MPEX-07-SPC-03 Rev0_signed.pdf

MPEX-07-SPC-03 R0

MATERIAL PLASMA EXPOSURE EXPERIMENT

TECHNICAL SPECIFICATIONS FOR A

SURFACE ANALYSIS STATION DIAGNOSTIC CHAMBER

Prepared by

OAK RIDGE NATIONAL LABORATORY

Oak Ridge, TN 37831-6283

Managed by

UT-BATTELLE, LLC

For the

US DEPARTMENT OF ENERGY

under contract DE-AC05-00OR22725

This report was prepared as an account of work sponsored by an agency of the United States government. Neither the United States government nor any agency thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise, does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States government or any agency thereof.

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Material Plasma Exposure Experiment Oak Ridge National Laboratory

Technical Specifications for a Surface Analysis Station Diagnostic Chamber for Material Plasma Exposure Experiment (MPEX) Project at Oak Ridge National Laboratory

Authors:

Ted Boyd, Mechanical Engineer Date

Xiao-Ying Yu, Group Lead of Advanced Nuclear Materials Date

Reviewer:

Douglas Curry, MPEX I&C CAM Instrument Lead Date

Theodore Biewer, Senior Scientist Date

Chad Parish, Senior Scientist Date

Milena Keys, Quality Assurance Representative Date

Aftab Hussain, Lead Engineer Date

Approver:

MPEX-07-SPC-03 R0 Page 3 of 21

Craig Deibele, MPEX Diagnostics CAM Date

Distribution:

Phillip Ferguson, MPEX Project Director Robyn Rose, MPEX Project Manager Juergen Rapp, Chief Scientist

MPEX-07-SPC-03 R0 Page 4 of 21

Technical Specifications for a Surface Analysis Station Diagnostic Chamber for Material Plasma Exposure Experiment (MPEX) Project at Oak Ridge National Laboratory

Revision History

Revision Date DESCRIPTION OF CHANGE

REVISION TYPE

Major Minor

0 Jan 20, 2024 Initial Issue ☐ ☐

MPEX-07-SPC-03 R0 Page 5 of 21

Technical Specifications for a Surface Analysis Station Diagnostic Chamber for Material Plasma Exposure Experiment (MPEX) Project at Oak Ridge National Laboratory

CONTENTS

1 SCOPE

2 APPLICABLE DOCUMENTS

2.1 ACCEPTANCE CRITERIA LISTING (ACL)

2.2 SHIPPING PLAN

3 TECHNICAL REQUIREMENTS

3.1 LAYOUT OF INSTRUMENTS AND INTERFACES

3.2 FUNCTIONAL AND PERFORMANCE

3.3 LABORATORY SPACE AND ENVIRONMENT

3.4 INSTRUMENTATION AND CONTROLS

3.5 BAKE-OUT

4 STANDARDS

4.1 STANDARDS FOR WELDING AND BRAZING

4.2 STANDARDS FOR COOLING WATER COMPONENTS

5 TEST AND ACCEPTANCE REQUIREMENTS

5.1 FACTORY ACCEPTANCE TESTS

5.2 SITE ACCEPTANCE TESTS

5.3 TESTS AND INSPECTIONS

6 QUALITY ASSURANCE REQUIREMENTS

6.1 UNITS

6.2 CALIBRATIONS AND CERTIFICATIONS

6.3 SOFTWARE

6.4 MATERIAL RECORDS

7 PACKAGING, HANDLING AND SHIPPING

7.1 PACKAGING

7.2 TRANSPORTABILITY

7.3 NAMEPLATE AND PRODUCT MARKING

7.4 STORAGE

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List of Figures

Figure 1: Arrangement of the SAS Diagnostic Chamber (green) and the SAS Vacuum System and support hardware (grey)

Figure 2: End view of the arrangement of the diagnostic ports for specific diagnostic system on the SAS Diagnostic Chamber

Figure 3: Cross-section of the diagnostic chamber with target position and Conflat flange dimensions

Figure 4: Diagnostic chamber Conflat flange sealing surface details

Figure 5: Diagnostic chamber flange mounting hole details

Figure 6: Conflat flange notch details

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1 SCOPE

This technical specification defines the requirements for the design, test, manufacture, and packaging of a Surface Analysis Station (SAS) Diagnostic Chamber to analyze a tungsten target in vacuo after it has been exposed to the plasma in the Material Plasma Exposure eXperiment (MPEX) project. This technical specification states requirements in terms of performance and it provides criteria for verifying compliance with the requirements. It does not define methods for achieving the results.

2 APPLICABLE DOCUMENTS

[1] Measurement requirements for MPEX off-device diagnostics systems (Surface Analysis

Diagnostics), MPEX-07-SRD-001, Section 3.2.3.

[2] Vacuum Handbook for Material Plasma Exposure Experiment (MPEX), MPEX-00-ENG-002.

2.1 ACCEPTANCE CRITERIA LISTING (ACL)

The ACL shall be developed and reviewed and approved by ORNL for the components in the SAS instrument package and mutually agreed between the Seller and ORNL.

2.2 SHIPPING PLAN

A packaging and shipping plan shall be developed by the Seller and reviewed and approved by ORNL. The plan shall be coordinated with the approved ACL for ORNL to review and accept the components of the SAS instrument.

3 TECHNICAL REQUIREMENTS

3.1 LAYOUT OF INSTRUMENTS AND INTERFACES

3.1.1 The SAS Diagnostic Chamber interfaces with the SAS Vacuum System as shown in the image below (Figure 1). The generic SAS Diagnostic Chamber is shown in green. The SAS Vacuum System and support structure is shown in grey. Other than the mounting flange, the shape of the SAS Diagnostic Chamber is for illustration purposes only and the final configuration shall be at the discretion of the vendor to meet the functional requirements. The shape of the SAS Vacuum System should be assumed fixed, and any

MPEX-07-SPC-03 R0 Page 8 of 21 changes implied by the SAS Diagnostic Chamber design must be approved in advance by the MPEX Project Team.

Figure 1: Arrangement of the SAS Diagnostic Chamber (green) and the SAS Vacuum System and support hardware (grey).

3.1.2 The layout of the diagnostic equipment in the SAS diagnostic chamber is shown below (Figure 2). The shape of the chamber is at the discretion of the supplier. The chamber body shall be perpendicular to the tungsten target face to allow maximal probing of the

MPEX-07-SPC-03 R0 Page 9 of 21 materials during analysis. The positions of the equipment shall be in the orientation shown.

Figure 2: End view of the arrangement of the diagnostic ports for specific diagnostic system on the SAS Diagnostic Chamber.

3.1.3 A cross-section of the SAS diagnostic chamber is shown below (Figure 3). The position of the target and the target positioner as shown in relation to the Conflat flange that interfaces with the SAS vacuum system. The SAS diagnostic chamber shall provide a DN275CF Conflat flange interface matching the dimensions in the MPEX

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Vacuum Handbook (MPEX-00-ENG-002) as illustrated in the image below. The dimension of the Conflat flange is nominally 13.25” diameter depicted in Figure 5.

Figure 3: Cross-section of the diagnostic chamber with target position and Conflat flange dimensions.

3.1.4 A detailed view of the SAS diagnostic chamber conflat face is shown below (Figure 4).

This face incorporates a knife-edge to distort a copper gasket to achieve a vacuum seal when the mounting bolts are tightened. The SAS diagnostic chamber DN275CF

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Conflat flange shall provide a knife edge matching the official dimensions in the MPEX Vacuum Handbook (MPEX-00-ENG-002) as illustrated in the image below.

Figure 4: Diagnostic chamber Conflat flange sealing surface details.

3.1.5 The mounting holes in the SAS Diagnostic chamber are shown below (Figure 5). The flange shall be assembled using thirty (30) 3/8-24 bolts. The SAS diagnostic chamber

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DN275CF Conflat flange shall provide a bolt pattern matching the dimensions of the MPEX Vacuum Handbook (MPEX-00-ENG-002) as illustrated in the image below.

Figure 5: Diagnostic chamber flange mounting hole details.

3.1.6 Conflat flanges are manufactured with two radiused notches in the sealing face located 180° apart. These notches are used for leak checking. The notches in the SAS Diagnostic chamber are shown below (Figure 6). The SAS diagnostic chamber shall

MPEX-07-SPC-03 R0 Page 13 of 21 provide two vertical (2) notches matching the dimensions of the MPEX Vacuum Handbook (MPEX-00-ENG-002) as illustrated in the image below.

Figure 6: Conflat flange notch details.

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3.2 FUNCTIONAL AND PERFORMANCE

3.2.1 The SAS diagnostic vacuum chamber shall be manufactured from Grade 316 stainless steel.

3.2.2 The SAS diagnostic vacuum chamber shall be capable of UHV, i.e., 10-9 Torr.

3.2.3 The SAS diagnostic chamber shall mount to a 13.25” Conflat flange with clearance holes for 3/8” bolts.

3.2.4 The SAS diagnostic chamber shall have a first harmonic resonance frequency ≥ 2 kHz when supported by the Conflat flange with the Conflat flange oriented vertically as in Figure 6.

3.2.5 The SAS diagnostic chamber shall have sufficient clearance to allow the target to be moved at least 5 mm in any direction parallel to the mounting face.

3.2.6 The SAS diagnostic chamber shall incorporate a plasma-based Focused Ion-Beam (Plasma FIB) located on the same axis as the target to provide capability of “trench” milling for cross-section examination by scanning electron microscopy (SEM).

3.2.7 The SAS diagnostic chamber shall incorporate a 100-400 Å SEM located on the target horizontal plane at an appropriate angle to view the “trench” created by the Plasma FIB.

3.2.8 The SAS diagnostic chamber shall incorporate a surface mapping X-ray spectrometer and associated detector(s) located 30° above the SEM.

3.2.9 The SAS diagnostic chamber shall incorporate a camera to provide positioning information for the target when it is inserted into the SAS chamber.

3.2.10 The SAS diagnostic chamber shall provide a port of ¼-inch OD for the future inclusion of a gas injection system. The optimal position of the port shall be determined by the Seller and approved by the Company.

3.2.11 The SAS diagnostic chamber shall provide two additional 2.75-inch Conflat ports (DN35CF) for the future inclusion of diagnostic equipment, such as a laser induced break-down spectroscopy quadrupole mass spectroscopy (LIBS-QMS) system. The optimal position of the ports shall be determined by the Seller and approved by the Company.

3.2.12 The SAS diagnostic chamber shall comply with the requirements in [2].

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3.3 LABORATORY SPACE AND ENVIRONMENT

The following describes the laboratory space in design and the instrument integration environment conditions.

3.3.1 SAS diagnostic power shall be supplied by a separate external circuit at 120 VAC or 208 VAC 60Hz.

3.3.2 Excessive dust and dirt shall be avoided, the cleanliness of the lab space shall be kept preventing degradation of instrument performance including the cooling system and the vacuum system. The lab space shall be a climate-controlled, dust-free environment.

3.3.3 A minimum floor space of 216 in × 216 in (549 cm × 549 cm) shall be provided to allow minimum clearance on all sides of the instrument for access to maintenance and diagnostics during operation or as required by the Seller, namely, supplier of the instrument package.

3.3.4 The floor shall be able to support the weight of the system. The weight of main components shall be determined and finalized by the Seller depending on the configuration. It is estimated that the microscope shall weigh approximately 1000 lb. and the instrument rack approximately 600 lb. The facility cart that contains the power box and other controls shall weigh approximately 250 lb. Finally, the PC workstation with monitor(s) shall weigh approximately 100 lb.

3.3.5 The floor levelness and flatness are important for instrument installation. The floor shall be constructed of an Alloy 49 plate grouted to the concrete slab. Measurement of environmental factors such as acoustic noise and vibration levels shall be performed within the perimeter of the proposed SAS instrument installation site. Such measurement results shall be provided to the Seller by the Company prior to the shipping date.

3.3.6 The instrument laboratory shall have proper magnetic shielding (< 1 Gauss) to reduce disturbance. Similarly, acoustic noise and electromagnetic interference shall be avoided.

If anticipated, they shall be reduced and mitigated.

3.3.7 Vibrations should be measured by the Company at the time of greatest vibration, such as during a shift change and with HVAC systems and any other nearby machinery in operational conditions. Several samples at various room locations should be taken to assure a worst-case measurement. Additional vibration measurements may be performed during a site inspection prior to delivery and/or installation.

3.3.8 Acceptable floor vibration design levels in the SAS room shall be 10 µm peak-to-peak between 1 to 5 Hz, 5 µm peak-to-peak between 5 to 10 Hz and 5 µm peak-to-peak between 10 to 500 Hz. These results are based on vibration measurements taken without the MPEX device installed and operational. Upon installation of the MPEX device, MPEX-07-SPC-03 R0 Page 16 of 21 additional vibration measurements shall be taken to identify the operational vibration levels.

3.3.9 The overall sound pressure level should be < 70 dBa to assure proper SAS SEM operations.

3.3.10 Although earthquake is not expected, consideration of weight distribution shall be included and discussed between the Seller and the “Company”, namely ORNL, including load distributions, center of gravity, and tie down locations during the SAS instrument configuration review meeting.

3.3.11 The SAS laboratory shall be maintained at ambient conditions, and it must be non-condensing to incoming cooling water and chiller pipes and connections.

3.3.12 The humidity in the surrounding of the instrument shall be non-condensing and preferably 40 – 70 %.

3.3.13 The temperature in the SAS laboratory shall be centrally controlled by the building operator and it shall be ambient room temperature.

3.3.14 Acoustic noise can be a source of vibration and it shall be curtailed. Acoustic noise frequency shall be less than or equal to 80 dB. The pumps and components that shall generate acoustic noise shall be placed in a service area, away from the detection unit, to minimize the noise level to be exposed to the instrument operator.

3.3.15 The clean dry house air shall be provided for necessary functions of the SAS instrument.

3.3.16 The clean compressed nitrogen with a purity of 99.99% shall be provided for necessary functions such as venting or pump down of the instrument.

3.3.17 A chase shall be provided to house the chiller unit of the SAS SEM instrument.

3.3.18 Ventilation of roughing pump(s) shall be provided if oil based pumps are used and provided by the Seller. A dry vacuum system (e.g., Pfeiffer ACP 28) shall be used, and no oil-based pumps shall be used either after delivery to ORNL nor during construction and testing at the Seller's site.

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3.4 INSTRUMENTATION AND CONTROLS

3.4.1 The SAS should interface to the local MPEX Instrumentation and Control network for data storage.

3.4.2 The SAS should have the ability to store specific instrument setups locally and be able to store device setups and retrieve device setups from the local MPEX Instrumentation and Control network.

3.4.3 The SAS operating temperature in the main analysis chamber shall be 70 ± 2 °F (21 ± 1 °C) by the Seller. The temperature shall be stable and controlled within ± 1.8 °F (1 °C)/

hr. in the analysis chamber by the Seller.

3.4.4 Suitable cooling shall be provided to properly cool the main components of the instrument as needed.

3.4.5 The SAS diagnostics shall be controllable from a centralized control area and shall possess one or more of the following interface methods: Ethernet, RS-232, or RS-485.

3.4.6 Control and monitoring of the SAS diagnostics can be operated from the SAS workstation and a centralized control area that mimics local control with the MPEX facility.

3.4.7 The equipment needs to have remote control capability, the details about implementation, protocol, and architecture shall be developed in cooperation with ORNL at a later stage.

3.4.8 The SAS diagnostic data output shall be in a format that is commonly accessible, and the format shall be approved by the MPEX Project in advance.

3.4.9 The instrument and supporting software shall be operated independently of any external network connections/access. If software licenses are in use, the SAS instrument users shall have access to the licenses via a local license manager.

3.4.10 The generated data files need to be in an open file format such as hdf5, tiff, etc. A standalone file converter is also acceptable.

3.4.11 The centralized data acquisition computer should have an additional network interface for transferring data out to an ORNL-controlled storage/location.

3.4.12 The Seller is expected to provide current versions of all source code developed by the Seller when the relevant Equipment is delivered to ORNL pending on the contract requirements mutually agreeable between the Seller and ORNL.

3.4.13 The Seller shall provide software design documentation including functional specifications, sequence diagrams, class diagrams, etc. for the software developed to meet the performance needs described in the technical descriptions. The software quality

MPEX-07-SPC-03 R0 Page 18 of 21 assurance requirements are expected at the time of instrument delivery to meet the Quality Level 1 procurement with the MPEX quality assurance program plan (QAPP).

3.5 BAKE-OUT

The SAS Diagnostic chamber shall be vacuum baked during initial pump down from atmosphere to assure a clean vacuum environment. This shall be achieved by wrapping the vacuum chambers with a custom heated blanket to bake the main vacuum chamber while the system is pumped down. The temperature may be up to 140 °C but no higher to prevent damage to the viton O-ring used in the target positioner.

3.5.1 The custom heating blanket shall be provided by the Company.

4 STANDARDS

4.1 STANDARDS FOR WELDING AND BRAZING

4.1.1 All welds shall be qualified and produced in accordance with ASME Section IX, AWS, (or equivalent), or the applicable design and construction code.

4.1.2 Welding and brazing processes shall be conducted using qualified welding or brazing procedure specifications and qualified welders or brazers supported by a welder or brazer qualification test records. Each welding and brazing procedure specification shall be supported by a procedure qualification record.

4.2 STANDARDS FOR COOLING WATER COMPONENTS

4.2.1 Any piping used in the SAS Diagnostic Chamber shall comply with the ASME B31.3 piping codes.

5 TEST AND ACCEPTANCE REQUIREMENTS

Results of acceptance tests and inspections described in Section 5 shall be documented and supplied to the Company.

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5.1 FACTORY ACCEPTANCE TESTS

A complete Factory Acceptance Test (FAT) Procedure shall be supplied by the Seller for review during the procurement process which shall encompass the testing to be performed for acceptance of the final SAS Diagnostic chamber performance prior to shipment.

The Test Procedure shall verify the following performance criteria:

• SAS Diagnostic chamber vacuum capability

• SAS Diagnostic chamber resonant frequency

• Plasma FIB operation

• SEM operation

• X-ray operation

• Camera operation

5.2 SITE ACCEPTANCE TESTS

A complete Site Acceptance Test (SAT) Procedure shall be supplied by the Seller for review during the procurement process which shall encompass the testing to be performed for acceptance of the final SAS Diagnostic chamber performance after shipment to ORNL and following installation at ORNL.

The Test Procedure shall verify the following performance criteria:

• SAS Diagnostic chamber vacuum capability

• SAS Diagnostic chamber resonant frequency

• Plasma FIB operation

• SEM operation

• X-ray operation

• Camera operation

5.3 TESTS AND INSPECTIONS

5.3.1 All tests, measurements and inspections shall be performed using approved procedures.

5.3.2 Testing and inspection procedures shall comply with applicable design and construction codes.

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6 QUALITY ASSURANCE REQUIREMENTS

6.1 UNITS

6.1.1 All inspection and test data shall be reported in SI units.

6.1.2 Diagrams and/or drawings shall be presented in dual units, where the imperial unit of length shall be inches.

6.2 CALIBRATIONS AND CERTIFICATIONS

6.2.1 Measurement and test equipment shall be calibrated, and calibrations shall be current and traceable to NIST standards.

6.2.2 The Nationally Recognized Testing Laboratory (NRTL) is an independent organization that was created by the Occupational Safety and Health Administration (OSHA) to ensure equipment be tested and certified for their safe use in the work. Equipment to be provided by the Seller must be meet NRTL inspections and certification by the Company’s Directorate Electrical Safety Officer (DESO) and qualified electrician. The equipment and main components should be properly recorded and marked after NRTL certification.

6.3 SOFTWARE

6.3.1 Any analysis software used in the design of the SAS diagnostics chamber subsystems and overall performance shall be verified and validated for accuracy and correctness.

6.4 MATERIAL RECORDS

6.4.1 Material certification records shall be submitted for review and approval by the Company for all materials used in construction of the SAS diagnostic chambers and associated components.

6.4.2 Material certifications shall be compliant to EN 10204 (or equivalent).

7 PACKAGING, HANDLING AND SHIPPING

7.1 PACKAGING

7.1.1 The equipment shall be packaged, handled, and shipped to prevent mechanical or physical damage to it during transit.

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7.1.2 Components shall be packed with adequate protection from thermal or mechanical stresses as well as particle or moisture accumulation that may adversely affect the operation of the component.

7.2 TRANSPORTABILITY

7.2.1 The equipment shall be packaged in a manner that facilitates movement, loading, and unloading by fork truck or crane. Any lifting fixtures or related hardware required to move, load, unload or install the equipment shall be considered part of the equipment.

7.2.2 Tilt and/or rough handling monitoring devices shall be required for shipment.

7.3 NAMEPLATE AND PRODUCT MARKING

7.3.1 The equipment shall be permanently marked to include the following information:

• Manufacturer

• Model number

• Serial number

7.4 STORAGE

7.4.1 Equipment shall be protected from damage during storage. Provisions shall be identified and implemented to ensure that the equipment is thoroughly drained and dried of all water prior to transport to prevent damage due to freezing.