The amazing materials that are produced through additive manufacturing (AM) and 3D machining often require post-processing heat treatments before these become final components that launch into space. What are the trends of AM/3D outside our planet, and what technical resources are available to you as you make one step into this field? This original content piece from the Heat Treat Today editors will help you understand where technology stands in 2024.
Why Does AM/3D Go to Space?
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A broad spectrum of industries have found the appeal of additively manufactured parts, industries ranging from mining to medical and automotive to space. Much of this has to do with complexity of components that new engineering techniques require, the desire to save on material costs, and the ability to condense lead time. For some, additive manufacturing is becoming essential to the space industry; as Tobias Brune, head of the Business Unit Additive Manufacturing at TRUMPF, has commented, “With our 3D printing technology, we are driving the commercialization of the space-travel industry. If you want to be successful in the space-travel industry today, you have to use additive manufacturing.”
When should you expect this transition? Now.
In January of this year (2024), the first metal 3D printer for space was launched to the Columbus module of the International Space Station (ISS). This is a very active, integrated sense of seeing AM in the aerospace industry, and test runs with this equipment will ensue.
Flight model of 3D Metal Printer Launched on NG-20 Source: ESA
The Exploration Company in Europe plans to use 3D printers from TRUMPF (laser specialist) to print core components in engines for spacecrafts. The intent: missions in Earth’s orbit and to the moon.
Heat Treat & thermal Processing Requirements of Post-ProcessingAM
If you are going to get involved in AM, it is essential to have the right equipment. One of the most talked about equipment is hot isostatic pressing (HIP) technology. Often, heat treat operations use HIP equipment for post-process heat treating in order to get the solid part they desire. For the most part, commercial heat treaters have positioned themselves to handle the R&D required to navigate the terrain of overcoming processing challenges of new/complex parts and creating standardizations. However, privateR&D facilities and departments are also building out their capabilities to handle AM in HIP.
However, so also have vacuum furnaces been a key leader in heat treating AM components. Here, commercial heat treaters have also made moves to expand their equipment/process offerings to accommodate AM parts.
So also do atmosphere considerations need to be considered, withgasses like H2 competing trying to capture the limelight.
Continue the Exploration: AM/3D Articles for Space
Looking for an introduction to the AM/3D topic for heat treaters? Begin with this article by Animesh Bose, an engineering pioneer: “The Role Of Heat Treat in Binder Jetting AM for Metals.” The article uncovers the history of one of the most important types of AM/3D manufacturing — binder jetting AM.
Then, take a step over for an industry focus on what “heat treatments for space” look like. Mike Grande eloquently summarized the current processes needed in space in this editorial from the March 2024 Aerospace print edition. Read “The Role of Heat Treatment in Space Exploration” in the digital edition of the magazine.
In-house or commercial? This article presents critical considerations of space components — with a particular emphasis on the importance of AM/3D — when considering how to grow your processing expertise and capabilities. Several examples from the frontlines of R&D are presented by Noel Brady in his article. Read the editorial, “Thermal Processing for Space and Additive Manufacturing,” for excellent illustrations.
Finally, hone in on the topic with a case study about developments in HIP technology for space component post-processing. This article begins with context confronting issues of structural integrity, especially of complex space components, with HIP. Andrew Cassese gets to the case study towards the end of his article, “High Pressure Prepares Parts for Space.”
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Dive into the role and benefits of HIP and HPHT™ in the space industry, highlighting how these key processes are shaping the future of space applications.
ThisTechnical Tuesdayarticle by Andrew Cassese, applications engineer, Quintus Technologies was originally published inHeat Treat Today’sMarch/April 2024 Aerospaceprint edition.
The realm of space exploration and technology is rapidly evolving, pushing the boundaries of what’s possible in engineering and material science. Among the key players in this revolutionary change are hot isostatic pressing (HIP) and High Pressure Heat Treatment™ (HPHT™). These processes have become indispensable in manufacturing components that can withstand the harsh conditions of space. In this demanding environment, the longevity and reliability of components are paramount.
Reducing Risk
Space missions have put increasing focus on the need to minimize risk and improve mission safety. Some well-documented, safety-related events include:
Outer space
Soyuz 11 decompression in 1971
Earth’s atmosphere
Soyuz 1 parachute failure in 1967
X-15 controls failure in 1967
Space Shuttle Challenger launch booster failure in 1986
Space Shuttle Columbia re-entry disaster in 2003
Structural integrity is therefore in focus for every single component involved in space missions, with exacting demands on quality and function. Material failure is not an option, and therefore component qualification is one of the main areas of focus. Predictable properties that are reliable and with minimal variation are critical for mission safety. Hot isostatic pressing helps to guarantee this by reducing the spread and variation in mechanical properties.1 It works to do this by using high temperatures and pressures to close internal defects in mission critical parts after casting or additive manufacturing. This increases the density of components and gives them a more anisotropic microstructure which in turn results in more consistent mechanical properties.2
What Properties Are Most Important
The harsh environment of space demands components with exceptional properties. They must withstand extreme temperatures, resist radiation, endure vacuum pressures, and cope with mechanical stress from vibrations and accelerations. HIP processing plays a pivotal role in this, enhancing material properties to meet these challenges. Space manufacturers also must think about thermal expansion/contraction due to temperature variations, compressive stresses, irradiation, and space debris. All of these can affect mission success and can ultimately prevent loss of life, see Figure 1.
Figure 1. Challenges that space-bound materials must endure
Through HIP, components gain increased fatigue life, improved ductility, and enhanced fracture toughness, which are crucial for surviving in space.
Common Materials and HIP Processing Requirements
Materials commonly processed by HIP for space applications include titanium, aluminum alloys, nickel-based superalloys, refractory alloys, shape memory alloys, and ceramics. High-strength aluminum and titanium alloys are used due to their high strength to weight ratio which is key for space missions to conserve fuel efficiency, increase payload capacity, and improve maneuverability.3 Nickel-based superalloys are used in exhaust valves and turbine rotors due to their exceptional creep resistance properties at high temperatures. Refractory alloys like Nb-C103 and TZM are used in high-performance rocket nozzles because of their high melting point and excellent strength at high temperatures. Newer shape memory alloys developed by NASA can recuperate their original shape when heating above specific critical temperatures, and their applications are expanding beyond just actuators.4
As new alloys and materials are developed in the space industry, certifications and standards are necessary for their adoption. HIP effectively eliminates porosity in these materials, ensuring structural integrity and performance under the extreme conditions of space. This means HIP recipes need to be developed and optimized for materials to be tested with their greatest potential in mind.
Collaborations with universities and national labs on projects at low TRLs will help set the foundation for HIP in the space industry. Quintus Technologies, through its application centers, is actively engaged in research to further enhance the capabilities of HIP for space applications. Optimizing the HIP process to reduce costs and improve efficiency through HPHT is one area where the company has already found success, see Figures 2 and 3.
Figure 2. Typical thermal processes for additively manufactured partsFigure 3. High pressure heat treatment with solution heat treatment
(SHT) process for the same parts, using an integrated heat
treatment approach
The HPHT process can combine stress relief, solution annealing, HIP, and aging into one cycle. Aft er a ramp up in pressure and temperature, the part is held for a specified amount of time before being rapidly cooled in the URC furnace. Aft er this, the temperature of the machine can be brought up to the aging temperature of the material for the completion of an in situ heat treatment.
A Space Case – Launcher Engine-2 Rocket Engine
Table 1. CuCrZr vs. GRCop-42: A Comparison
One application of this is on the Launcher Engine-2 (E-2) rocket engine.
Quintus Technologies, EOS Group, and Launcher worked together to develop a tailored HPHT cycle for Launcher’s 3D printed E-2, first vetted out in an applications center at small scale. The powder alloy in question, CuCrZr, was developed by EOS and printed on an AMCM M4K machine. EOS compared CuCrZr to the NASA alloy of GRCop-42 and found that the CuCrZr alloy was a more economically viable solution for thermal applications with lower strength requirements, see Table 1. The rapid cooling at 200°C/min in the QIH 122 URC furnace at Aalberts surface technologies allowed the team to HIP and solution heat treat the CuCrZr combustion chamber in a single step. The aging treatment was also performed in the QIH 122 directly aft er the solution.5
In October 2020, a full-scale test firing of the E-2 injector and combustion chamber was conducted at the Launcher NASA Stennis Space Center test stand. On April 21, 2022, Launcher’s E-2 liquid rocket engine was able to demonstrate full thrust. Continued tests from Launcher have been successful with performance boost testing and the first fully integrated engine was ready for shipping on October 12, 2023.6
As humanity reaches further into the cosmos, the role of HIP and HPHT in manufacturing space-bound components becomes increasingly significant. These processes not only enhance the essential properties of materials for space applications but also address the unique challenges of manufacturing for an environment as hostile as space. With ongoing research and development, HIP and HPHT continue to evolve, promising to unlock new possibilities in space exploration and technology, and their contribution will ensure the success of space missions, safeguarding the lives of those who venture into the final frontier.
Figure 5. Test firing of the High Pressure Heat Treated Launcher Engine 2 produced using additive manufacturing
References
[1] Dominik Ahlers and Thomas Tröster, “Performance Parameters and HIP Routes for Additively Manufactured Titanium Alloy Ti6Al4V. EuroPM,” 2019. https://www.semanticscholar.org/paper/Performance-Parameters-and-HIP-Routes-fortitanium- Ahlers-Tr%C3%B6ster/faeb46e6eb8ef3e30bc00b91cd1bd8a7c0619200. [2] Jake T. Benzing et al., “Enhanced strength of additively manufactured Inconel 718 by means of a simplified heat treatment strategy,” Journal of Materials Processing Technology 322, (December 2023). https://www.sciencedirect.com/science/article/abs/pii/S0924013623003424?via%3Dihub. [3] “Engineering Materials for Space Building Stronger Lighter Structures,” Utilities One, last modified November 2023. https://utilitiesone.com/engineering-materials-for-space-building-stronger-lighter-structures. [4] Girolamo Costanza and Maria Elisa Tata, “Shape Memory Alloys for Aerospace, Recent Developments, and New Applications: A Short Review,” Materials (Basel) 13, no. 8 (April 2020): 1856. https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7216214/. [5] Mahemaa Rajasekar, “Processing Copper Alloys with Powder Bed Fusion,” LinkedIn, last modified November 2022. https://www.linkedin.com/pulse/processing-copper-alloys-dmls-technology-mahemaarajasekaran/. [6] LAUNCHER (@launcher), “The first fully integrated E-2 engine is ready for shipping to @NASAStennis for our upcoming full engine test campaign later this year. E-2 is a 22,000 lb. (10 ft) thrust LOX/Kerosene,” X post, October 12, 2023. https://twitter.com/launcher/status/1712636548997607752.
About the Author
Andrew Cassese, Applications Engineer, Quintus Technologies
Andrew Cassese is an applications engineer at Quintus Technologies. He has a bachelor’s degree in welding engineering from The Ohio State University.
For more information: Read J Shipley, “Hot Isostatic Pressing in Space – Essential Technology to Ensure Mission Safety,” 2020. Contact Andrew at andrew.cassese@quintusteam.com.
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The race to space is in full swing with public and private sector companies staking their claim in this new frontier. And breakthroughs in technology and materials offer the potential to propel humanity to unprecedented distances. Success hinges not only on the ability to discover novel solutions but also on the capacity to prepare those solutions for efficient, large-scale production.
ThisTechnical Tuesdayarticle by Noel Brady of Paulo was originally published inHeat Treat Today’sMarch/April 2024 Aerospaceprint edition.
Space Today: Making Life on Earth Better, Safer, and More Connected
Noel Brady, Metallurgical Engineer, Paulo Source: Paulo
According to NASA, 95% of space missions in the next decade will stay in low Earth orbit (LEO) and geostationary orbit (GEO). Th at means the first wave of commercial activity in space will be largely focused on making life on Earth better.
Several worldwide broadband satellites are already in orbit, offering more consistent, reliable internet signals around the globe. Defense campaigns are using advanced satellite machine learning to improve asteroid and missile detection, along with revolutionary laser technology that has made intersatellite communication possible for the first time — and the travel of information faster. And to help make life in space safe and successful, NASA is developing a scalable network of public GPS receivers for easy, short-range space navigation and tourism.
All this to say, parts are being developed for a wide range of applications, a huge portion of which are being additively manufactured.
Thermal Processing Standards Necessary for AM Adoption
However promising additive manufacturing is for space, the adoption of AM has still been limited due to the lack of standards for proprietary material and 3D printing applications. Many thermal processing experts are joining research institutions and OEMs in the drive to bring AM into mainstream manufacturing with new industry standards and production-ready solutions that help achieve ROI.
The R&D process for discovering these standards can be lengthy and expensive because it requires trial and error. A prototype or small run of parts must be manufactured, then heat treated, and tested for the desired properties. If a test part’s yield strength is not where it should be, for example, then the heat treating recipe is adjusted, perhaps by lowering the temperature and increasing the pressure, and can be tested again on a new batch of parts.
Coach vs. Custom Cycles
In heat treating, there are two different types of cycles, and it’s important to know the difference when you’re working with any commercial heat treater. Coach cycles tend to be more economical because these are shared cycles — existing recipes that are in high demand and run on a regular schedule — with the potential to have multiple clients’ parts in the furnace at once. For example, a heat treater may have a standard titanium coach cycle they run once a day. See Table A for several coach cycles run at Paulo.
Table A. Example of Coach Cycles for Space Alloys
Coach cycles use recipes that were designed for cast parts and have been around since before additive was a viable form of manufacturing. While it’s true that cast parts and AM parts have similarities, such as their high porosity, it doesn’t mean that the recipes are optimal for preparing today’s parts for heavy space applications. That’s where custom cycles come into play.
Custom cycles are ideal for new or proprietary materials that don’t yet have recipes defined or that are not commonly heat treated enough to run on a regular schedule. The distinction between the two is important because not all heat treaters are equipped to run both types. While you may be able to find a coach recipe that gets you close to where you need to be, it certainly may not be optimal, especially for parts that will have a heavy life of service.
Heat treaters with flexibility of custom and coach cycles, along with full-cycle data reporting, offer a high level of control that is vital for helping the industry progress and scale for production. This is also a big reason why some in-house heat treating operations may choose to outsource some of their work: first collaborating with experienced commercial heat treaters to prove the specification for a new part with custom cycles before scaling for production.
Common Cycle Adjustments for AM
There are five primary parameters that can be adjusted in the heat treating of AM parts to achieve the desired results: temperature, pressure, time, cooling rate, and heating rate. For AM parts, adjustments to the temperature and pressure are a go-to for achieving parts with higher yield strength. For example, running a cycle 50°F cooler, but at 5 ksi higher pressure may yield better results.
There may also be certain heating ramp rates and intermediate holds before parts get to the max temperature, to allow for consistent heating and enhance the material properties. The same goes for the cooling process: controlling the rate at which a part cools with specific holding times and intermediate quenches.
Hot Isostatic Pressing, Space, and Additive Manufacturing
Hot isostatic pressing (HIP) combines high temperature and pressure to improve a part’s mechanical properties and performance at extreme temperatures. The sealed HIP vessel provides uniform pressure to bring parts to 100% theoretical density with minimal distortion. The high level of control and uniformity has made HIP the gold standard for AM parts for space.
Similar to cast parts, 3D-printed materials tend to have porous microstructures that can compromise part performance. HIP is the only process that’s able to eliminate these pores without compromising the complex geometries and near-net dimensions that are achieved in the printing process.
Benefits of HIP for space parts include the following:
Better fatigue resistance
Greater resistance to impact, wear, and abrasion
Improved ductility
For this process, Paulo’s Cleveland division is equipped with a Quintus QIH-122 HIP vessel, which is specially modified with additional thermocouples for more precise temperature control and greater data collection. A higher level of accuracy allows us to iterate with confidence and find an efficient path to production-ready development.
One primary benefit of the Quintus QIH-122 HIP is the ability to have faster cooling at a controlled rate, which allows you to heat treat and solution treat in one furnace. This cooling rate allows great efficiency that cannot be seen with other HIP vessels on the market.
It is critical that heat treaters adapt to meet the needs of this fast-evolving industry. Many commercial heat treaters do not yet have the level of data or dynamic cycle offerings necessary and will only run HIP coach cycles with set parameters. In other words, many are not equipped to economically iterate and adapt heat treating recipes for new parts. Without custom cycles, controlled cooling, and a higher level of data, it is impossible to push the boundaries of what’s possible.
Space Parts Requiring Thermal Processing
The future of space travel requires parts that can not only perform under high levels of mechanical pressure and extreme temperatures but are also durable enough for long-range and repeat missions. Heat treatment is a critical step in preparing rocket engine components, among others, for commission. Other space components commonly heat treat treated are:
Volutes
Turbine manifolds
Bearing housings
Fuel inlets
Housings, support housings
Bearing supports
Turbo components
Since the inception of NASA’s Space Shuttle Program, Paulo has treated integral components for launch and propulsion, along with many parts currently in orbit on the International Space Station.
Materials Used in Space Parts
New materials and applications are being explored every day. Proprietary alloy blends bring unique properties and promising potential in the push for stronger, faster, longer-lasting parts. But with unique properties comes the need for unique heat treating processes. Several high-performance superalloys used for space include:
Inconel 718, 625
Titanium (Ti-6Al-4V)
Hastelloy C22
Haynes 214, 282
GRCop Copper
Inconel 718, a championed space alloy, was originally used as a premier casting material before being adopted for AM. This nickel-based material features an extremely high tensile and yield strength that makes it ideal for components taking on a high mechanical load in extreme environments ranging from combustive to cryogenic — making this a natural material to adopt for space in the early days of 3D printing.
Because casting and 3D printing both result in similar porous microstructures, the heat treating process used for Inconel castings could also be adapted. Finding new opportunities within existing alloys like this is a highly efficient way to gain material advantage in today’s race to space.
Noel joined Paulo in 2011 and spent several years as quality manager before stepping into his current role as a metallurgical engineer. Noel holds a bachelor’s degree in engineering and metallurgy materials science, and he is responsible for thermal process development and hot isostatic pressing process development.
For more information: Contact Noel Brady at nbrady@paulo.com or visit this link to download the full space guide from Paulo.
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How often do you think about the intelligent designs controlling the thermal loop system behind your heat treat operations? With ever-advancing abilities to integrate and manage data for temperature measurement and power usage, the ability of heat treat operations to make practical, efficient, and energy-conscious change is stronger than ever. In part 1, understand several benefits of thermal loop systems and how they are leveraged to comply with industry regulations, like Nadcap.
This Technical Tuesday article by Peter Sherwin, global business development manager – Heat Treatment, and Thomas Ruecker, senior business development manager, at Watlowwas originally published inHeat Treat Today’sJanuary/February 2024 Air & Atmosphere Heat Treat print edition.
Introduction
Heat treatment processes are a crucial component of many manufacturing industries, and thermal loop solutions have become increasingly popular for achieving improved temperature control and consistent outcomes.
A thermal loop solution is a closed loop system with several essential components, including an electrical power supply, power controller, heating element, temperature sensor, and process controller. The electrical power supply provides the energy needed for heating, the power controller regulates the power output to the heating element, the heating element heats the material, and the temperature sensor measures the temperature. Finally, the process controller adjusts the power output to maintain the desired temperature for the specified duration, providing better temperature control and consistent outcomes.
Performance Benefits
Heat treatment thermal loop solutions offer several advantages over traditional heat treatment methods, including improved temperature control and increased efficiency. The thermal loop system provides precise temperature control, enabling faster heating and cooling and optimized soak times. In addition, the complete design of modern thermal loop solutions includes energy-efficient heating and overall ease of use.
Figure 1. Watlow Industry 4.0 solution (Source: Watlow)
Heat treatment thermal loop solutions are integrated with Industry 4.0 frameworks and data management systems to provide real-time information on performance. Combining artificial intelligence and machine learning algorithms can also provide additional performance benefits, such as the ability to analyze data and identify patterns for further optimization. Ongoing performance losses in a heat treatment system typically come from process drift s. Industry 4.0 solutions can explore these drift s and provide opportunities to minimize these deviations.
Heat treatment thermal loop solutions can be optimized using Failure Mode and Effects Analysis (FMEA). FMEA is a proactive approach to identifying potential failure modes and their effects, allowing organizations to minimize the risk of process disruptions and improve the overall efficiency of their heat treatment processes. Historically, this was a tabletop exercise conducted once per year with a diverse team from across the organization. Updates to this static document were infrequent and were primarily based on organization memory rather than being automatically populated in real time with actual data. There is a potential to produce “live” FMEAs utilizing today’s technology and leveraging insights for continuous improvement.
Th e effectiveness of heat treatment thermal loop solutions can be measured using metrics such as overall equipment effectiveness (OEE). OEE combines metrics for availability, performance, and quality to provide a comprehensive view of the efficiency of a manufacturing process. By tracking OEE and contextual data, organizations can evaluate the effectiveness of their heat treatment thermal loop solutions and make informed decisions about optimizing their operations.
Regulatory Compliance
Nadcap (National Aerospace and Defense Contractors Accreditation Program) is an industry-driven program that provides accreditation for special processes in the aerospace and defense industries. Heat treatment is considered a “special process” under Nadcap because it has specific characteristics crucial to aerospace and defense components’ quality, safety, and performance. Th ese characteristics include:
Process sensitivity: Heat treatment processes involve precise control of temperature, time, and atmosphere to achieve the desired material properties. Minor variations in these parameters can significantly change the mechanical and metallurgical properties of the treated components. This sensitivity makes heat treatment a critical process in the aerospace and defense industries.
Limited traceability: Heat treatment processes typically result in changes to the material’s microstructure, which are not easily detectable through visual inspection or non-destructive testing methods. Th is limited traceability makes it crucial to have strict process controls to ensure the desired outcome is achieved consistently.
Critical performance requirements: Aerospace and defense components often have strict performance requirements due to the extreme conditions in which they operate, such as high temperatures, high loads, or corrosive environments. The heat treatment process ensures that these components meet the specifications and can withstand these demanding conditions.
High risk: The failure of a critical component in the aerospace or defense sector can result in catastrophic consequences, including loss of life, significant financial loss, and reputational damage. Ensuring that heat treatment processes meet stringent quality and safety standards is essential to mitigate these risks.
Nadcap heat treatment accreditation ensures suppliers meet industry standards January/February and best practices for heat treatment processes. The accreditation process includes rigorous audits, thorough documentation, and ongoing process control monitoring to maintain high quality, safety, and performance levels.
The aerospace industry’s AMS2750G pyrometry specification and the automotive industry’s CQI-9 4th Edition regulations are crucial for ensuring consistent and high-quality heat treated components. Adherence to these regulations is essential for meeting the stringent quality requirements of the aerospace and automotive industries and other industries with demanding specifications.
Temperature uniformity is a crucial requirement of both AMS2750G and CQI-9 4th Edition, mandating specific temperature uniformity requirements for heat treating furnaces to ensure the desired mechanical properties are achieved throughout the treated components. AMS2750G class 1 furnaces with strict uniformity requirements +/-5°F (+/-3°C) provide both quality output and predictable energy use. However, maintaining this uniformity requires significant maintenance oversight due to all the components involved in the thermal loop.
Calibration and testing procedures are specified in the standards to help ensure the accuracy and reliability of the temperature control systems used in heat treat processes.
Detailed process documentation is required by AMS2750G and CQI-9 4th Edition, including temperature uniformity surveys, calibration records, and furnace classifications. This documentation ensures traceability, enabling manufacturers to verify that the heat treat process is consistently controlled and meets the required specifications.
Figure 2. Eurotherm data reviewer (Source: Watlow)
Modern data platforms enable the efficient collection of secure raw data (tamper-evident) and provide the replay and reporting necessary to meet the standards.
The newer platforms also offer the latest industry communication protocols – like MQTT and OPC UA (Open Platform Communications Unified Architecture) – to ease data transfer across enterprise systems.
MQTT is a lightweight, publish-subscribe-based messaging protocol for resource-constrained devices and low-bandwidth, high-latency, or unreliable networks. IBM developed it in the late 1990s, and it has become a popular choice for IoT applications due to its simplicity and efficiency. MQTT uses a central broker to manage the communication between devices, which publish data to “topics,” and subscribe to topics that they want to receive updates on.
OPC UA is a platform-independent, service-oriented architecture (SOA) developed by the OPC Foundation. It provides a unified framework for industrial automation and facilitates secure, reliable, and efficient communication between devices, controllers, and software applications. OPC UA is designed to be interoperable across multiple platforms and operating systems, allowing for seamless integration of devices and systems from different vendors. The importance of personnel and training is emphasized by CQI-9 4th Edition, which requires manufacturers to establish training programs and maintain records of personnel qualifications to ensure that individuals responsible for heat treat processes are knowledgeable and competent. With touchscreen and mobile integration, a significant development in process controls has occurred over the last decade.
Figure 3. Watlow F4T® touchscreen and Watlow PM PLUS™ EZ-LINK®
mobile application
By integrating these regulations into a precision control loop, heat treatment thermal loop solutions can provide the necessary level of control and ensure compliance with AMS2750G and CQI-9 4th Edition, leading to the production of high-quality heat treated components that meet performance requirements and safety standards.
Continuous improvement is also emphasized by both AMS2750G and CQI-9 4th Edition, requiring manufacturers to establish a system for monitoring, measuring, and analyzing the performance of their heat treatment systems. This development enables manufacturers to identify areas for improvement and implement corrective actions, ensuring that heat treat processes are continuously improving and meeting the necessary performance and safety standards.
To Be Continued in Part 2
In part 2 of this article, we’ll consider the improved sustainability outcomes, potential challenges and limitations, and the promising future this technology offers to the heat treat industry.
About the Authors
Peter Sherwin, Global Business Development Manager – Heat Treatment, WatlowThomas Ruecker, Senior Business Development Manager, Watlow
Peter Sherwin is a global business development manager of Heat Treatment for Watlow and is passionate about offering best-in-class solutions to the heat treatment industry. He is a chartered engineer and a recognized expert in heat treatment control and data solutions.
Thomas Ruecker is the business development manager of Heat Treatment at Eurotherm Germany, a Watlow company. His expertise includes concept development for the automation of heat treatment plants, with a focus on aerospace and automotive industry according to existing regulations (AMS2750, CQI-9).
For more information: Contact peter.sherwin@watlow.com or thomas.ruecker@watlow.com.
This article content is used with the permission of heat processing, which published this article in 2023.
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Thinking about travel plans for the upcoming holiday season? You may know what means of transportation you will be using, but perhaps you haven't considered the heat treating processes which have gone into creating that transportation.
Today’s Technical Tuesday original content round-up features several articles from Heat TreatToday on the processes, requirements, and tools to keep planes in the air and vehicles on the road, and to get you from one place to the next.
Standards for Aerospace Heat Treating Furnaces
Without standards for how furnaces should operate in the aerospace, there could be no guarantee for quality aerospace components. And without quality aerospace components, there is no guarantee that the plane you're in will be able to get you off the ground, stay in the air, and then land you safely at your destination.
In this article, written by Douglas Shuler, the owner and lead auditor at Pyro Consulting LLC, explore AMS2750, the specification that covers pyrometric requirements for equipment used for the thermal processing of metallic materials, and more specifically, AMEC (Aerospace Metals Engineering Committee).
This article reviews the furnace classes and instrument accuracy requirements behind the furnaces, as well as information necessary for the aerospace heat treater.
Dissecting an Aircraft: Easy To Take Apart, Harder To Put Back Together
Curious to know how the components of an aircraft are assessed and reproduced? Such knowledge will give you assurance that you can keep flying safely and know that you're in good hands. The process of dissecting an aircraft, known as reverse engineering, can provide insights into the reproduction of an aerospace component, as well as a detailed look into the just what goes into each specific aircraft part.
This article, written by JonathanMcKay, heat treat manager at Thomas Instrument, examines the process, essential steps, and considerations when conducting the reverse engineering process.
If you are one of the growing group of North Americans driving an electric vehicle, you may be wondering how - and how well - the components of your vehicle are produced. Electric vehicles (EVs) are on the rise, and the automotive heat treating world is on the lookout for ways to meet the demand efficiently and cost effectively. One potential solution is laser heat treating.
Explore this innovative technology in this article composed by Aravind Jonnalagadda (AJ), CTO and co-founder of Synergy Additive Manufacturing LLC. This article offers helpful information on the acceleration of EV dies, possible heat treatable materials, and the process of laser heat treating itself. Read more to assess the current state of laser heat treating, as well as the future potential of this innovative technology.
When the Rubber Meets the Road, How Confident Are You?
Reliable and repeatable heat treatment of automotive parts. Without these two principles, it’s hard to guarantee that a minivan’s heat treated engine components will carry the family to grandma’s house this Thanksgiving as usual. Steve Offley rightly asserts that regardless of heat treat method, "the product material [must achieve] the required temperature, time, and processing atmosphere to achieve the desired metallurgical transitions (internal microstructure) to give the product the material properties to perform it’s intended function."
TUS surveys and CQI-9 regulations guide this process, though this is particularly tricky in cases like continuous furnace operations or in carburizing operations. But perhaps, by leveraging automation and thru-process product temperature profiling, data collection and processing can become more seamless, allowing you better control of your auto parts. Explore case studies that apply these two new methods for heat treaters in this article.
Those familiar with vacuum heat treatments are surely acquainted with the vacuum heat treatment of titanium and how such furnaces create the ideal environment for titanium's heat treatment. However, not all titanium and its alloys are created equal. Enter the beta titanium alloy.
In this best of the web article from TAV Vacuum Furnaces, discover the potential applications for beta titanium alloys, as well as the effects that various vacuum heat treatments can have on the mechanical properties of the alloy. Additive manufacturing (AM) technologies, specifically laser powder bed fusion, are gaining increased interest in the treatment of beta titanium alloys, due to their efficiency and their cost-cutting potential. Learn more about the chemistry and applications of this unique material below.
An excerpt:
Beta titanium alloys have an unique combination of desirable properties: their high specific strengths, creep resistance, oxidation and corrosion resistance, excellent temperature resistance up to 600°C and hardenability, make them very attractive for aerospace applications. On the other hand, the excellent biocompatibility and low elastic modulus, closer to that of human bone compared to other alloys, make Ti beta alloys an excellent material for biomedical applications.
In December 2022, the first HIP batch on Latin American soil was performed. The journey to success in HIP, as any HIP user will agree, is a bumpy road. What are the challenges that aerospace manufacturers with in house heat treating should be aware of when considering HIP processing? Learn how HT-MX Heat Treat & HIPing — the heat treater who ran the first HIP batch in Latin American history — navigated the transition from small tooling jobs to HIP processing for aerospace parts.
Read the English version of the article below, or find the Spanish translation when you click the flag above right!
This original content article, first published in English and Spanish translations, is found in Heat Treat Today's March Aerospace Heat Treatingprint edition.
Writing this story as the first Latin American company to offer Nadcap accredited hot isostatic pressing brings a flood of memories and images to mind. HT-MX’s beginnings were simple, but also filled with challenges, failures, and lessons. When the company began, we were certain that, though small, we were still a “heat treat plant” and not just a shop.
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Being located in Mexico means that there were large companies with headquarters located far away — potential customers — that would be deciding on their heat treat supplier close to their location. We worked hard to be and to present ourselves as being very professional. But a lesson soon learned was that achieving trust with partners takes a lot more than a good speech and a clean plant.
Unsurprisingly, the first jobs were simple tooling work, like quench and tempering tooling and carburizing gears. A junior engineer and I would drive around in my old hatch-back to local machine shops and pick up a small shaft or gear and bring it back to the plant. We would get so excited when we got the case depth right.
With minimal resources, we decided to complete quality control ourselves. We became friends with a quality manager from a local company, and he came over to help on weekends and after 6:00pm until the audit date came. His knowledge is still in use at HT-MX to this day. I remember celebrating with a “Carne Asada” (a Mexican style barbecue) when we finished that first audit, thinking we had just made a huge step forward, not realizing how far away we still were from our vision.
HT-MX Team
Source: HT-MX Heat Treat & HIPing
But as time passed, we turned our attention to the aerospace industry in Chihuahua, a city with four OEMs. We received the AS9100 certification and started working on Nadcap accreditation. This required time, but by then, a pretty strong engineering team was in action, and successfully obtained Nadcap accreditation in late 2019. Again, we celebrated with a Carne Asada, this time, with a better understanding on where we were and what future challenges we needed to face.
Taking On Hot Isostatic Pressing
HIP system at HT-MX
Source: HT-MX Heat Treat & HIPing
The pandemic hit. Boeing’s 737 Max crisis continued to impact the industry. Moving into aerospace was slow with limited volume, especially compared to what we had seen in the automotive and oil and gas industry. But by now, international companies were more willing to transfer heat treat operations to Mexican suppliers, and we were ready, beginning with running aluminum batches, precipitation hardening, annealing, and other standard processes. It was during this early start to serve the aerospace industry that we heard about hot isostatic pressing (HIP).
Around 2019 during an aerospace cluster event, an OEM with a local presence approached us with their HIP requirements. I had only heard of HIP, but I was immediately interested — until I found out how much one of those machines cost!
But good financing through government programs helped make this HIP project a reality. Timing was not the best, as the federal election in Mexico caused a temporary Mexican currency depreciation, handicapping the project at its beginning.
Getting the proper certifications and validations proved to be a long and complex process, too. Theoretically, we knew what to expect, in terms of getting the Nadcap checklist approved, but the reality was a little different. Gaining Nadcap certification slowly builds a certain culture into any company in its day-to-day activities. Translating that culture into a completely different business unit, new crew, and new process proved to bring its own challenges.
HIP Challenges: Pressure, Temperature, Thermocouples, and Argon Supply
Heat treating usually handles temperature, atmosphere control (or lack of), and regular traceability requirements. HIP, however, adds a few new dimensions to what we usually see: internal pressure, very high temperatures — up to 3632°F (2000°C) — and argon supply. It was the first time HT-MX dealt with a process that incorporated up to 30,000 psi and also used a lot of high purity argon.
Pressure has its own challenges, though the HIP press takes care of those challenges. Still, the internal workings on these kinds of presses are fundamentally different than that of a regular heat treat furnace. Yes, you need to heat it up, but apart from that, it’s not even a furnace but a press. Understanding how the machine works, what happens inside with all that pressure, how it affects the components undergoing hot isostatic pressing, and how it affects the baskets you’re using is a critical learning curve.
High temperatures change everything about running these types of cycles. We work with metals, which means temperatures range between 1832°F and 2372°F (1000°C and 1300°C). This has an impact on thermocouple selection, calibration, and more; with the company’s thermocouple product suppliers based in the U.S., this entails more challenges and extra costs. I have lost count on those urgent same-day trips to the border to retrieve critical spares in time. It’s an 800-km/498-mi roundtrip! We have fortunately found a great supplier that has offered the technical feedback we needed, and we have started to finally understand and control our thermocouple consumption. Although, I must be honest here, we still have a lot to learn in this aspect.
Then, there’s the argon supply. HT-MX never expected it to be a challenge, but it turns out getting the proper supplier — one that understands the requirements and is willing to work with you from validation to production — is key. You might be able to start your validation process using argon transported in gas containers but eventually you will need to switch to liquid argon. That proved to be more difficult than expected. There are not many projects requiring these kind of alliances locally. Getting the right supplier was key and more of a challenge than expected. And then came the lessons on efficiently using the liquid argon, avoiding excessive venting of the tank, and being all around smart with the HIP schedule. This has been a constant learning process, one that has high costs.
Final Hurdles: Certifications, Current Events, and Energy Costs
Once our company had the Nadcap certification, we still needed to get the OEM’s approval for the HIP process, then the approval for the specific version of the HIP process, and then the actual approval for the part numbers.
These approvals were handled by the headquarters’ engineering department and not locally. It was a time-consuming process, with several test runs, lab testing, multiple audits, visits, and more testing, etc. And while all of this was happening, we still had to design the operation, locate critical suppliers not available in Mexico, create alliances with suppliers, etc. Writing this down in a few lines makes it seem simpler and quicker than it really was.
Additionally, in instances like this, Mexican companies, especially small ones, face much more scrutiny than U.S. or European-based companies, and must prove themselves in every single step. It makes sense, even if it feels a little unfair, as HT-MX had no proven track record of high tech processes such as HIP. It does cost extra time, extra care, and sometimes extra testing, but it is the reality we face and we must overcome the extra hurdles.
While navigating HIP approval, the pandemic hit. Months later, the war in Europe began with significant impacts on the cost of energy. Our main clients were high volume and low margin, and with energy prices rising, our competitiveness began to diminish. To adapt and evolve, we decided to add some smaller furnaces for smaller parts, invest in training and increased sales efforts, and focus on AMS/Nadcap-based customers, letting go of major clients. Slowly, things began to turn around.
The First Official HIP Batch in Latin America History
In December 2022, HT-MX ran the first official HIP batch in Latin American history. It was a long time coming. I always thought that running that first batch would feel like reaching the Everest summit. When the day came, it just felt like reaching Everest’s base camp. We still have a long way to go to be truly an established HIP supplier. Now, it’s back to climbing and shooting for that summit, that summit that will perpetually precede the next summit.
There are still several challenges: stabilizing new processes and improving established ones. But I am confident we will move forward in this new stage. And I am so looking forward to the next Carne Asada.
About the Author: Humberto Ramos Fernández is a mechanical engineer with a master’s degree in Science and Technology Commercialization. He has over 14 years of industrial experience and is the founder and current CEO of HT-MX Heat Treat & HIPing, which specializes in Nadcap-certifi d controlled atmosphere heat treatments for the aerospace, automotive, and oil and gas industries. With customers ranging from OEMs to Tier 3, Mr. Ramos has ample experience in developing specific, high complexity secondary processes to the highest requirements.
En diciembre de 2022, se realizó la primera horneada de HIP en suelo latinoamericano. El camino hacia el éxito en HIP, como cualquier usuario de HIP estará de acuerdo, es un camino lleno de baches. ¿Cuáles son los desafíos que deben tener en cuenta los fabricantes aeroespaciales con tratamiento térmico interno al considerar el procesamiento HIP? Aprenda directamente de HT-MX Heat Treat & HIPing, un tratador térmico que ejecutó la primera horneada de HIP en la historia de Latinoamérica, cómo navegaron la transición desde trabajos pequeños de herramentales hasta el procesamiento HIP para piezas aeroespaciales.
Read the Spanish translation of this article in the version below, or see both the Spanish and the English translation of the piece where it was originally published: Heat Treat Today's March Aerospace Heat Treating print edition.
Si quisieras aportar otros datos interesantes relacionados con HIP, nuestros editores te invitan a compartirlos para ser publicados en línea en www.heattreattoday.com. Puedes hacerlos llegar a Bethany Leone al correo bethany@heattreattoday.com
De herramientas simples al tratamiento térmico aeroespacial
Humberto Ramos Fernández Founder and CEO HT-MX
Escribir esta historia de como llegamos a ser la primera compañía latinoamericana en ofrecer prensado isostático en caliente acreditado por NADCAP trae a la mente una avalancha de recuerdos e imágenes. Los comienzos de HT-MX fueron simples, pero también llenos de desafíos, fracasos y lecciones. Cuando comenzamos la compañía, estábamos seguros de que, aunque éramos pequeños, éramos una “planta de tratamiento térmico” y no solo un taller.
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Estando ubicados en México quiere decir que hay grandes plantas con corporativos lejos de aquis — clientes potenciales — que estarían decidiendo sobre su proveedor de tratamiento térmico lejos de nuestra ubicación. Trabajamos arduamente para ser y presentarnos como profesionales y confiables. Pero pronto aprendimos que lograr la confi anza con los clientes requiere mucho más que un buen discurso y una planta limpia.
Como era de esperar, los primeros trabajos fueron trabajos simples de herramentales, algunos templados y revenidos de herramentales y carburizado de engranes. Recuerdo como un ingeniero junior y yo dábamos la vuelta en mi viejo hatchback alrededor de talleres locales y recogíamos un pequeño eje o engranaje y lo llevábamos de regreso a la planta. Nos emocionábamos mucho cuando lográbamos la profundidad de capa correcta.
HT-MX Team Source: HT-MX Heat Treat & HIPing
Con recursos mínimos, decidimos implementar el sistema de calidad nosotros mismos. Nos hicimos amigos de un gerente de calidad de una empresa local, venía a ayudarnos los fines de semana o después de las 6:00 p.m. hasta que llegó la fecha de la auditoría. Su enseñanzas aún se usan en HT-MX hasta el día de hoy. Recuerdo celebrar con una “Carne Asada” cuando terminamos esa primera auditoría, pensando que habíamos dado un gran paso adelante, sin darme cuenta de lo lejos que aún estábamos de nuestra visión.
Con el tiempo, dirigimos nuestra atención a la industria aeroespacial en Chihuahua, una ciudad con cuatro OEMs. Recibimos la certificación AS9100 y comenzamos a trabajar en la acreditación NADCAP. Esto requirió tiempo, pero para entonces contábamos con un equipo de Ingenieros bastante sólido y obtuvimos con éxito la acreditación de NADCAP a finales de 2019. Nuevamente, celebramos con una Carne Asada, esta vez con una mejor comprensión de dónde estábamos y qué futuros desafíos tendríamos que enfrentar.
Entrándole al Prensado Isostático en Caliente
La pandemia llegó. La crisis del 737 Max de Boeing continuó afectando a la industria. Empezar en sector aeroespacial fue lento y con un volumen limitado, especialmente en comparación con lo que habíamos visto en la industria automotriz y de oil&gas. Pero para entonces, las empresas internacionales estaban más dispuestas a trasladar las operaciones de tratamiento térmico a proveedores mexicanos, y estábamos listos, comenzando a procesar aluminio, endurecimiento por precipitación, recocido y otros procesos estándar. Fue durante estos inicios en la industria aeroespacial que escuchamos hablar del prensado isostático en caliente (HIP) por primera vez.
Alrededor de 2019, durante un evento del Cluster Aeroespacial de Chihuahua, un OEM con presencia local se acercó a nosotros con sus requerimientos de HIP. No conocíamos mucho de HIP, pero de inmediato me interesé . . . ¡hasta que descubrí cuánto cuesta una de esas máquinas!
Pero un buen financiamiento a través de programas gubernamentales ayudó a hacer realidad este proyecto de HIP. El momento no fue el mejor, ya que las elecciones federales en México causaron una depreciación temporal de la moneda mexicana, lo que obstaculizó el proyecto al principio.
HIP system at HT-MX Source: HT-MX Heat Treat & HIPing
Obtener las certificaciones y validaciones adecuadas resultó ser un proceso largo y complejo también. Teóricamente, sabíamos qué esperar en términos de obtener la aprobación para el checklist de NADCAP, pero la realidad fue un poco diferente. Obtener la certifi cación de NADCAP construye lentamente una determinada cultura en cualquier empresa en sus actividades diarias. Traducir esa cultura a una unidad de negocio completamente diferente, con un nuevo equipo y un nuevo proceso, demostró traer sus propios desafíos.
Retos en el HIP: presión, temperatura, termopares y argon
El tratamiento térmico generalmente trata de temperatura, control de la atmósfera (o la falta de ella) y los requisitos regulares de trazabilidad. HIP, sin embargo, agrega algunas dimensiones nuevas a lo que normalmente vemos: presión interna, temperaturas muy altas, de hasta 3632°F (2000°C) y suministro de argón. Fue la primera vez que HT-MX lidiaba con un proceso que incorporaba hasta 30,000 psi y también usaba mucho argón de alta pureza.
La presión tiene sus propios desafíos, aunque la prensa de HIP se encarga de ellos. Aún así, el funcionamiento interno en este tipo de prensas es fundamentalmente diferente al de un horno de tratamiento térmico regular. Sí, necesitas calentarlo, pero aparte de eso, no es ni siquiera un horno, sino una prensa. Comprender cómo funciona la máquina, qué sucede dentro con toda esa presión, cómo afecta a los componentes sometidos a prensado isostático en caliente y cómo afecta a las canastas y fi xtures que estás utilizando, es una curva de aprendizaje crítica.
Las altas temperaturas cambian todo sobre el funcionamiento de estos tipos de ciclos. Trabajamos con metales, lo que significa que las temperaturas oscilan entre 1832°F y 2372°F (1000°C y 1300°C). Esto tiene un impacto en la selección de termopares, calibración y más; con los proveedores de termopar basados en EUA, esto implica más desafíos y costos adicionales. He perdido la cuenta cuantos viajes urgentes de ida y vuelta por refacciones a la frontera he hecho. ¡Es un viaje redondo de 800 km! Afortunadamente, hemos encontrado un gran proveedor que nos ha ofrecido la retroalimentación técnica que necesitábamos, y finalmente hemos comenzado a comprender y controlar nuestro consumo de termopares. Aunque, debo ser honesto aquí, todavía tenemos mucho que aprender en este aspecto.
Luego está el suministro de argón. En HT-MX nunca esperamos que fuera un desafío, pero resulta que conseguir el proveedor adecuado, un que entienda los requisitos y esté dispuesto a trabajar contigo desde la validación hasta la producción, es clave. Es posible que puedas iniciar tu proceso de validación usando argón transportado en contenedores de gas, pero eventualmente necesitarás cambiar a argón líquido. Eso resultó ser más difícil de lo esperado. No hay muchos proyectos que requieran este tipo de alianzas a nivel local. Conseguir el proveedor adecuado fue clave y resultó ser un desafío mayor de lo esperado. Y luego vinieron las lecciones sobre cómo utilizar eficientemente el argón líquido, evitar el excesivo venteo del tanque y ser inteligente con el calendario de HIP en general. Esto ha sido un proceso de aprendizaje constante, uno que tiene altos costos.
Últimos obstáculos: certificaciones, eventos globales y costos energéticos
Una vez que nuestra empresa obtuvo la certificación NADCAP, todavía necesitábamos la aprobación de los OEM para el proceso HIP, luego la aprobación para la versión específica del proceso HIP y luego la aprobación real para los números de parte.
Estas aprobaciones fueron manejadas por el departamento de ingeniería del corporativo y no localmente. Fue un proceso que consumió mucho tiempo, con varias pruebas, pruebas de laboratorio, múltiples auditorías, visitas y más pruebas, etc. Y mientras todo esto sucedía, todavía teníamos que diseñar la operación, localizar proveedores críticos que no estaban disponibles en México, crear alianzas con proveedores, etc. Escribir esto en pocas líneas parece más simple y rápido de lo que realmente fue.
Además, en casos como este, las empresas mexicanas, especialmente las pequeñas, enfrentan mucho más escrutinio que las empresas estadounidenses o europeas, y deben probarse en cada paso. Tiene sentido, aunque se siente un poco injusto, ya que HT-MX no tenía un historial comprobado de procesos de alta tecnología como HIP. Cuesta tiempo extra, cuidado adicional y a veces pruebas adicionales, pero es la realidad que enfrentamos y debemos superar los obstáculos adicionales.
Mientras navegábamos en la aprobación de HIP, llegó la pandemia. Meses después, comenzó la guerra en Europa con impactos significativos en el costo de la energía. Nuestros principales clientes eran de alto volumen y bajo margen, y con el aumento de los precios de la energía, nuestra competitividad comenzó a disminuir. Para adaptarnos y evolucionar, decidimos agregar algunos hornos más pequeños para piezas más pequeñas, invertir en capacitación y aumentar los esfuerzos de ventas y enfocarnos en clientes basados en AMS / NADCAP, dejando ir a clientes principales. Poco a poco, las cosas comenzaron a mejorar.
La Primera Horneada Ofi cial de HIP en la Historia de Latinoamérica
En diciembre de 2022, HT-MX llevó a cabo la primera horneada oficial de HIP en la historia de Latinoamérica. Tomo bastante tiempo. Siempre pensé que hacer esa primera horneada se sentiría como llegar a la cima del Everest. Cuando llegó el día, solo se sintió como llegar al campamento base del Everest. Todavía nos queda mucho camino por recorrer para ser realmente un proveedor de HIP establecido. Ahora, volvemos a escalar y apuntamos a esa cima, esa cima que perpetuamente precederá a la próxima cima.
Todavía hay varios desafíos: estabilizar nuevos procesos y mejorar los establecidos. Pero estoy seguro de que avanzaremos en esta nueva etapa. Y estoy muy emocionado por la próxima Carne Asada.
Acerca del Autor:Humberto Ramos Fernández es un ingeniero mecánico con una maestría en Ciencia. Tiene más de 14 años de experiencia industrial y es el fundador y actual CEO de HT-MX Heat Treat & HIPing, que se especializa en tratamientos térmicos de atmósfera controlada, con certifi cación NADCAP, para las industrias aeroespacial, automotriz y de petróleo y gas. Con clientes que van desde OEM hasta Tier 3, el Sr. Ramos tiene una amplia experiencia en el desarrollo de procesos secundarios específi cos de alta complejidad para los requisitos más exigentes.
What is the connection between AMS2750 specifications and furnace classifications? With tight specifications, what does the heat treater need to know to be compliant? Follow along as we take a brief look into this often-overlooked topic.
This Technical Tuesday article, written by Douglas Shuler, owner and lead auditor, Pyro Consulting LLC, was first published in Heat Treat Today's March 2023 Aerospace Heat Treating print edition.
Doug Shuler Lead Auditor Pyro Consulting
AMS2750 is the specification that covers pyrometric requirements for equipment used for the thermal processing of metallic materials. AMEC (Aerospace Metals Engineering Committee) is one of the committees which oversees the changes and revisions of AMS2750. There are five main sections in the technical requirements of the specification: sensors, instrument calibrations, thermal processing classification, SAT (system accuracy testing), and TUS (temperature uniformity surveys). Additionally, there are quality provisions that detail what happens if a calibration or test is either past due or fails.1
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Revisions to the original requirements have occurred over the years, with the newest being Revision G. The structure of Revision G has carried over from Revision F and has remained the current structure of the AMS2750 specification. This structure includes furnace classes, which are based on the minimum requirements for temperature uniformity.
Furnace classes are defined in Figure A of Revision D Figure 1.
Figure 1. AMS2750G furnace class uniformity tolerances Source: Doug Shuler
Originally, furnace classes were based on temperature uniformity, but also subzero transformation, refrigerated storage of aluminum alloys, and embrittlement relief, Figure 2.
Figure 2. Original AMS2750 instrument accuracy requirements, no class structure Source: Doug Shuler
AMS2750 Revision C was released in May 1990 and started to implement the class and instrumentation type structure and differentiated between furnaces for heat treating parts versus furnaces for heat treating raw materials. Furnaces for heat treating parts were classified based on uniformity, but also on a readability requirement. Furnaces for heat treating raw materials were classified based on a readability requirement alone.
AMS2750 Revision D was released in September 2005 and continued to define equipment class (Figure A)* and instrumentation type (Section 3.3.1.1)*. It also clarified chart recorder resolution (Table 4)*, print and chart speed (Table 5)*, and testing frequencies for SAT (Tables 6, 7)* and TUS (Tables 8, 9)* for the processing of parts versus raw materials.
AMS2750 Revision E was released in July 2012 and continued to build on the clarity presented in Revision D by adding an instrumentation type table (Figure 3)* instead of a simple text description in the body of the specification.
Figure 3. AMS2750 Revision C: distinguishment between furnaces for heat treating parts versus raw materials Source: Doug Shuler
Moving to AMS2750 Revision F, the specification saw a major rewrite and restructuring where the tables were moved from the end of the document to the first area text that called out the specific table. Revision F also put into place a sunset date for analog instruments.
That brings us to the current revision of AMS2750, Revision G, which has carried forward the structure of Revision F and only sought to further clarify the intent of the requirements.
Over the years, the technology of sensor, instrument, and furnace manufacture and capability has continued to produce better and tighter controls for the process of heat treating. The evolution of AMS2750 has recognized these advancements and has kept pace with them in technology. The understanding of the origins of AMS2750 and how it has evolved is vital in understanding its application to today’s heat treat special processes.
*Specified figure, table, or section is associated with the AMS2750 revision being discussed.
About the Author: In 2009, Douglas (Doug) Shuler became the owner of Pyro Consulting LLC and also began working with Performance Review Institute (PRI), first as an instructor and course developer and later as an auditor for the Nadcap program. As a lead auditor for Nadcap, he has conducted over 380 Nadcap special process and aerospace quality management system audits on behalf of the Aerospace Primes over the past 10+ years. Doug continues to focus on instruction, training, and education for the heat treat industry, developing courses, authoring exams, and employing the PIE method: “Procedures that Include all requirements, and Evidence to show compliance.”
What are the factors that lead to carburization and carbon transmission? How can heat treater avoid these unwanted reactions? Discover the challenges of CFC fixtures and the steps heat treaters can take to mitigate these challenges.
This Technical Tuesday article, written by Dr. Jorg Demmel, founder, 0wner, and president, High Temperature Concept, was first published in Heat Treat Today's March 2023 Aerospace Heat Treating print edition.
Introduction
Dr. Jorg Demmel Founder, Owner, President High Temperature Concept
The main advantages of CFC fixtures were introduced in “CFC Fixture Advantages and Challenges in Vacuum Heat Treatment, Part 1,” which was released in Heat Treat Today’s November 2022 publication. This included a discussion of the limits of CFC in vacuum and protective atmosphere heat treatment. Successful applications of CFC workpiece carriers in heat treatment were presented along with field test results that included a brief discussion of undesired contact reactions (i.e., carburization and melting of parts). In Part 2 of this paper, the mechanisms involved with carburization and carbon transmission due to direct contact of parts with CFC fixtures will be further explained.
Mass Transfer from CFC Fixtures
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The mass transport of carbon from CFC fixtures into steel parts at high temperatures will be examined in the following areas:
Reactions in oxygen (i.e., the reaction medium)
Transport of carbon in CFC during exposure to oxygen
Transfer mechanism into the steel parts
Diffusion of carbon into the steel parts
Part reactions (melting, carbide formation)
Figure 1: 1.6582 steel samples and GDEOS depth profile analysis Source: Dr. Jorg Demmel, High Temperature Concept
CFC samples were tested in contact with steel samples under laboratory conditions in a vacuum of 7.5 x 10-7 Torr (1 x 10-6mbar). Results of the contact with CFC for steel samples at different temperatures are presented to the left (Figure 1). It is important to note that:
Sample (0) is the reference sample and had no exposure to the contact test.
Sample (0’) is the back side of Sample (0).
Sample (1) is the contact side at 1922°F (1050°C).
All three samples are visually identical, therefore only one is shown. Sample (2) at 1967°F (1075°C) and Sample (3) at 2012°F (1100°C) exhibited a distinct visual surface pattern after CFC contact. This was analyzed by Glow Discharge Optical Emission Spectroscopy (GDOES) and the test location (gray spot) clearly observed on Samples (2) and (3). For Sample (4) run at 2057°F (1125°C), the CFC was found to have adhered to the steel surface.
The carbon content in 10mm depth measured with GDOES (see the profiles in Figure 1) increased from initially 0.29 weight-% for the 1922°F (1050°C) test, although nothing was visible on metal surfaces. For carbon contents, see Table 1.
Table 1. Carburizing of 1.6582-samples in 10 µm depth after CX-27C1-contact (GDOES) Source: Dr. Jorg Demmel, High Temperature Concept
CFC Reactions with Oxygen
The chemical reactions of CFC with various gases are essential in Step 1 (referenced in Part 1 of this article) and an indicator of chemical thermal suitability.
In the case of the unwanted contact carburization considered above is similar, in a sense, to carburization of steel in contact with carbon powder or granulate. However, the actual carburization mechanism, which occurs between approximately 1616°F and 1697°F (880°C and 925°C), does not take place directly via the carbon contact but is based on the fact that solid carbon reacts with atmospheric oxygen according to the Equation Table to form carbon dioxide (CO2).
Equation Table. Reaction rates and activation energies for graphite (800°C; 0.1 bar) Source: Dr. Jorg Demmel, High Temperature Concept
Carbon monoxide (CO) is then formed from CO2 by the Boudouard reaction (Equation 3). At high temperatures and low pressures (see Figure 2), almost only CO is present.
Figure 2. Boudouard equilibrium Source: Dr. Jorg Demmel, High Temperature Concept
Transport of Carbon
The carbon carrier must be transported to the surface of the parts.
The cases considered in Part 1 of this article were conducted in vacuum, that is in the absence of a carburizing atmosphere. The laboratory tests were even carried out in a vacuum as low as 7.5 x 10-7 Torr (1 x 10-6mbar). Nevertheless, part surface reactions were observed.
Transfer Mechanism into the Steel Parts
Theoretically, carbon from the CFC fixtures can be transferred into the steel via solid phase (as opposed to gaseous phase) reactions. Gas particles can be adsorbed by surfaces via physisorption and/or chemisorption. The author’s personal research experience has shown that metal samples usually oxidize after a short time, even in a high vacuum of 7.5 x 10-7 Torr (1 x 10-6mbar). In particular, elements such as iron, molybdenum, and chromium have a strong ability to chemically adsorb oxygen or CO.
Furthermore, there is a disproportionately large amount of adsorbed oxygen in the CFC samples. CFC has open porosities as high as 30%. CFC in industrial practice is never completely evacuated. So, there is a disproportionately large amount of oxygen present in CFC fixtures.
It can be assumed that oxygen repeatedly escapes from the CFC and is initially available in the contact area. Proof of this can be provided by the GDOES analysis. Outside the contact areas, no (gas) carburization took place (as evidenced by the non-contact side of steel samples).
The oxygen and carbon surplus combined with close contact lead to complete reaction of oxygen creating carbon dioxide as in Equation (1). Because of the carbon surplus, almost only carbon monoxide is produced as shown in Equation (2). Because of the very close contact between CFC and steel, C-adsorption by gamma iron and desorption of carbon dioxide as in Equation (5) takes place:
Equation 5 Source: Dr. Jorg Demmel, High Temperature Concept
Since carbon dioxide immediately comes in contact with carbon in the CFC again, carbon monoxide is produced according to Equation (3). In other words, carbon dioxide regenerates immediately and the reaction starts again.
Direct carbon transfer from CFC to metal via solid phase is very unlikely since carbon atoms in CFC are firmly bound in rings.
Diffusion of Carbon in the Steel Parts
In solids, the surface diffusion usually takes place at significantly higher diffusion rates than in the bulk material. The thermodynamic driving force of diffusion or carburizing reactions is the difference in carbon activity for a specific concentration in the austenite to that of the reaction medium. The carbon activity is the ratio of the vapor pressure of the carbon in state under consideration to vapor pressure of pure carbon (graphite/CFC). Alloying elements of the steel influence the activity of the carbon.
Part Reactions (Melting and Carbide Formation)
Steel can begin to melt if, at the given values for temperature and pressure, a partially liquid phase is reached, that is, the solidus line in the phase diagram is exceeded. At even higher temperatures, the liquidus temperature can be reached and steel is completely liquid.
According to metastable iron-carbon diagram phase diagram (Figure 3), a steel such as SAE/ AISI 4340 (34CrNiMo6) alloy (DIN 1.6582) with around 0.47% by weight percent carbon does not begin to melt at 1922°F (1050°C), the exposure temperature for Sample (1), or Sample (2) at 0.56% and 1967°F (1050°C) for Sample (3) with 0.67% for 2012°F (1100°C). The iron-iron carbide phase diagram applies to steels with less than 5% (by mass) of alloying elements and thermodynamic equilibrium, so it is an accurate representation for a SAE/AISI 4340 (34CrNiMo6) alloy.
Figure 3. Metastable equilibrium diagram Fe-Fe3C for steel (good fit for 1.6582) Source: Dr. Jorg Demmel, High Temperature Concept
A calculation of the solidus temperature shown on the iron-iron carbide diagram (Figure 3), which is dependent on the carbon content and alloying elements, yields a value of 2703.2°F (1,484°C) (J’).
For an SAE/AISI 4340 (34CrNiMo6) steel (DIN 1.6582) with 0.3% C and one for 0.5% C, the calculated solidus temperature is 2640°F (1449°C). This is shown on the J’-E’ blue dotted line in Figure 3. In other words, a lower solidus line (cf. dashed blue line in Figure 3) and thus a slight reduction in austenite phase region.
The iron-carbon diagram also indicates that melting of surfaces that have absorbed carbon (e.g., Sample No. 2) will occur at 1967°F (1075°C). This value is within approximately 90°F (50°C) of the temperature used (dotted line E’-C’-F’). From this information we can conclude that the observations seen in Figure 1 are not the result of melting, but rather imprints due to surface softening.
The melting (c.f., Figure 1) observed in Test No. 4, which occurred at 2057°F (1125°C) is likely due to partial carburization of the steel surface and exceeding the solidus temperature. A micrograph confirms eutectic melting and high carbon content, which could also be indirectly confirmed by hardness measurement.
Carbide Formation
Additional reactions can occur between carbon absorbed from the CFC fixtures and the steel parts due to either separation of carbides (e.g., iron carbide in the form of secondary cementite) or carbide formation with alloying elements such as Ti, V, Mo, W, Cr, or Mn (listed in decreasing tendency to form carbides).
Table 2. Reactions between C and metal Source: Dr. Jorg Demmel, High Temperature Concept
Table 2 lists various elements in alphabetical order that react with carbon above the specified temperatures to form reaction products mentioned, primarily carbides. It should be noted that the temperatures listed apply only to pure metals and pure carbon. As such, they provide only rough approximations of a temperature at which a reaction might begin.
Countermeasures
There are several measures to avoid these unwanted reactions:
Ceramic oxide coatings such as aluminum oxide (Al2O3) or zirconium oxide (ZrO2) layers placed onto the CFC
Hybrid CFC fixtures having ceramics in key areas to avoid direct contact with metal workpieces
Alumina composite sheets
Boron nitride sprays
Special fixtures made of oxide ceramics
An yttrium-stabilized zirconium oxide layer (93/7) was applied to CF222 by thermal plasma spray and tested successfully (see Figure 4).
Figure 4. Yttrium-stabilized zirconium oxide layer with an average layer thickness of 110µm on CF222 material. The photograph on the right shows a hybrid CFC fixture. Source: GTD Technologie Deutschland
Summary
It is important to consider the specific process conditions in advance so that unwanted reactions — from carburization to catastrophic melting of the workpieces — can be avoided. Effective countermeasures can be taken.
References
Atkins, P. W.: Physikalische Chemie. 1. vollst. durechges. u. berichtigter Nachdr.d. 1. Aufl ., Weinheim, VCHVerlag, 1988 – ISBN 3-527-25913-9.
Bürgel, R.: Handbuch Hochtemperatur-Werksto technik: Grundlagen, Werksto bean-spruchungen, Hochtemperaturlegierungen. Braunschweig, Wiesbaden: Vieweg, 1998. ISBN 3-528-03107-7.
Demmel, J.: Advanced CFC-Fixture Applications, their scientific challenges and economic benefits, In: 30th Heat Treating Society Conference & Exposition, Detroit, MI, USA, 15th Oct. 2019.
Demmel, J.: Werkstoffwissenschaftliche Aspekte der Entwicklung neuartiger Werkstückträger für Hochtemperaturprozesse aus Faserverbundkeramik C/C und weiteren Hochtemperaturwerkstoffen, Dissertation, TU Freiberg, Germany, 2003.
Demmel, J.: Why CFC-Fixtures are a Must for Modern Heat Treaters, FNA 2020 Technical Session Processes & Quality, USA, 30th Sept. 2020.
Demmel, J., et al: Applications of CMC-racks for high temperature processes. In: 4th Int. Conf. on High-Temperature Ceramic Matrix Composites, 3.10.2001, p. A-17.
Demmel, J. und J. Esch: Handhabungs-Roboter sorgt für Wettbewerbsvorsprung. Härterei: Symbiose von neuen Werkstoffen und Automatisierung. In: Produktion (1996), No. 16, p. 9.
Demmel, J. und U. Nägele: CFC revolutioniert die Wärmebehandlung. In: 53. Härterei-Kolloquium, Wiesbaden, 10.10.97. Vortrag und Tagungsbericht.
Demmel, J., Lallinger, H.: CFC-Werkstückträger revolutionieren die Wärmebehandlung. In: Härtereitechnische Mitteilungen 54, No. 5, p. 289-294, 1999.
Eckstein, H.-J., et al: Technologie der Wärmebehandlung von Stahl. 2nd Edition, VEB Deutscher Verlag für Grundstoffindustrie, Leipzig, 1987. ISBN 3-342-00220-4.
Godziemba-Maliszewski, J.; Batfalsky, P.: Herstellung von Keramik-Metall-Verbindungen mit Diffusionsschweißverfahren. In: Technische Keramik, Jahrbuch, Essen, 1 (1988), S. 162-172. ISBN 3-80272141-1.
Grosch, J.: Grundlagen-Verfahren-Anwendungen-Eigenschaften einsatzgehärteter Gefüge und Bauteile, ExpertVerlag, 1994, ISBN 3-8169-0739-3.
Hollemann, A.F.; Wiberg, E.: Lehrbuch der anorganischen Chemie / Hollemann-Wiberg. 91.-100. Aufl ., de Druyter Verlag, 1985 – ISBN 3-11-007511-3.
Kriegesmann, J.: Technische Keramische Werkstoffe. Loseblattwerk mit 6 Ergänzungslieferungen pro Jahr.
Kussmaul, K.: Werkstoffkunde II. Stuttgart, Universität, Lehrstuhl für Materialprüfung, Werkstoffkunde und Festigkeitslehre, Vorlesungsmanuskript, 1993.
Lay, L.: Corrosion Resistance of Technical Ceramics. 1. Aufl ., Teddington, Middlesex, Crown-Verlag, 1983 – ISBN 0-11-480051-0.
Marsh, H.; u.a.: Introduction to Carbon Science. 1. Aufl ., London, Butterworths-Verlag, 1989 – ISBN 0-40803837-3.
Spur, G.: Wärmebehandeln. Berlin, 1987, ISBN 3-446-14954-6.
Samsonow, G.V.: Handbook of refractory compounds. New York, 1980.
Schulten, R.: Untersuchungen zum Kohlenstofftransportmit Carbidbildung in Nickelbasis-legierungen. RWTH Aachen, Fakultät für Maschinenbau, Diss., 1988 Deutsche Keramische Gesellschaft, 1990 following. ISBN 3-87156-091-X.
About the Author: Dr. Jorg Demmel is the founder, owner, and president of High Temperature Concept. He received his Engineering Doctorate in the field of CFC workpiece carriers for heat treatment and served in different leading positions for Volkswagen before moving to the U.S. In this article, Demmel draws on his dissertation, “Material scientific aspects of the development of new Fixtures for high temperature processes made of fiber-composite ceramics C/C and other high temperature materials” (Technical University Mining Academy Freiberg, Germany, 2002/3), and his personal experiences. For more information, contact Jorg at jorg.demmel@high-temperature-concept.com
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