2

Applied Chemicals and Materials

INTRODUCTION

The National Institute of Standards and Technology (NIST) Boulder campus houses 76 staff members and associates from the Material Measurement Laboratory (MML) Applied Chemicals and Materials Division (ACMD). The division operations occupy multiple locations across the site, with its primary concentration in two buildings.

The personnel at the ACMD characterize the properties and structures of industrially important fluids and materials. Their materials research efforts include the development of fundamental techniques, measurements, and models for analysis of materials structure and reliability. Their fluids research focuses on the characterization of complex mixtures and thermophysical properties. The division was recently reorganized to better align functions with their programmatic plans. Activities of the division are now conducted within the division office and with five research groups.

The division office provides administration and oversight for the division’s personnel and resource allocations. The Thermodynamics Research Center compiles and critically evaluates thermophysical and thermochemical data and disseminates this information through a variety of software channels. The Fatigue and Fracture Group provides standard reference materials (SRMs), calibration and measurement services, property data, and predictive models to ensure materials reliability against fatigue and fracture—especially for structural applications (e.g., buildings, bridges, pipelines, and medical devices). The Nanoscale Reliability Group develops and disseminates scientific information, standards, and technology for high-resolution measurements of material structure, chemistry, and physical properties, in order to ensure reliability of materials and devices with critical dimensions in the micrometer to nanometer regime.¹ The Fluid Characterization Group performs experimental research geared toward understanding how the composition of fluids—especially complex fluids—relates to chemical and physical properties, with the goal of property calculation from composition.

The Thermophysical Properties of Fluids Group performs experimental, theoretical, correlative, and molecular simulation research on the thermodynamic and transport properties of fluids and fluid mixtures over wide ranges of temperature, pressure, and composition,² including regions of fluid-fluid and fluid-solid phase equilibria.

___________________

¹ NIST, Nanoscale Reliability Group, https://www.nist.gov/mml/acmd/nanoscale-reliability-group, accessed September 25, 2017.

² NIST, Thermophysical Properties of Fluids Group, https://www.nist.gov/mml/acmd/thermophysical-properties-fluids-group, accessed September 25, 2017.

ASSESSMENT OF TECHNICAL PROGRAMS

Accomplishments

The ACMD has effectively started the process of refining its focus to align itself to the new (2015) strategic plan and 5-year program plan. That process was undertaken in response to the last National Academies Assessment in 2014. An example of further establishing this alignment is its exit from antibiotic testing by resonance methods, with a good plan for technology transfer to maximize the initial investment in this work. Although that effort was showing signs of success, it was clearly outside the scope of the division.

The following illuminates several examples of outstanding accomplishments in the ACMD groups. The Nanoscale Reliability Group’s innovative research is developing techniques to expand the capabilities of scanning electron microscopes through the development of a method for detecting transmitted electrons, which has resulted in unprecedented levels of angular selectivity during transmission imaging. The technology transfer effort, through patents associated with this research activity, seems to be supporting the dissemination of the results to industry. The atom probe effort is a high-risk project that has promise to provide a unique measurement technology for atomic-level chemical identification of a wide range of materials, from liquids (by cryogenic methods) to solids.

The Thermophysical Properties of Fluids Group has strong and rare expertise, which needs to be preserved. Their ability to measure the thermodynamic properties of fluids (gas and liquid) to a very high precision, as well as the coupling of this effort to the equation of state modeling for vapor-liquid equilibrium, is of essential value.

Certain fluid mixtures, such as crude oil and many of the fuels that arise from it, are not readily characterized by the tools used for pure fluids. The ability of the Fluid Characterization Group to describe the properties of such materials, particularly their vapor pressure and solubility characteristics, is essential for fluids validation. The group has also impacted forensic science through the remarkable development of the porous layer open tubular cryoadsorption (PLOT-cryo) method, and its portable version.

The Thermodynamics Research Center Group is dedicated to data and information accumulation and qualification efforts, historically more in the area of fluids, with initial inroads into metals. Their research relates to the Materials Genome Initiative (MGI). A number of methods to input and qualify vast amounts of data are under development.

The Reference Fluid Thermodynamic and Transport Properties Database (REFPROP) standard reference data (SRD) is an essential component of the process simulators utilized globally by industry and has relevance to such areas as climate modeling. The application of the tools to the screening of millions of compounds for low-global warming potential (low-GWP) refrigerants is an excellent example.

The Charpy Impact Machine Verification Program in the Fatigue and Fracture Group provides a very good example of a mature SRM program that is run very effectively. The importance of that effort to industrial quality control of structural materials cannot be overstated and needs to be maintained. The group is making an interesting effort to expand the capabilities of the test. This program is an exceptional example of the close connections that the ACMD has to industry. In addition, the measurement of fracture toughness in high-pressure hydrogen environments to study embrittlement of steels provides a one-of-a-kind capability/facility. The techniques that are being developed allow an order of magnitude more samples to be tested than other approaches.

Opportunities and Challenges

The opportunities in the ACMD are extensive—for example, the Nanoscale Reliability Group’s efforts to design very high speed atomic force microscopy (AFM) capabilities are high risk with equally high potential rewards. The Thermophysical Properties of Fluids Group has some exquisitely accurate and precise measurement techniques. One opportunity might be to dramatically increase the speed of some of

those techniques while minimizing the trade-off in lost precision on their results. Such an effort could lead to the development of new instrumentation useful to industry. The PLOT-cryo effort within the Fluid Characterization Group could yield products in the very near future.

There appear to be groups in various divisions that are related in such a way that they might benefit from being within the same division—one example is the MML research in mechanical properties of solid materials. There are programs in the Materials Measurement Science Division (MMSD) that are also closely related to those in the ACMD. Some parts of the AFM effort in the Fatigue and Fracture Group and an effort concerning nanoindentation could be considered technologies that are related, but at different stages of maturity.

It is not clear what formal programs exist to encourage collaboration between groups in different divisions working on related projects. Each division needs to encourage collaborations between divisions.

The programs in the ACMD are well thought out and are starting to fit together as the division refines its focus. Some opportunities within the division, such as those in the Fatigue Fracture Group, are associated with finding research efforts that fit with the mature efforts in the group to allow a full spectrum of projects—from mature to high-risk. Expanding the efforts to have projects at various stages of development, from high-risk research to mature support programs, would further increase the cohesion in the division. There are diverse interests within the division, and focusing efforts has been a priority since the 2014 National Academies Assessment, with notable progress.

PORTFOLIO OF SCIENTIFIC EXPERTISE

Accomplishments

The scientific staff has many accomplishments of which it can be proud. There are significant accomplishments yielding both external and internal awards. These include the first ever American Gas Association award and a Presidential Early Career Award for Scientists and Engineers (PECASE). Many products of the division are extremely important to a number of stakeholders. The division members are active in standards efforts, as well as publishing a significant number of articles in domain-appropriate peer-reviewed journals, including one article in Nature Communications.

Retaining excellent personnel in research areas of high interest at the national and international level (such as in the electron microscopy effort and the AFM effort) can be challenging. While government pay scales are not always competitive, the division seems to have a high retention rate, even in such areas of keen technical interest. This speaks well of the ACMD efforts to promote an attractive combination of work environment and compensation.

The ACMD personnel publish substantially in the open literature, as demonstrated by the links to the Google Scholar sites from the online personnel biographies that are readily available. Publishing is one avenue to monitor stakeholder interest, and the citation rates associated with many of the ACMD personnel are very high. Additionally, ACMD staff members actively participate in seminars, workshops, and conference presentations.

Opportunities and Challenges

One general challenge is the acquisition of specialized personnel to support mature programs in technical areas that are not currently considered high interest at many educational institutions. Simply finding personnel with excellent measurement expertise in any area of research is becoming difficult. Clearly, the division effectively generates new hire opportunities through the National Research Council (NRC) Associateship Program and industrial exchange programs.

The exchange of expertise and examples of collaboration between the two main sites (Gaithersburg, Maryland, and Boulder, Colorado) are somewhat isolated. It appears that the exchange program between

the Gaithersburg site and the Boulder site could be expanded with positive impact on the level of interaction between the sites. A formalization of that effort in an exchange or a sabbatical-type program could be useful. The physical aspects of an exchange process are important as well. Everything from designated office space and on-site housing could have an impact on the success of the exchange program.

The staff in this division is excellent and compares favorably with the staff at other national laboratories. This division is heavily reliant on the retention of personnel from the National Research Council Associateship Program for permanent employees—this cooperation needs to be maintained and encouraged. A concerted effort to nominate staff for external awards could be an effective means to increase the profile of individuals as well as the laboratory itself.

ADEQUACY OF FACILITIES, EQUIPMENT, AND HUMAN RESOURCES

Accomplishments

The combination of facilities available in the ACMD is quite unique. The scientific equipment within the ACMD facilities seems adequate for the mission in most cases, with some pointed exceptions regarding beyond life, critical equipment in the Fluid Characterization Group and the Thermophysical Properties of Fluids Group.

Opportunities and Challenges

There are some improvements in the building facilities since the 2014 National Academies Assessment; however, there are still significant issues. The management seems well aware of these issues and is making progress toward solving the problems; still, continued efforts are needed. Additionally, there are clear frustrations with some of the NIST administrative processes among the ACMD scientific staff. These frustrations were noted in the last report. Specifically, the purchasing process and legal assistance with contracts seems to still be a problem. Additional personnel have been hired to address purchasing process issues, which appears to have resulted in a significant reduction of the problem. Further training of the new administrative personnel associated with the purchasing problem, along with joint meetings between the scientific staff and the new personnel to brainstorm solutions to this issue seems to be in order. There are also some indications of insufficient technician assistance. There may be opportunities associated with further leveraging the uniqueness of the combination of expertise and equipment available in the division. Encouraging groups to extend beyond their comfort zone with regard to maturation of their technology focus may yield positive results. For instance, it may be worthwhile to look for additional new areas of research closely associated with the work being performed by the Fatigue and Fracture Group. In addition, it may be important to look for opportunities to develop standards associated with the Nanoscale Reliability Group’s work.

One challenge is the maintenance expenses associated with some of the new equipment. This is an issue at most high-technology laboratories. It is clear that additional help from management with that problem is very important. Some equipment associated with best-in-the-world measurement expertise that has been developed over a significant time frame is clearly at or beyond its expected life.

In general, the facilities and scientific staff are adequate to support the mission of the division. Structural inclusion of maintenance fees in the budget when high-performance equipment is purchased would be helpful.

DISSEMINATION OF OUTPUTS

Accomplishments

As mentioned above, the ACMD personnel publish substantially in the open literature, with 282 archival journal publications, 69 conference proceedings, 24 NIST reports, and 37 books and chapters. This is one avenue to monitor stakeholder interest. ACMD staff members actively participate in seminars, workshops, and conference presentations. The ACMD has worked closely with a variety of agencies, such as with the American Society for Testing and Materials (ASTM), in developing standards. The staff participates in many other standards committees as well—with at least 10 staff members assuming leadership positions on these committees.

There are several favorable examples of programs driven by stakeholder needs that were discussed above—these include the Charpy Impact Machine Verification Program and the Thermophysical Properties of Fluids. A program for which there is significant anticipated stakeholder need is the hydrogen embrittlement testing using the unique high-pressure facilities for fracture toughness testing. The Charpy Impact Machine Verification Program serves over 1000 stakeholders, whose Charpy Testing Machines are being certified by the ACMD, and is an excellent example of monitoring stakeholder use of outputs through SRMs.

The technology transfer office at NIST is available to assist with patent applications and personnel. This suggests that the office has been effective. The ACMD has been awarded 4 patents (and 6 patents pending) over the past 3 years. NIST does not receive financial compensation for patents and stakeholder activity surrounding the patents generated by the ACMD. These patents are monitored by contacts of NIST. NIST chemical property data sets expand capabilities, and in some cases may be an essential enabler of commercial process modeling software available to 45,000 corporate customers and widely taught in chemical engineering academic curricula. Sometimes, a NIST patent is licensed for no fee so that the company associated with technology transfer is protected. One such technology transfer has been pursued to help to efficiently wind down a live bacteria detection program that was outside the identified mission areas of the ACMD.

One novel program, the NIST Science and Technology Entrepreneurship Program (N-STEP) is available and already utilized for entrepreneurial efforts by personnel and serves to transfer NIST activities to the general stakeholder community.

Opportunities and Challenges

Overall, the ACMD does an excellent job of disseminating the outputs of its technical work. One way to possibly facilitate and expand dissemination to more organizations, laboratories, and industries is through establishing an exchange program. Such an exchange program would be between ACMD personnel and other organizations in industry, universities, and national laboratories. These exchanges could be both to and from the ACMD. Making convenient and economic living space available for these exchanges would be valuable, particularly because the cost of housing in the Boulder area is very high. Other organizations, such as universities, have found these kinds of exchange programs very valuable in terms of facilitating and expanding dissemination and the enhancement of staff.