5-Year Reauthorization Report for the Applied Chemical

5-Year Reauthorization Report for the Applied Chemical & Morphological

Analysis Laboratory

ACMAL is managed by the Department of Materials Science and Engineering

October 25, 2019

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Table of Contents

Abstract ..................................................................................................................................... 3

Purpose...................................................................................................................................... 4

Mission Statement..................................................................................................................... 4

ACMAL Footprint ....................................................................................................................... 4

Equipment or Instrumentation .................................................................................................. 5

Operational Summary ............................................................................................................... 6

Use fee history ........................................................................................................................... 7

Shared Facility Users and Supported Research ........................................................................ 11

Staff Wages Funding Sources ................................................................................................... 13

Scholarly Activities .................................................................................................................. 14

Equipment Maintenance ......................................................................................................... 14

Safety ....................................................................................................................................... 18

Financial Reporting .................................................................................................................. 18

Strategic Plan ........................................................................................................................... 20

Concluding Comments ............................................................................................................. 21

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Abstract This document is the application for renewal of the ACMAL Shared Facility status. The report draws on information presented in previous Annual Reports. The Applied Chemical and Morphological Analysis Laboratory (ACMAL) is a University-recognized Shared Facility research instrumentation laboratory that houses high-end materials characterization equipment, including electron microscopes and X-ray equipment, along with numerous specimen preparation tools. ACMAL was established in 2003 and recognized as a Shared Facility in 2014. Operational costs of the equipment are recouped through hourly use fees. Equipment use is encouraged by maintaining a service organization mind set and offering training to faculty and students in the most flexible way. ACMAL is staffed by professional staff, and we minimize labor costs by employing undergraduate and part-time lab assistants. Expenses are also reduced by choosing the lowest cost maintenance and repair schemes that make sense for each tool. Identifying a need and the necessity to look into the future to ensure that the right mix of instruments are offered are constant challenges. As new research tools are purchased, ACMAL serves as a key resource to pinpoint the required infrastructure for successful operation. The equipment managed by ACMAL as more than doubled since 2014 from 5 instruments to 11 in 2019. ACMAL is dedicated to offering high-end research instrumentation capabilities for the lowest cost, ensuring users are well trained, and faculty receives value for the fees paid. As such, it is proposed that the ACMAL Shared Facility status be extended.

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Purpose

The Applied Chemical and Morphological Analysis Laboratory is a major research instrumentation facility available to the university community and managed by the Department of Materials Science & Engineering. ACMAL instrument operating costs are offset by use fees charged to all facility clients. We provide outstanding training to all clients to prepare them to effectively utilize the equipment in a safe and productive manner. Our focus is providing value to the researcher for use fees they pay that ultimately supports ACMAL equipment.

Mission Statement

ACMAL is a University Shared Facility service organization committed to providing access to major research instrumentation, outstanding training, and value to Michigan Tech faculty, students and corporate clients.

ACMAL Footprint

The primary ACMAL facility is located on the 6th and 7th floors of the Minerals and Materials Engineering Building (M&M), a satellite lab housing the Laser Scanning Confocal Microscope (LSCM) in the sub-basement of the Chemical Sciences & Engineering Building (Chem Sci), and a new low noise lab at the Advanced Technology Development Complex (ATDC). Sample preparation equipment is located in M&M 637, 617, Chem Sci S012 and ATDC 149 and 150. ACMAL occupies 8200 sq ft in the M&M, Chem Sci and ATDC buildings. Most ACMAL instrument labs consist of a separate outer room for mounting specimens with the inner room housing the instrument itself.

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Equipment or Instrumentation

ACMAL houses all of Michigan Tech’s major electron optical and x-ray characterization instrumentation including: Electron Optics Instrumentation

• JEOL 6400 Scanning Electron Microscope/Microprobe (SEM) with 4pi Energy and Wavelength Dispersive Spectrometers (EDS)

• JEOL 2010 Transmission Electron Microscope (TEM) with 4pi Energy Dispersive Spectrometer (EDS) and 2K High Speed Camera

• Hitachi S4700 Field Emission Scanning Electron Microscope (FESEM) with 4pi Energy Dispersive Spectrometer (EDS)

• Hitachi FB2000A Focused Ion Beam Milling System (FIB) with NPGS Pattern Generation System

• FEI XL40 Environmental Scanning Electron Microscope (ESEM) with Oxford Energy Dispersive Spectrometer (EDS) and Electron Backscatter Diffraction system (EBSD)

• Olympus FV1000 Laser Scanning Confocal Microscope (LSCM) • FEI Scanning Transmission Electron Microscope (S-TEM) with FEI Energy Dispersive

Spectrometers (EDS), Gatan EELS + GIF and 16MP Camera (New in 2017) • Perkin Elmer 5800 X-ray Photoelectron Spectrometer (XPS) (New in 2017) • Asylum Research MFP-3D Origin+ Atomic Force Microscope (New in 2018) • Veeco Atomic Force Microscope (AFM) • Perkin Elmer Phi 660 Auger Electron Microprobe • iMicro Nanoindenter (New in 2019)

Ancillary Specimen Preparation Equipment - Electron Optics

• Cressington 208HR High Resolution Iridium Sputter Coater • Anatech USA Hummer 6.2 Plasma Etch Unit • Denton Carbon Evaporator (2 units) • Leica Critical Point Dryer • Leica Ultramicrotome with cryogenic attachment • JEOL CP Cross Section Ion Polisher

X-Ray Characterization Instrumentation

• Scintag XDS2000 X-Ray Powder Diffractometer (XRD) /Graphite Monochrometer (2 units)

• Scintag X2 X-Ray Powder Diffractometer (XRD) /Solid State Detector • Scintag XDS2000 X-ray Pole Figure Diffractometer (XRD) • Xenemetrics X-Ray Fluorescence Spectrometer (XRF)

Ancillary Specimen Preparation Equipment – X-ray Diffraction

• Ball Mills • Hydraulic Pellet Press • Electropolisher

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Operational Summary ACMAL Staffing

The ACMAL professional staff includes MSE staff Mr. Jerry Anzalone, Dr. Edward Laitila, Dr. Tim Leftwich, Mr. Owen Mills, Dr. Pinaki Mukherjee, and Chemistry staff Mr. Jerry Lutz. Their salary distributions follow:

• Anzalone. Mr. Jerry Anzalone is a project funded employee whose wages are direct charged for work including lab instruction, sponsored and start-up projects. He charges the ESEM use fee index for maintenance and repair. Mr. Anzalone left the University on September 27, 2019.

• Laitila. 100% of Dr. Edward Laitila’s salary and fringes are charged to the MSE general fund. The MSE general fund receives 75% of Dr. Laitila’s salary as a component of its yearly budget.

• Leftwich. Dr. Timothy Leftwich is classified as a Research Assistant Professor. He direct charges his wages to XPS users.

• Mills. In FY19, 64% of Mr. Owen Mills’ salary and fringe were charged to the MSE general fund index. Seven percent was paid by the VPR. The remaining fraction was charged to facility use fee indexes.

• Mukherjee. Dr. Pinaki Mukherjee joined the ACMAL staff in 2018. A 15% fraction of his wages were charged to the S-TEM use fee index beginning in FY19. The remainder is funded by the MSE general fund.

• Lutz. Mr. Lutz is an employee of the Chemistry Department who offers part-time training and support of the LSCM. Mr. Lutz’s salary and fringe are charged to the Chemistry general fund index and lab fee index. None of his wages were charged to the LSCM index in FY18.

ACMAL lab assistants Elizabeth Miller and Aleister Kerr (Physics) assist Mr. Mills and, to a lesser degree, other ACMAL staff, with routine lab activities, and are qualified to train users of the SEMs, AFM and Nanoindenter and to conduct studies for researchers who choose not to operate the equipment themselves. They are paid $10-$12/hour and work approximately 10 hours each week during the semester and summer. Their wages are distributed to the ACMAL use fee indexes or are direct charged to faculty indexes for training. Management Structure

Mr. Mills coordinates activities of professional staff Dr. Laitila, Dr. Leftwich, Dr. Mukherjee and to a much lesser degree, Mr. Lutz. Mr. Mills supervises Ms. Miller and Mr. Kerr. Dr. Stephen Kampe is the MSE staff supervisor and Dr. John Jasczcak supervises Mr. Lutz.

ACMAL Safety Report

The ACMAL facility has passed the annual Shared Facilities safety inspection each year since inception in 2014. In those 4 years, only minor issues required attention including:

• proper use of surge suppression strips • frayed power cable • chemical and waste labeling

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• updated door signs • age of first aid kit • ladder type • battery disposal • gas cylinder restraint • electrical panel clearance • liquid nitrogen container labeling • appropriate sharps containers

Each of these issues has since been resolved. In October of 2015, a glass bottle

exploded when nitric acid was inadvertently mixed with solvent in a waste bottle. No one was seriously injured, the lab was cleaned, and new chemical storage and labeling protocols were put into place. A Chemical Hygiene plan was put into place. A Canvas-based safety module and exam is now in place.

Major shared use equipment (hourly) Internal External

• JEOL 6400 Scanning Electron Microscope/Microprobe $30 $100 • JEOL 2010 Transmission Electron Microscope $45. $150 • Scintag XDS2000 X-ray Diffractometer $8.25 $20 • Hitachi S4700 Field Emission Scanning Electron Microscope $42 $130 • Hitachi FB2000A Focused Ion Beam Milling System $50 $170 • FEI XL40 Environmental Scanning Electron Microscope (2014) $35 $100 • Olympus FV1000 Laser Scanning Confocal Microscope (2014) $24 NA • FEI Scanning Transmission Electron Microscope (2017) $70 $300 • Perkin Elmer 5800 X-ray Photoelectron Spectrometer (2017) $30 $150 • Asylum Research MFP-3D Origin+ Atomic Force Microscope (2018) NC NA • iMicro Nanoindenter (2019) in progress

Use fee history With the exception of 2 instruments all other operational costs for ACMAL equipment are shared via use fees. The use fee history is shown in Table 1. Unless the proposed fee is new, use fees are normally approved for 2 fiscal year periods, however reapplications can be made between those periods. Managing use fees is a task that requires attention during the fiscal year. The choice of a use fee is a balance between what it costs to operate the equipment versus what researchers are willing to pay to use the equipment. Uses fees are also chosen to provide researchers with a stable rate for budgeting. Exceptions occur when a deficit use fee index balances occur. Then a use fee must be increased as shown in the FY18 XRD fee below. The S-TEM rate has been increased to $70/hour in FY20, which is in line with the fee other schools charge for their instrument. ACMAL monitors what other universities charge for the same equipment.

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SEM TEM XRD FESEM FIB LSCM ESEM S-TEM XPS FY19 $30.00 $45.00 $8.25 $42.00 $50.00 $17.75 $35.00 $40.00 $30.00 FY18 $6.75 $50.00 FY17 $30.00 $40.00 $2.00 $45.00 $28.00 $25.00 $27.00 FY16 $30.00 FY15 $40.00 $34.00 $5.50 $40.00 $51.00 $60.00 $30.00 FY14 $50.00 $5.50 $30.00 Table 1. Use fee history for ACMAL indexes FY14 to FY19. Instrument use patterns

Overview. Four new instruments were added to the facility since 2016; the FEI S-TEM, Phi XPS, Oxford AFM and in the last month the iMicro nanoindenter. Use of these new instruments is increasing. Use fees were established for two of the four; the S-TEM and XPS. The use of the other major ACMAL instruments has decreased in some cases, notably the JEOL SEM/Probe, the JEOL 2010 TEM, the Hitachi FIB and FESEM. Use of the ESEM is increasing. S-TEM use is stable. Figure 1 shows use patterns for ACMAL equipment over the last 5 years. Equipment use generally scales with the number of university researchers using the facility and is largely dependent on the availability and nature of the external research funding secured by those users. With the exception of the LSCM, ESEM, XPS and S-TEM, use of ACMAL equipment has decreased. Decrease in hours of use without a change in research group use can be attributed to fewer and shorter sessions on the equipment. All use data presented below is per year.

Details. The SEM/Probe use dropped yet again in FY19 to 162 after a FY15 high at 686 hours. As use and revenue decreased we could no longer justify maintaining a service contract so we dropped the $13K service contract in FY15. The cause of the use decrease is the emphasis placed on ESEM use since the 2 instruments have similar resolution and we have added new capabilities to the ESEM including a new modern EDS system with an EBSD camera. Finally, in FY20 we elected to pay off the deficit balance, close the use fee index and sell the microscope.

The JEOL 2010 TEM use has dropped from a of 497 hours by 14 research groups in FY 18 to 274 hours by the same number of users in FY19. Use of the TEM had been stable in the period FY14 – FY18 at ~400 hours before dropping in FY19. There were 2 repairs that required service engineer trips that increased the deficit balance. We concluded that the TEM had become too unreliable and made the decision to pay off the deficit, close the use fee index and sell the microscope. We transferred all TEM use to the S-TEM including the MSE5550 Introduction to TEM course offer each spring semester.

XRD facility use dropped by half in FY15 due to the completion of four MSE projects led by Drs. Hackney, Kampe, Moran and Sanders. Use of the instrument then rebounded in FY16 and leveled off at 1700 hours each of the fiscal years 16, 17, and 18 even with a significant use

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fee increase in FY18. Unfortunately, FY19 brought a drop to 705 hours by 18 research groups that may be a response to the use fee increase.

FESEM use has been decreasing for the last 3 fiscal years from a high in FY15 of 1200 to 570 hours in FY19. The microscope is under service contract and is nearly always online and operational. Training to use the equipment is available on demand, so few barriers to use exist. The decrease can only be attributed to fewer projects requiring the equipment. This particular FESEM is a type that was perfect for the work we were doing in 2004 when it was purchased; namely high-resolution imaging. However, it is not ideal for the analytical characterization work we do today. A faculty team has been formed to prepare a second NSF MRI proposal for a new environmental FESEM having the required capabilities.

The FIB use dropped considerably after FY15 when a project of Dr. Levy’s (PH/MSE) ended. Instrument use and the number of groups using the FIB has been stable at 140 hours since then. New users include Dr. Suh (PHYS), Dr. Perrine (Chemistry) and Drs. Jin and Wang (MSE) who now use of the instrument and join regular users including Dr. Levy (PHYS), Dr. Hackney (MSE) and Mr. Mills (ACMAL). We anticipate FIB use to remain stable or increase further as the advanced specimen preparation capability of the FIB is required for S-TEM work. We cancelled the service contract on the FIB in FY14 when revenue was inadequate to amortize the $23K cost. Unfortunately, the lack of a service contract safety net led to unfunded major repair expenses of $30K. Routine use of the FIB will never pay that down to zero, so it is our intention to use the FY19 Shared Facilities funding we were awarded. We need to revisit the service contract issue since the high repair cost would have been covered with a service contract.

The LSCM was merged into ACMAL as a satellite facility in FY14. ACMAL responsibility is to serve as a consultant for facility management issues. Briefly, the microscope was purchased in FY13 and use of the instrument was free in the first few months as it was set up and the facility organized. During that period, it was used ~40 hour each week, but immediately after a rate was levied, use of the microscope dramatically decreased to 100 hours/month and the revenue collected was inadequate to amortize the maintenance contract cost. In the following 3 years, rates were adjusted twice to simultaneously encourage use and offset the service contract cost. We were unsuccessful and carried a deficit into FY16. A Shared Facilities grant was applied for and awarded to pay down the deficit and the $20K service contract was cancelled. Since then a modest $25/hour rate has attracted new users and use has increased to 385 hours by 8 research groups. As with the FIB and SEM/Probe, we are without a safety net service contract for the LSCM. There are several $20K lasers in the LSCM that have a limited lifetime. When the time comes, we will have to depend on Shared Facilities funding for repairs.

The ESEM use is increasing since ACMAL took over operational and management responsibility in FY14. Use and the number of research groups using the instrument dropped in FY16, but then increased after an MSE undergraduate course began using the ESEM for the MSE4530/5530 SEM course labs in both the fall and spring semesters. The new EDS x-ray analysis and EBSD crystallographic analysis attachment, funded by Shared Facilities grant funds, are fueling new use of the microscope, too. The ESEM EDS system is the only modern SEM microanalysis system in ACMAL. In FY19 the ESEM reached 516 hours of use and 31 researchers using the instrument. Previously, the 6400 SEM/Probe was used for the course lab sections. The change has negatively impacted use of the 6400.

The S-TEM came online in FY18 and first year use was 225 hours. This is less than we expected, however, since we have had a few repair problems during the initial use period that took the system offline. Use increased to 483 hours by 28 research groups in FY19. The other

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aberration corrected S-TEMs in the US are usually booked up with users and it can take months to get access to one. Ours is not, and we believe more external work will come our way because of this situation. The specialist that we hired to operate the S-TEM instrument lab, Dr. Pinaki Mukherjee, was an excellent hire. He has familiarity with the instrument and has taken ownership. Thus far, Mukherjee brought six projects to the lab. We are also working for Greg Odegard’s (MEEM) collaborator from Florida State on the US Comp project. We received manufacturer training on the in-situ specimen holders this year. These are powerful and unique capabilities that set the ACMAL S-TEM lab apart from other labs. We are promoting them now. The use fee was increased from $40/hour to $70/hour in FY20. That rate is commonly used at other labs with atomic resolution S-TEMs.

The XPS was installed in the M&M Building in FY18. It was an ARMY donation arranged by Drs. Chabalowski and Perrine in the Chemistry department. It did not function when it arrived but Dr. Leftwich, a surface scientist familiar with this equipment, was able to get it running properly. Tim is a Research Assistant Professor in MSE who is soft funded – he direct charges labor for work he does. The XPS ran during part of FY18 and generated 16 hours of use. That increased to 100 hours in FY19. Eleven research groups used the XPS in FY19. The use fee for XPS is $30/hour and the FY19 year-end balance was $154.

The Oxford AFM was installed in early January 2018. There is no use fee for the AFM. ACMAL trains users in basic operation and direct charges labor and cantilevers. There were 94 hours of use in the remainder of FY18. In FY19, 777 hours were used. In both FY18 and FY19, 10 research groups from 7 departments used the AFM.

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Figure 1. Hours of use in red and the number of research groups in blue using ACMAL major equipment for the previous five fiscal years.

Shared Facility Users and Supported Research

The number of users and faculty research groups during the FY14-FY19 period is shown in Figure 2 below. During the 5-year period covered by this report, users of the ACMAL facility include 118 researchers from 7 COE departments, 4 CSA departments, SFRES school, KRC Center and Seaman Museum. Faculty ACMAL users is steady at 80, but users (students) dropped from FY18 and FY19. This decrease in use pattern is shown in other graphics in this

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report and in this case shows that the same faculty are working in the labs, but for less time (shorter use sessions).

Figure 2. ACMAL users including students and faculty research groups by fiscal year. Sources of funding for work performed on ACMAL equipment during the 6-year period is shown below. The majority of work is carried out with sponsored research funds at 11K hours. Other funding sources include general fund, designated, gifts, IRAD and external work as shown in the figure below (Figure 3). As expected, sponsored research amounts to the largest share of funding sources, however, general fund use is high owing to course and lab fee use of the equipment. Designated use of the equipment is, in part, an indicator of maintenance of the equipment. Gifts use is Senior Design and Enterprise equipment use. Our interpretation of IRAD use is that it is funding to bridge grant awards. External work is a funding source we intend to expand in the coming years through partnering with Industrial Relations.

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Figure 3. Sources of funding for use of ACMAL equipment by fiscal year for the 6-year period.

Staff Wages Funding Sources The MSE department contributes 3 salary lines for staff that manage ACMAL. MSE funded staff have, in some cases, department responsibilities, such as instruction, committee work, supply ordering, equipment coordination and other tasks. Mr. Jerry Anzalone 100% soft funded (left university September 2019) Dr. Edward Laitila 100% general fund Dr. Tim Leftwich 100% soft funded Owen Mills 64% general fund, 29% use fees, 7% VPR (retiring June 2020) Dr. Pinaki Mukherjee 85% general fund, 15% use fees Aleister Kerr 100% use fees Liz Miller 100% use fees

Mr. Anzalone was employed in ACMAL as an equipment manager during all of the period only leaving in the last month. He direct charged SW&F for all work. ACMAL staff are encouraged to direct charge S&F for actually performing the analysis, training and operation. As an example, Dr. Mukherjee was able to direct charge $27K of his SW&F last fiscal year. Direct charging is expected of the student and part-time lab assistants who are front-line trainers for the most heavily used equipment including the AFM and the 2 SEMs.

Staff salary and fringe benefits charged to use fee indexes drives up the per hour fee for equipment usage. In some institutions, rates can be lower because 100% of salary and fringe are paid by other units (departments, colleges, VPR).

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Scholarly Activities

Training users is the most important activity ACMAL conducts. Prospective users can access the equipment in 3 ways. Course work including;

• Scanning Electron Microscopy – MSE4530 • Diffraction and Crystallography – MSE5130 • Transmission Electron. Microscopy – MSE5550 • Surface and Interface Science – CH5665/MSE5665

The ideal training is through the introductory course where the students receive theory

in lecture and practical experience during a hands-on laboratory session. Lab sections are kept small (4 students) so that each student has time to use the equipment each week. At the end of the course students take a simple practical exam to earn independent use of the equipment. One-on-one or small group training is a way to prepare students between course offerings. This training prepares students to use the equipment for one sample type and is done in 4-6 hours. Again, a practical exam is required. Finally, the ACMAL staff are available to operate the instrument for the researcher under their direction. Charges for the one-on-one and ACMAL-does-the-work include labor and equipment use fee.

ACMAL equipment is also used in Materials Characterization I and II, MSE 3120 and 3130. In this case ACMAL staff conduct lab sections for the courses to demonstrate the operation and capabilities of the equipment. ACMAL conducts instrument demonstrations for Physics, MEEM, ECE, and CEE courses.

Funding for equipment use in the course lab sections are charged to the MSE lab fee index.

The ACMAL staff participate in all University sponsored activities including Open House and Preview day. The equipment is utilized every year for SYP activities. Data management Facility users are responsible for removing their data from equipment computers immediately after the session is complete. ACMAL has D: drives on PC where a clone of the C: drive is kept. Updates are made to the D: drive including data. The S-TEM microscope images are too large for local storage so images are directly stored on a network drive where they can be opened at other locations. This is a model that is being explored for other ACMAL instruments, but not every instrument computer is (or can be) connected to the network.

Equipment Maintenance In terms of equipment maintenance, the most recent 2 years have been difficult. Four instruments have suffered major failures that required factory service to return to operational condition. In 3 of these cases, the repair was not covered by a service contract and was paid from use fee indexes. This threw each of the indexes into 5 figure deficits. Those deficits were not offset with use fee revenue. A Shared Facility grant was submitted and funded that will cover most of the deficit but it is likely another proposal of this type will need to be submitted again in the next cycle. The details follow.

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Focused Ion Beam System In FY18 a high voltage discharge in the sample chamber ruined a scintillator and preamplifier in the imaging system. Mr. Mills replaced the scintillator but could not make the preamp repair without assistance. A factory field service engineer was called in. The total cost for that repair was $8,842. Within 2 months, in FY19, a column contamination issue prevented stable focusing and a factory engineer was again called in to make the complex repair that required special tooling and fixtures. That repair cost $10,320. Total cost for the 2 repairs is $19,162. The FY 19 revenue was $7621. Including other expenses, the FY19 balance was $25,914. A chart (Figure 4) follows that describes the financial status. The plan is to use SF and IRAD funds to pay down the deficit as far as possible this year. Then, apply for additional SF funds next cycle to pay off the remainder. This instrument needs to be on a service contract and that will be investigated.

Figure 4. Revenue versus expense for the period FY14 – FY19 showing deficit balances. JEOL Transmission Electron Microscope The JEOL TEM suffered a high voltage problem in FY19 that requires a service engineer visit and an expensive part. Additionally, we had the engineer come back to make complicated alignment of the microscope to carry out a particular analysis. The total cost for these repairs was $10,328. Including other operational costs, the index deficit at FY19 closing was -$21,763. The plan is to pay off this deficit with SF funds received this cycle, close the use fee index and transfer all use of this microscope to the FEI S-TEM instrument. The S-TEM is fully capable of doing everything the JEOL TEM could do in addition to unique state-of-the-art capabilities. A chart showing the revenue and expense during the reporting period is shown below (Figure 5).

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Figure 5. Revenue versus expense for the period FY14 – FY19 showing increasing deficit balances beginning in FY17. Hitachi Field Emission Scanning Electron Microscope The FESEM has been under service contact since its installation in 2004. Ensuring operability at all times required the service contract. The annual cost is approximately $20K/year. The FESEM was once the most used ACMAL SEM, however a ~40% drop in use fee revenue has led to a deficit balance. Several key researchers once used the FESEM more often that today including Drs. Yoke Kin Yap, Miguel Levy, Claudio Mazzoleni. Dr. Yap’s group was once the most frequent users of the microscope. The chart below (Figure 6) shows the very close revenue vs expenses for most of the years in the period, usually ~-$4K. The -$22K deficit in FY16 was due to a mistimed purchase that should have ended up in the next FY and higher than usual wages and fringe. The chart clearly shows the large decrease in FY19 revenue, resulting in a -$17K balance.

Maintaining the service contract for this instrument is important because the vendor is willing to charge travel to the FESEM contract when they come up to work on the FIB. SF funds and IRAD will be used to pay down the deficit as far as possible and if needed a new proposal will be written for this purpose next SF funding cycle.

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Figure 6. Revenue versus expense for the period FY14 – FY19 showing FY 16 and FY19 deficits. The 40% decrease in FY19 use fee revenue is also shown. FEI Titan Themis Scanning Transmission Electron Microscope When the S-TEM was purchased 2 years of service contact at a 50% discount was negotiated. That service was paid by the COE Dean’s office. The 2-year contract expired in July of 2019 and the new contract was priced at $194K. Dr. Jason Carter and Mr. Mills worked to secure the funding from numerous sources including; COE Dean $28,000 CSA Dean $9,366 HRI $8,000 MARC/MuSTI $12,000 IMP $9,000 MSE $27,611 (return of Mukherjee direct charges) VPR $50,000 Use fee $50,000 Total $193,977 The point that needs to be made is that the service contract must be paid each year. The contract cost will increase ~5% each year. It can be expected that the cost will be evaluated with use of the instrument in consideration. As of October 7, the S-TEM has been used 220 hours. The rate has been increased from $40/hour to $70/hour, a rate equal to the figure used by 17 other universities with the same or similar equipment.

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Safety ACMAL safety reports can be found at these URLs. M&M labs https://www.mtu.edu/acmal/policy/safety/acmal-2019-full-inspection-report-mm-labs.pdf Chem Sci labs https://www.mtu.edu/acmal/policy/safety/acmal-2019-inspection-report-confocal-microscope-chemsci.pdf ATDC labs https://www.mtu.edu/acmal/policy/safety/acmal-2019-inspection-report-electron-microscope-atdc.pdf A key source of safety liability is electropolishing samples for the S-TEM in the M&M 637 lab. This is a process that involves shooting jets of solvent+acid solution towards a 3mm disc in the presence of voltage. The mixture of methanol and nitric acid is a dangerous solution. There was an explosion in 2015 when a student poured concentrated acid into a solvent waste bottle. No one was seriously injured but immediately steps were taken to eliminate the possibility of a recurrence. Furthermore, we ran a safety audit of the lab with EHS and identified other changes that could be made to increase safety. Today there are designated waste bottles for each solvent, acid and mixture that we use. Those bottles are policed to ensure they are being used. All electropolisher users are trained by experience staff, not other students. There was a nitric acid splash mishap that resulted in additional Personal Protective Equipment (PPE) gear being introduced including face shield and safety glasses and double gloves. A Chemical Hazard Plan was written and placed into service. In summary, many key changes have been made to make the facility safer.

Financial Reporting Shared Facility Grant use ACMAL has applied for SF Grants each year since the inception of the program in FY14. The funds have largely been used to acquire sample preparation tools and accessories for the electron microscopes. In two cases it was used to pay down deficits and two times for equipment repair.

Funds to upgrade an electron microscopy/x-ray facility are scarce. The <$100K price tags are too small for NSF grants but too large for solely IRAD funded purchases. The SF funds have been augmented with IRAD funds on nearly every proposal to increase purchasing power.

The Table 2 below shows the proposals by fiscal year.

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Shared Facility Grant Use FY14 – FY19 FY14 X-ray microanalysis system upgrade for ESEM $25,900 FY15 High resolution sputter coater and LSCM deficit paydown $43,000 FY16 Electron Backscatter diffraction system for ESEM $60,000 FY17 XRD software upgrade and programmable door locks $54,000 FY18 X-ray fluorescence repair and ESEM repair $45,600 FY19 Nano indentation system and deficit paydown $63,900 Table 2. Showing SF Grant purchases for period FY14 – FY19 Financial Statement The ACMAL operational strategy has been to safeguard that the equipment is operating and ensure that users receive the best possible service. In the process of carrying out this approach in the years prior to FY18, ACMAL has run minor deficits each fiscal year. The average of those balances is -$11,500. When revenue dropped, service contracts were cancelled on the SEM and FIB and the equipment was largely trouble free. Two years ago, that changed when the FIB and TEM both failed twice each. Then our keep it running strategy produced large deficits that could only be offset by SF grants and we incurred the expenses with this in mind. Examining expenditures in the table below (Table 3) the total expenditures between $103K in FY17 and $141K in FY19 or in the range ~20%. These figures represent the accumulation of revenue and expense for all equipment use fee indexes. The increase from $103K in FY17 to $141K in FY19 is due to the inclusion of a portion on Dr. Mukherjee’s SW&F to the S-TEM use fee. Expenses increase between FY14 and FY15 as the LCMS is added to the ACMAL equipment list. The $20K LSCM service contract was not renewed in FY17, so the decrease of expense in FY17 is due to the lack of expenditures in the LCSM index. Expenditures increase slightly in FY18 and FY19 due to additional S-TEM and XPS expenses. Again, looking at the table (Table 3), revenue for the 6-year period decreases from $134K in FY15 to $103K in FY19 as use of the SEMs and FIB drop. As shown in previous figures (Figures 4, 5 and 6), use fee revenue for the JEOL SEM dropped from $14K in FY17 to $4K in FY19. Revenue for the JEOL TEM dropped from $19K in FY18 to $9K in FY19. We will be taking both of these microscopes offline, pay off and close the use fee index. The Hitachi FESEM revenue dropped from $50K in FY15 to $23K in FY19. Significant deficits began to accumulate in FY17 into the current FY. SF, MSE, MuSTI funds and use fee index IRAD are being used to pay down deficits.

Carry forwards represent closing balances from the prior year and beginning in FY17 reflect the increasing debt due to equipment failure and repair.

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Table 3. Revenue and expense for period FY 14 – FY19.

Strategic Plan

Advancing ACMAL into the next 5 years would involve replacing obsolete equipment with new, modern tools that researchers need to maintain a competitive edge over their peers at other institutions. Due to the high cost of this equipment major research instrumentation (MRI) proposals would need to be submitted. ACMAL maintains a good relationship with faculty capable of writing those proposals. Additionally, setting aside optimal space for this highly sensitive equipment is paramount to achieving faculty research goals. Basement space in the new H-STEM building would be ideal. A discussion of the needed equipment is presented below. Any discussion of ACMAL strategy will include plans for encouraging use of the equipment. That discussion is included below as well.

A new, modern, thermal FE-ESEM is needed in ACMAL. The current microscope was perfect for our needs in 2004 when it was purchased during the DARPA contract period. It is a good high vacuum FESEM, capable of nanometer resolution however it is a poor analytical instrument since it generates low beam current. The new FESEM we envision would generate far higher beam current and would permit high quality chemical and crystallographic results in addition to nanometer scale resolution. The current research in Chemistry, Biomedical Engineering and Chemical Engineering requires a FESEM that is capable of low vacuum work for hydrated and non-conductive samples. The envisioned instrument can be operated in low vacuum mode to successfully analyze such samples. An NSF MRI proposal, written by Dr. Kathryn Perrine (CH), was submitted for the 2019 cycle, unfortunately, it was not funded. Another proposal, authored by Dr. Larry Sutter (MSE), is being constructed at this time. The instrument package would be ~$900K.

The XRD instruments are 25+ years old and have been identified as in need of replacement. The goniometer in the powder XRD system was used over 9500 hours during the 6-year period and is showing signs of age. Early discussions with Dr. Laitila are underway to identify a team to write and submit an NSF MRI proposal to replace it with modern XRD capabilities. New XRDs with modern accessories are ~$750K. The current M&M 6th floor space is suitable for this new instrument.

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Cost control in the next 5 years will require tough decisions regarding the need for certain underutilized equipment. The JEOL 6400 SEM and 2010 TEM are both underutilized, unreliable and are not needed at this point. The use fee indexes will be zeroed and closed. The equipment will be sold or scrapped. ACMAL offers other capable instruments for the same purpose including two other SEMs and the new S-TEM – all use of the decommissioned equipment will be funneled to that newer, better configured instruments. There will be no adverse impact on ACMAL equipment users.

Each room in the M&M 6th floor space has all utilities for analytical equipment including lighting, power and water. However, it is on the 6th floor of a building, not the optimal location for sensitive high-resolution equipment. All of the high-resolution equipment suffers as a result of floor vibration and poor air conditioning. The negative effects include artifacts in the data as a direct result of floor vibration. Brief discussion with AVPRD and VPR indicated that there was a possibility that low noise space could be constructed in the new H-STEM Building basement, although at this time no confirmation or notification has been received. Basement space that is specifically designed to minimize or eliminate vibration, and electric field would be an ideal solution for the M&M 6th floor problems. The equipment could operate at specified resolution and would be far more useful for certain types of work. ACMAL would be available to discuss environmental requirements during planning phases for the new building.

An example of low equipment use would be the 54% decrease in use of the current FESEM between FY15 and FY19. Granted, the microscope isn’t ideal for the work done today, but something will be done to increase use. Adding attachments to the FESEM would make it more useful. We have seen use increase 50% in 3 years of the ESEM after adding new x-ray attachments to it. SF funds were used for the ESEM upgrade and that could be done with the FESEM too.

Another approach to increase equipment use is by making faculty aware of ACMAL equipment and our capabilities. One plan is to give presentations during department seminar series across campus. Contributing to faculty Tech Talks is another opportunity. Participating in national and regional microscopy and characterization societies is an opportunity. Dr. Mukherjee has for 2 years given a talk at the national microscopy society, the Microscopy Society of America (MSA). ACMAL will team with Corporate Research to identify enterprises that may need capabilities we possess.

Concluding Comments

ACMAL has been a shared-use research instrumentation facility since 2003 gaining practical knowledge of running a shared facility by studying the practices at other universities and adapting those practices to the MTU environment. As a result of this experience, ACMAL is an MTU resource for issues related to shared facility operation. For example, Mr. Mills has been a member of the university Use Fee Committee since its inception. ACMAL supports a suite of useful major research instrumentation and specimen preparation tools. The mission is to ensure that ACMAL users are productive, and this is accomplished through proper training, offered flexibly, and with post-training staff support.

Financial issues are always a challenge, but adjustments are made, often during a fiscal year, to reduce expenses. Labor costs are contained by our effective staffing structure utilizing student and part-time staff where possible. The future is brightened by the installation of a true state-of-the-art S-TEM. The Shared Facility Funding proposal is an important opportunity

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for SFs by making resources available for upgrades and specimen preparation equipment to modernize the facilities.

Relationships with productive faculty have been fostered who are willing and capable of writing major research instrumentation proposals. The proposed thermal analytical FESEM is an example. The latest cutting-edge instrumentation is required if MTU faculty are to have a competitive research advantage relative to their peers.

Finally, as previously mentioned, ACMAL is dedicated to offering high-end research instrumentation capabilities for the lowest cost, ensuring that users are well trained, and MTU faculty receive value for the use fees paid.

Documents

5-Year Reauthorization Report for the Applied Chemical