as this information contains the strength of the chemical bonds between atoms in these ever more complex molecules. Traditionally the best thermochemical measurements were accurate to no better than 5 percent, but the advanced computational (quantum chemical) and measurement (NMR) methodologies being developed by ACMD are achieving accuracies of 2 percent. This will open new avenues in computational materials science that have yet to be imagined.

Worldwide, there are only a handful of examples of new materials being designed computationally prior to being discovered experimentally in the laboratory. With more accurate thermophysical data, the ability to computationally design new materials prior to synthesizing the material in the laboratory will provide breakthrough methodologies in materials design and remove the empiricism that has ruled the past 100 years. Greater accuracy in thermophysical calculations and measurements will be one of the great scientific accomplishments of the first half of the 21st century. NIST’s AMCD is leading the way in establishing both new computational methods and unique experimental methods that exceed the accuracy of past methods. The computational methods open pathways that are not available experimentally for many new materials.

In the area of vapor science for forensics and public safety, development of a breath-analyzer for Cannabis involves 8 orders of magnitude greater sensitivity than current alcohol breath-analyzers. This requires a multi-prong methodology involving unproven techniques. This project started as a NIST internal program that has expanded to U.S. Department of Justice funding because of the national need. Initial results show promise of meeting the aggressive high-risk goals.

Challenges and Opportunities

Some ACMD programs are “legacy” in nature (low risk, high monetary value) that utilize headcount and resources to maintain, for example, Charpy standards (SRM) and REFPROP (SRD).

High-risk programs that explore new methodologies to obtain legacy SRM properties would improve the technical program portfolio and add to the high-risk portfolio. There is a conundrum in that a successful high-risk project would eliminate a significant source of funding from the legacy SRMs. But to ignore the opportunity means someone else will take away the legacy program with a new less invasive

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² National Academies of Sciences, Engineering, and Medicine (NASEM), 2017, An Assessment of the National Institute of Standards and Technology Material Measurement Laboratory: Fiscal Year 2017, Washington, DC: The National Academies Press.

methodology. It would be better for ACMD to lead in improving on this demonstrated national need rather than have another country take the standard away from the United States.

Adding additional experimental methods (e.g., microwave or other electromagnetic measurements for evaluating thermodynamic properties) is an area for which the MML has extensive expertise and can add to the methods being employed in ACMD.

The area of additive manufacturing is high profile, but the MML work, both within ACMD and in other divisions, appears disjointed and is not focused on the MML mission statement.

A number of ACMD projects utilize the outstanding capabilities of NIST in making precision measurements, but the individual projects appear to be driven by client needs rather than fulfilling the MML mission. Attempts must be made to coordinate client needs with the MML mission; otherwise, ACMD risks becoming a high-class service laboratory rather than a leader in measurement technologies.

Improved Accuracy of Thermophysical Data

While NIST and a few other laboratories are making progress in obtaining more accurate thermophysical data, the challenge is to communicate the availability of these new methodologies and the potential uses of such information in advancing new materials design. NIST can do this by hosting or encouraging workshops that highlight the new methodologies with examples where the greater accuracy can make a difference and improve time to market for new materials.

Vapor Science for Forensics and Public Safety

This is a high-risk project but one for which NIST researchers are highly qualified. Challenges include working on regulated substances; ability to administer a multi-year program with only year-to-year funding, especially with 2-year postdocs.

PORTFOLIO OF SCIENTIFIC EXPERTISE

Accomplishments

Since the time of the 2017 report,³ ACMD has realized a budget growth of 18 percent from $16.8 million to $19.9 million with the majority of growth coming from services ($1.1 million) and agency interactions ($1.9 million). ACMD has used this funding to support significant scientific expertise.

The ACMD, with 58 scientists (an increase of 7 or 14 percent from the 2017 reporting period), has demonstrated impressive productivity in scientific publications, standards interactions, intellectual property activity, and customer engagement. As noted previously, publication frequency is averaging over 1.3 articles per year per scientist. Of significance is ACMD personnel participation in 44 standards committees with leadership positions in 16 of these committees. It is critical that NIST and ACMD remain in the forefront of these standards committees to better initiate, evaluate, and maintain the strategies for industry standards that impact U.S. manufacturing needs.

Customer engagement is viewed as a key metric for ACMD. ACMD is active in multiple customer interactions where the customer is industry within the United States in the form of either cooperative research and development agreements (CRADAs) or non-disclosure agreements (NDAs). In particular, the NDA approach is a proven path to commercialization of NIST intellectual activities.

Scientific expertise is also viewed from the perspective of initiating new and likely high-risk projects. Two ACMD programs that demonstrated this perspective were vapor forensics for cannabis

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³ Ibid.

detection and advanced NMR strategies or microwave strategies for the determination of thermodynamic properties of materials.

Opportunities and Challenges

Interaction and/or collaboration between the two main NIST sites (Gaithersburg and Boulder) was not emphasized in the ACMD presentations. Formalizing such interactions would be beneficial to the ACMD goals.

One source of acquiring talent for ACMD is a continued and more aggressive effort in sponsoring positions for the National Research Council (NRC) Research Associateship Program (RAP). This is one of the most efficient ways of initiating new and high-risk programs.

As noted, the growth of associate positions in the ACMD was unusually high during this last 3-year period (from 16 to 29 persons, or an 81 percent increase). Three of the associates are paid to work for NIST full time. Most of the remaining 26 are external collaborators. Since many of these positions are subject to renewal on a 2-year cycle, ACMD must establish a plan to retain or renew talent to sustain existing programs and/or create new programs.

ADEQUACY OF FACILITIES, EQUIPMENT, AND HUMAN RESOURCES

Accomplishments

There have been no major new facilities in the Boulder Campus or at least none were described during the review. The major concern repeated numerous times was the housing in 50-year old laboratories. This may be a concern, but it is beyond the charge of the panel review.

The Nanoscale Reliability Group within ACMD noted the “aging” of key characterization equipment, including the following: focused ion beam (FIB) sample preparation tool; transmission electron microscope (TEM); and field emission scanning electron microscope/electron backscatter diffraction microscope. A capital equipment replacement plan for these critical tools was not presented.

Over the last 3-year review period, ACMD showed total staff growth of 23 percent (76 to 94) with number of scientists increasing 14 percent (51 to 58) and number of associates increasing 81 percent (16 to 29). The growth rate for associates appears unusually high when compared to the MML total number of associates actually decreasing by 6 percent (919 to 858).

Opportunities and Challenges

The ACMD dependence on a significant increase in associate staff for new programs may lead to potential program continuity issues as the tenure for short-term employees ends. It was apparent that tenure prospects have not been adequately conveyed to associates. ACMD may not succeed in sustaining additional program growth through reliance on increases in future associates. As associates complete their terms, new programs will need to be initiated and old programs ended.

If capital equipment replacement for aging tools is mission critical, then this might best be accompanied by a priority list provided to higher organizational management. ACMD noted potential equipment sources from the U.S. government surplus listings.

RECOMMENDATION 10-1: The Applied Chemicals and Materials Division should create a capital equipment replacement plan that considers also the requirements for space and ongoing maintenance.

DISSEMINATION OF OUTPUTS

Accomplishments

The ACMD has done a good job of disseminating its output in several different ways. The ACMD personnel publish substantially in the open literature, with 222 papers in archival journals, 26 in conference proceedings, 18 book chapters, and 20 reports from April 2017 to August 2020. This amounts to a journal publication rate of 1.3 papers per researcher per year; this is about average in comparison with other research facilities, including universities and national laboratories. The ACMD staff members actively participate in seminars, workshops, and conference presentations with over 102 invited presentations in the last 3 years. The ACMD has worked closely with a variety of agencies, such as the American Society for Testing and Materials (ASTM), the International Organization for Standardization (ISO), and the American National Standards Institute (ANSI), in developing standards. As noted, the staff participates in as many as 44 standards committees with several staff members assuming leadership positions on these committees.

The ACMD does an excellent job of disseminating its output in the traditional area. Dissemination of output by the Thermodynamics Research Center is excellent. The Fatigue and Fracture Group disseminates its work through its influence on codes and standards for testing and designing with structural materials. There are several favorable examples of programs driven by stakeholder needs, most notably the Charpy Impact Machine Verification Program and the Thermophysical Properties of Fluids. The Charpy Impact Machine Verification Program serves over 1,200 manufacturers and users worldwide, whose Charpy Testing Machines are being certified by the ACMD for compliance with ASTM and ISO standards, and is an excellent example of monitoring stakeholder use of outputs through SRMs. It has remained the leading NIST SRM year after year with worldwide impact. The ACMD’s thermodynamic and chemical property data sets assist stakeholders and, in some cases, are an enabler of commercial process-modeling software. The ACMD validates the impact of its work through database (SRDs) access and SRMs sales; there were 17 SRM/RM activities and 14 SRD activities in the division. One example for the impact validation of the SRD programs is the REFPROP (Reference Fluid Thermodynamic and Transport Properties) equation of state engine with 1,423 annual licenses.

The ACMD has been awarded 10 patents with 18 additional invention disclosures and patent applications over the past 3 years.

Overall, the ACMD does an excellent job of disseminating its output to all stakeholders.

Opportunities and Challenges

ACMD has created significant impact with key SRDs and SRMs. The challenge for ACMD is to properly value their SRD/SRM portfolio so that new programs can be initiated, in particular programs that explore new solutions to legacy SRM strategies.

While the ACMD is making progress in obtaining more accurate thermophysical data, the challenge is to communicate the availability of these new methodologies and the potential uses of such information in advancing new materials design. MML and the ACMD in particular can do this by hosting or encouraging workshops that highlight the new methodologies with examples where the greater accuracy can make a difference and improve time to market for new materials.

Overall, the ACMD does an excellent job of disseminating the outputs of its technical work. One way ACMD could improve its dissemination would be through establishing an exchange program between ACMD personnel and organizations in industry, universities, and national laboratories—both to and from ACMD. Universities and other organizations have benefited from these kinds of exchange programs in facilitating and expanding dissemination and the enhancement of staff.

CONCLUSIONS AND RECOMMENDATIONS

ACMD has SRD and SRM activities that utilize personnel resources to maintain legacy standards. Initiating new programs to examine replacement or improvement strategies for these standards activities would position ACMD at the forefront of the next generation of standards requirements. Properly valuing the SRD and SRM activities would create revenue to support such activities.

RECOMMENDATION 10-2: The Applied Chemicals and Materials Division should take steps to realize the true value of standard reference data and standard reference materials thereby enabling revenue for growth of new programs.

Over the past 15-20 years, NIST’s MML has evolved from a Materials Science and Engineering focused research laboratory to become the nation’s premier material measurement laboratory specializing in precision measurement methodologies and standards, supporting industry in the chemical, biological, and materials fields. ACMD has the same breadth of industries as does the larger MML, with an outstanding history of precision chemical, thermodynamic, and mechanical property measurements. Virtually all of the projects within ACMD fit within the competencies of divisions housed in Gaithersburg, yet it is not clear that the interaction between these two physically distant laboratories are as close as they might be in an era where virtual discussion is becoming the norm.

RECOMMENDATION 10-3: MML should (1) clearly define the Applied Chemicals and Materials Division’s (ACMD’s) mission and how ACMD aligns within the Material Measurement Laboratory mission; and (2) integrate teams more closely with corresponding efforts in NIST Gaithersburg facilities.

High-risk project activity is one measure of the technical vitality of an organization. High-risk projects include—for example, vapor forensics for public safety and NMR and microwave techniques for thermodynamic property characterization.

RECOMMENDATION 10-4: The Applied Chemicals and Materials Division should continue to increase the number of high-risk projects.