High Pressure Gas Quenching

Case Study: Heat Treat Equipment Meets the Future Industry Today

OCModern industry trends and expectations pose new challenges to heat treating equipment; in addition to the expected requirements (e.g., safety, quality, economy, reliability, and efficiency), factors like availability, flexibility, energy efficiency, environmental, and the surrounding carbon neutrality are becoming increasingly important.

Maciej Korecki, vice president of Business Development and R&D at SECO/WARWICK, presents this special Technical Wednesday case study for the last day of FNA 2022 to focus on an equipment solution that meets these modern industry demands: a semi-continuous vacuum furnace for low-pressure carburizing (LPC) and high-pressure gas quenching (HPGQ).


Maciej Korecki
Vice President of Business of the Vacuum Furnace Segment
SECO/WARWICK

Introduction

At least 60 years ago, vacuum furnaces first appeared in the most demanding industries (i.e., space and aerospace), then spread to other industrial branches, and are now widely implemented in both mass production and service plants. Use of vacuum technology does not look like it is slowing down anytime soon.

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The driving forces behind this growth in vacuum technology are two-fold: first, the increasing heat treatment requirements that result from the directions of industrial development and production systems, and second, environmental protection, where the advantages of vacuum technologies are undeniable.

 

Traditional Atmospheric Technology

Case hardening by carburizing is one of the most widely used heat treatment technologies. It consists in carburizing (introducing carbon to the surface) followed by quenching of the carburized layer. Typically, the work is carburized in a mixture of flammable gases (CO, H2), and quenched in oil in an atmosphere furnace, using methods developed in the 1960s.

These methods have a history of development, though the question remains if the technological developments can keep up with the requirements of modern industry. Safety is an issue with this method due to the use of flammable (and poisonous) gases and flammable oil, as well as open flame, which in the absence of complete separation from the air can lead to fire, or poisoning.

In addition, they affect their environment by releasing significant amounts of heat, polluting the surroundings with quenching oil and its vapors. They require the use of washers and cleaning chemicals, emit annually tens or even hundreds of tons of CO2 (greenhouse gas, the main culprit of global warming and dynamic climate change) coming from the carburizing atmosphere, and for these reasons, they need to be installed in dedicated so-called “dirty halls” separated from other production departments.

The resulting requirement to limit the temperature of the processes to 1688-1706 oF (920-930oC) is also not without importance, as it blocks the possibility of accelerating carburization and increasing production efficiency (due to the use of metal alloys in the construction, the service life of which drops dramatically at higher temperatures) and the formation of unfavorable intergranular oxidation (IGO), which is a characteristic feature of the atmospheric carburizing method.

Quenching in oil is effective, but it does not have precise controllable, repeatable, and ecological features that heat treaters may need. Due to the multiphase nature of oil quenching (steam, bubble, and convection phase) and the associated extremely different cooling rates, it is characterized by large and unpredictable deformations within a single part and the entire load. Furthermore, there is no practical method to influence and control the quench process.

Modern Vacuum Technology with LPC and HPGQ

Vacuum carburizing appeared as early as the 1970s, but it could not break through for a long time due to the inability to control and predict the results of the process, and heavy contamination of the furnaces with reaction products.

The breakthrough came in the 1990s, when acetylene began to be used as a carbon-bearing gas and computers were employed to control and simulate the process. Since the beginning of the 21st century, there has been a rapid development of the low pressure carburizing (LPC) technology and an increase in its industrial demand, which continues today with an upturn.

Vacuum carburizing occurs with the aid of hydrocarbons (usually acetylene), which catalytically decompose at the surface, providing carbon that diffuses into the material. The process is carried out under negative pressure (hundreds of times less than atmospheric pressure) and is very precise, efficient, and uniform due to the very high velocity and penetration capacity of the gas molecules, allowing the carburizing of large and densely packed loads and hard-to-reach surfaces such as holes.

In addition, the use of non-oxygen-containing hydrocarbon atoms eliminates the qualitative problem of intergranular oxidation (IGO). The process is completely safe, there is no flammable or poisonous atmosphere in the furnace and no open flame, and the furnace can work unattended and is fully available and flexible, i.e., it can be turned on and off on demand, which does not require any preparation. Similarly, changing the carburizing parameters takes place efficiently.

Due to the design of the vacuum furnace and the use of materials with high resistance to temperature, i.e., graphite — the only limitation for the temperature of the carburizing process is the steel from which the parts are made — it is possible to carburize at higher temperatures than traditional methods allow. The result is a significantly shorter carburizing time and increased furnace efficiency versus what can be achieved in an atmosphere furnace.

Neutral gas cooling was included with the vacuum furnaces. Initially, engineers used a cooling gas (nitrogen or argon) at near ambient pressure and natural convection. Subsequent solutions introduced fan-forced gas flow in a closed circuit. The cooling efficiency under such conditions was hundreds of times lower compared to that of oil, allowing only high-alloy steels and parts with very limited cross-sections to be hardened. Over the following decades, the development of HPGQ was focused on improving cooling efficiency by increasing pressure and velocity and using different types of gas and their mixtures. Current systems have cooling efficiencies on a par with oil-based systems and enable the same types of steel and parts to be hardened, with the advantage that deformation can be greatly reduced and reproducible, and the process is completely controllable (through pressure and gas velocity) allowing any cooling curve to be executed.

Vacuum technologies have an ecological edge. Because of their design and processes, vacuum furnaces do not interfere with the immediate surroundings and are environmentally friendly, so they can be installed in clean halls, directly in the production chain (in-line). They emit negligible amounts of heat and post-process gases which are not poisonous and contain no CO 2 at all. Gas quenching eliminates harmful quenching oil and the associated risk of fire and contamination of the immediate environment, as well as the need for equipment and chemicals for its removal and neutralization. Nitrogen used for cooling is obtained from the air and returned to it in a clean state, creating an ideal environmentally friendly solution.

The presented advantages of vacuum technologies influence its dynamic development and increase the demand of modern industry, and the gradual replacement of atmospheric technologies.

Vacuum furnaces are available in virtually any configuration: horizontal, vertical, single, double, or multi-chambered, tailored to the process and production requirements. In light of recent global changes, requirements, and industrial trends, special attention should be paid to disposable, flexible, and rapidly variable production and process systems, as well as independent and autonomous systems, which include a three-chamber vacuum furnace for semi- continuous heat treatment, equipped with LPC and HPGQ.

Three-Chamber Vacuum Furnace — CaseMaster Evolution Type CMe-T6810-25

This is a compact, versatile, and flexible system designed for vacuum heat treatment processes for in-house and commercial plants, dedicated to fast-changing and demanding conditions in large-scale and individual production (Fig. 1). It enables the implementation of case hardening by LPC and HPGQ processes and quenching of typical types of oil and gas hardened steels and allows for annealing and brazing. It is characterized by the following data:

  • working space 610x750x1000 mm (WxHxL)
  • load capacity 1000 kg gross
  • temperature 2282oF (1250oC)
  • vacuum range 10-2 mbar
  • cooling pressure 25 bar abs
  • LPC acetylene gas
  • Installation area 8x7m

The furnace is built with three thermally and pressure-separated chambers (Fig. 2.), and operates in a pass-through mode, loaded on one side and unloaded on the other, simultaneously processing three loads, hence its high efficiency. The load is put into the pre-heating chamber, where it is pre-heated to the temperature of 1382oF (750oC), depending on the requirements: in air (pre-oxidation), nitrogen or vacuum atmosphere. It is then transferred to the main heating chamber, where it reaches process temperature and where the process is carried out (e.g., LPC).

In the next step, the charge is transported to the quenching chamber, where it is quenched in nitrogen under high pressure. All operations are automatic and synchronized without the need for operator intervention or supervision.

Fig. 2. Construction and schematic furnace cross-section CMe-T6810-25.
Source: SECO/WARWICK

Particularly noteworthy is the gas cooling chamber, which in nitrogen (rather than helium) achieves cooling efficiencies comparable to oil (heat transfer coefficient >> 1000 W/m2K), thanks to the use of 25 bar abs pressure and hurricane gas velocities in a highly efficient closed loop system. The cooling system is based on two side-mounted fans with a capacity of 220 kW each, forcing with nozzles an intensive cooling nitrogen flow from above onto the load, then through the heat exchanger (gas-water), where the nitrogen is cooled and further sucked in by the fan (Fig. 3). The cooling process is controllable, repeatable, and programmable by gas pressure, fan speed and time. An intense and even cooling is achieved. The result is the achievement of appropriate mechanical properties of parts with minimal hardening deformations, without the use of environmentally unfriendly oil or very expensive helium.

Fig. 3. Cross-section of the furnace CMe-T6810-25 cooling chamber.
Source: SECO/WARWICK

An integral part of the furnace system is the SimVaC carburizing process simulator, which enables the design of furnace recipes without conducting proof tests.

Distinctive Features of the CMe-T6810-25 Furnace

The advantages of this type of furnace — versus more traditional or past forms — can be demonstrated in a number of usability and functional aspects, the most important of which are the following:

Safety:

  • Safe, no flammable and poisonous atmosphere
  • No open fire

Production and installation:

  • Intended for high volume production (two to three times higher output when compared to single- and double-chamber furnaces)
  • Effective and efficient LPC (even five times faster than traditional carburizing)
  • Total process automation & integration
  • Clean room installation
  • Operator-free
  • Compact footprint

Quality:

  • High precision and repeatability of results
  • Uniform carburizing of densely pack loads and difficult shapes (holes)
  • No decarburization or oxidation
  • Elimination of IGO
  • Ideal protection and cleanliness of part surfaces
  • Accurate and precise LPC process simulator (SimVaC)

Quenching:

  • Powerful nitrogen quenching (neither oil nor helium is needed)
  • Reduction of distortion
  • Elimination of quenching oil and contamination
  • Elimination of washing and cleaning chemicals

Operational:

  • Flexible, on-demand operation
  • No conditioning time
  • No human involvement and impact
  • High lifespan of hot zone components — i.e., graphite
  • No moving components in the process chamber

Ecology:

  • Safe and environmentally friendly processes and equipment
  • No emission of harmful gases (CO, NOx, SOx)
  • No emission of climate-warming gas CO2

Based on the CMe-T6810-25 furnace performance, it is rational and reasonable to build heat treatment systems for high-efficiency and developmental production in a distributed system by multiplying and integrating further autonomous and independent units. The reasons for doing so are because the furnace design affords:

  • No risk of production total breakdown
  • Unlimited operational flexibility
  • Less initial investment cost
  • Unlimited multiplication
  • No downtime while expansion
  • Independent quenching chamber
  • Independent transportation
  • Independent control system

The characteristics, capabilities and functionalities of the CMe-T6810-25 furnace fit very well with the current and developmental expectations of modern industry and ecological requirements, which is confirmed by specific implementation cases.

Case Study

The three-chamber CaseMaster Evolution CMe-T6810-25 vacuum furnace was installed and implemented for production at the commercial heat treatment plant at the Polish branch of the renowned Aalberts surface technologies Group in 2020.

Fig. 4. Gearwheel used in the case hardening process.
Source: SECO/WARWICK

The CMe furnace, together with the washer and tempering furnace, forms the core of the department's production, which is why the furnace is operated continuously. Last year, the furnace performed over 2000 processes and showed very high quality (100%) and reliability (> 99%) indicators. The very high efficiency of the furnace was also confirmed, which, with relatively low production costs, contributes to a very good economic result.

The case hardening process on gearwheels used in industrial gearboxes was taken as an example. The wheel had an outer diameter of about 80 mm and a mass of 0.52 kg (Fig. 4), and the load consisted of 1344 pieces densely packed in the working space (Fig. 5) with a total net weight of 700 kg (920 kg gross) and 25 m2 surface to be carburized. The aim of the process was to obtain an effective layer thickness from 0.4 – 0.6 mm with the criterion of 550 HV, surface hardness from 58 – 62 HRC (Rockwell Hardness C), core hardness at the gear tooth base above 300 HV10 and the correct structure with retained austenite below 15%.

Fig. 5. A photograph of the arrangement of gearwheels in the load.
Source: SECO/WARWICK

The LPC process was designed using the SimVaC® simulator at a temperature of 1724oF (940oC) and a time of 45 min, with 3 stages of introducing carburizing gas (acetylene), obtaining the appropriate profile of carbon concentration in the carburized layer, with a content of 0.76% C on the surface (Fig. 6).

The process was carried out in the CMe-T6810-25 furnace and had the following course from the perspective of a single load (Fig. 7):

  1. Loading into a pre-heating chamber, heating and temperature equalization in 1382oF (750oC) (100 min in total).
  2. Reloading to the main heating chamber, heating and temperature equalization in 1724oF (940oC), LPC, lowering and equalizing the temperature before quenching in 1580oF (860oC), reloading to the cooling chamber (total 180 min).
  3. Gradual quenching at a pressure of 24, then 12 and 5 bar, discharge of the load from a quenching chamber (total of 25 min).

The load stayed the longest in the main heating chamber – for 180 minutes. This means that with the continuous operation of the furnace in this process, the cycle will be just 180 minutes, i.e., once every three hours the raw load will be loaded, and the processed load will be removed from the furnace.

In the next step, the parts underwent tempering at a temperature of 160oC.

The result of the process was tested on ten parts taken from the reference corners and from the inside of the load. The correct layer structure (Fig. 8) and hardness profile (Fig. 9) were achieved, and all the requirements of the technical specification were met (Tab. 1).

Tab. 1. Comparison of the parameters required and obtained in the process.
Source: SECO/WARWICK

During the process, the consumption of the costliest energy factors was monitored and calculated, and the results per one load are as follows:

  • Electricity – 550 kWh
  • Liquid nitrogen – 160 kg
  • Acetylene – 1.5 kg
  • CO2 emissions – 0 kg

Cooling water and compressed air consumption have not been included as they have a negligible impact on process costs.

Summary: Efficiency and Economy

As a result of the process, all technological requirements have been met, obtaining the following indicators of efficiency and consumption of energy factors calculated for the entire load and per unit net weight of the load (700 kg):

  • Capacity: 3h/load; 233 kg/h; 5 thousand tons/year (6500 h)
  • Electricity: 550 kWh; 0.79 kWh/kg
  • Liquid nitrogen: 160 kg; 0,23 kg/kg
  • Acetylene: 1,5 kg; 2,1 g/kg
  • CO2 emissions : 0 kg; 0 kg/kg

On this basis, it is possible to estimate the total cost of energy factors in the amount of approximately EUR 100 per load or approximately EUR 0.14/kg of net load (assuming European unit costs of 2021). It is important that these costs are not burdened by CO2 emission penalties, as can happen with more traditional furnaces.

To sum up the economic aspect, based on an example process, a CMe furnace capacity of 1,500 net tons of parts per year was achieved for 6500 hours of annual furnace operation, at a cost of energy factors of about 100 EUR per load, or 0.14 EUR per kg of parts. The economic calculation is very attractive, and the return on investment (ROI) is estimated at just a few years.

Conclusion

While the advantages of this type of vacuum application are clear from this case study, the example discussed here does not represent the full capabilities of the CMe-T6810-25 furnace, even this process can be optimized and shortened, thereby increasing the furnace's efficiency, and reducing costs. It is possible to carry out carburizing processes (LPC) or hardening alone in a 1.5 h cycle, which would double the capacity of the furnace and similarly reduce the cost of energy factors and shorten the ROI time.

 

For more information:

Go to www.secowarwick.com


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Medical Heat Treater Receives “A to Z” HIPing Solution

HTD Size-PR Logo A hot isostatic press (HIP) was recently delivered to T.A.G. Medical Products Corporation Ltd. (TAGMPC), a manufacturer of medical and dental solutions that improve surgical procedures. The HIP will ensure the production of implants and surgical tools with the optimal material properties required by the exacting environments in which they are used.

Ran Weizman
Executive Vice President
T. A. G. Medical Products Corporation

"To increase production capacity, we invested in a new MIM (metal injection molding) production line," states Ran Weizman, Executive VP at TAGMPC. "The [Quintus Technologies] press will serve us for the implants and minimal cutting tools production, where high material uniformity and good mechanical properties are required."

Advanced proprietary features such as High Pressure Heat Treatment™ (HPHT™) and Uniform Rapid Quenching (URQ®) enable the Quintus press model QIH 15L to produce finished MIM parts with maximum theoretical density, ductility, and fatigue resistance. Incorporating heat treatment and cooling in a single process, HPHT combines stress-relief annealing, HIP, high-temperature solution-annealing (SA), high pressure gas quenching (HPGQ), and subsequent ageing or precipitation hardening (PH) in one integrated furnace cycle.

"All T.A.G. manufacturing processes, from A to Z, are done under one roof. Therefore, it is important for us to work with equipment that gives us this option,” Mr. Weizman comments.

With a new emphasis on disposable surgical instruments in the TAGMIM production chain, faster throughput and higher workpiece quality are also essential. The QIH 15L’s URQ capability achieves a cooling rate of >80K/s while minimizing thermal distortion and non-uniform grain growth. The press’s furnace chamber has a diameter of 6.69 inches (170 mm) and a height of 11.4 inches (290 mm) and operates at a maximum pressure of 207 MPa (30,000 psi) and a maximum temperature of 2,552°F (1,400°C).

The press was installed in the T.A.G. facility in May 2022.

 

 


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Thermal Processing for Firearms: The Essential Guide

OC

What do gas nitriding, hot isostatic pressing (HIPing), black oxide coating, and high pressure gas quenching have in common? They all are key processes in heat treating firearm components.

Written by Rob Simons, manager of metallurgical engineering at Paulo, this in-depth Original Content article covers Paulo’s perspective on the thermal processing of firearms components and best practices for handling and lot traceability.

Check out more of Heat Treat Today’s Technical Tuesday articles by searching “technical tuesday” in the search bar.


Rob Simons
Manager of Metallurgical Engineering
Paulo

While many industries are continuing to reel from the ongoing coronavirus pandemic, the firearms industry in the United States is booming. Over the past decade, the sector’s strong growth has only accelerated in 2020, fueled by consumers’ response to the pandemic and ongoing civil unrest. According to the NSSF’s 2020 Firearm and Ammunition Industry Economic Impact report, the firearms industry is responsible for well over 300,000 American jobs—a figure that has doubled since 2008.

Consumer demand for firearms also drives the need for heat treatment services for this highly regulated industry. Proper thermal processing is critical for safety and also plays a key role in delivering the quality finish that manufacturers want and consumers expect. In this article, we’ll share our firearms heat treatment expertise, delving into the common processes, specifications, and considerations of servicing this thriving industry.

Key Heat Treatment Processes for Firearms Components

Gas Nitriding

Nitrided 17-4.

Gas nitriding is used to case harden parts that must retain softer, more ductile cores. Because it is carried out at a lower temperature, gas nitriding helps prevent the part distortion that can sometimes occur as a result of conventional heat treatment. In addition to hardness characteristics, parts are often nitride coated for cosmetic purposes and to enhance corrosion resistance. Nitriding results in a beautiful, highly durable black coating that is often used in place of black oxide coatings or other blackening processes. Nitride coating is much harder than the alternatives, so the black finish will stand up to heavy use significantly longer.

Components and Materials Commonly Treated With Nitride Coating

Nitride coating is typically performed on outwardly visible components (and those you’d see while cleaning the gun) such as handgun slides and barrels, as well as muzzle devices such as flash hiders, muzzle breaks, and compensators.

These components are usually manufactured using the following materials, which can be nitrided to achieve the desired black finish and case hardness:

  • 4140 steel. AISI 4140 is a chromium-, molybdenum-, and manganese-containing low alloy steel (usually referred to as chrome-moly steel). It has high fatigue strength, abrasion and impact resistance, toughness, and torsional strength.[1]
  • Grade 416 stainless steel. Grade 416 steel is a free-machining, martensitic stainless steel with a machinability of 85%. [2]
  • Grade 410 stainless steel. Grade 410 stainless steels are general-purpose martensitic stainless steels containing 11.5% chromium. Grade 410 steels have good corrosion resistance properties which can be further enhanced by hardening, tempering, and polishing.[3]
  • Grade 420 stainless steel. Grade 420 stainless steel is higher incarbon than 410 with a minimum chromium content of 12%.
  • 4340 steel. AISI 4340 alloy steel is a low alloy steel containing chromium, nickel, and molybdenum. When heat-treated, it exhibits high toughness and strength. This material is considered extreme duty and is typically used for higher-end firearms.[4]
  • 17-4 stainless steel. 17-4 stainless steel is an age-hardening martensitic alloy combining high strength with the corrosion resistance of stainless steel. It is relatively cost-effective and more weldable than other martensitic alloys.[5]

Nitriding Specifications

The most common measurement that firearms manufacturers specify in desirable nitriding results is intermetallic depth. Typical specifications fall between four and 25 microns of white layer depth. The amount of allowable porosity within the case depth is also commonly specified, and while there are varying ranges, less than 50% porosity is a typical target.

While porosity is often regarded as an undesirable characteristic, there are advantages to some porosity in the finished material. These microscopic voids can hold oils and enhance corrosion resistance. The resulting porosity in nitrided materials allows the coating to last dramatically longer than phosphate- or black-oxide-coated steels.

Some manufacturers utilize blanket aerospace specifications such as AMS 2757 or AMS 2959/12 because they encompass the desired porosity and case hardness depth for nitrided firearms components.

Vickers hardness testing is our preferred method for evaluating intermetallic depth in nitrided components. While 850 HV is typically the top achievable hardness for stainless steel, our team has consistently achieved 2000 HV with our nitriding processes. Higher-end hardness is beneficial for firearms components because it enhances wear resistance in components that slide against each other.

Casting of unknown material showing consolidation of macro pores through HIP.

Hot Isostatic Pressing (HIP)

With hot isostatic pressing, parts are heated to very high temperatures in a sealed chamber capable of generating very high pressures in the presence of inert gas. During processing, heat and pressure combine to close the voids that formed during part manufacturing, eliminating weakness in the parts. Most firearms components respond well to standard coach cycles for HIP, which commonly run at 2050–2200°F and 15,000 psi.

Firearms Components and Materials Commonly Processed With HIP

HIP is especially well suited for removing porosity from metal injection molded (MIM), additively manufactured (AM), and investment cast parts.

MIM is a fast, cost effective way to produce fire control components such as hammers, triggers, and safety selectors, especially for AR-15’s. Traditionally, MIM components have had a reputation in the industry for being inferior to those manufactured with conventional machining because they have been known to fail early in the field.

Common MIM grades used in the manufacturing of firearms include 4140 steel, 17-4 stainless steel, and…

  • FL-4605. FL-4605 is a low alloy steel with prealloyed manganese, molybdenum and nickel content for enhanced hardenability.[6]
  • 420 stainless steel. 420 stainless steel is relatively high in carbon with a minimum chromium content of 12%, which gives it the highest hardenability of stainless steel grades.[7]

Additive manufacturing has not yet been widely adopted in the firearms industry, but we have seen it increasingly used in the manufacture of suppressors. These components—commonly known as silencers—trap the expanding gas as the weapon is fired to reduce noise, and are used for military sniper rifles. AM is an ideal method of manufacture for these components due to their complex geometry that is difficult or even impossible to achieve with traditional machining.

Investment casting is another process we see used in the production of handgun frames, specifically in the M1911 pistol.

MIM, AM, and investment castings all have one thing in common: these manufacturing methods leave voids behind in the internal structure of parts. HIP eliminates unwanted porosity in these parts, increasing their toughness, gross strength, and fatigue life which allows firearms components to withstand being repeatedly subjected to high impact.

MIM 316L before (top) and after (bottom) HIP. Porosity has been consolidated, but there are solid inclusions in the material.

HIP Specifications

For additive manufactured firearms components, we encounter two primary specifications:

  • ASTM F3301, a specification that outlines standards for thermal post-processing for metal parts made with powder bed fusion. ASTM F3301 identifies hot isostatic pressing as an acceptable means to stress relieve additive manufactured components.
  • ASTM F3055, the standard specification for additive manufacturing nickel alloy with powder bed fusion. In this specification, HIP is required for Class B, C and D components and is considered optional for Class G.

In both specifications, components must be processed under inert atmosphere at no less than 100 MPa within the range of 2048 to 2165°F (1120 to 1185°C). Parts must be held at the selected temperature within ∓27°F (15°C) for 240 min ∓60 min, and cooled under inert atmosphere to below 797°F (425°C), or to parameters as agreed upon between the component supplier and purchaser.

Black Oxide Coating

Black oxide gives firearms a sharp black appearance, enhances corrosion resistance, and minimizes light reflection. Unlike paint, black oxide doesn’t add any additional thickness to gun components. The desired result in the black oxide process is creating magnetite (Fe3O4), an alloy of iron and oxygen, on the surface of the metal. The black oxide process enhances corrosion resistance by adding rust preventive oils to the metal part.

While it doesn’t last as long as gas nitride coating, black oxide is still a popular, cost-effective option to give visible gun parts the perfect black look. Finding a partner that can provide heat treatment and black oxide under one roof can reduce your transportation costs, speed up turnaround time, and simplify your overall process since one supplier owns the final results.

Firearms Components and Materials That Use Black Oxide Coating

Like nitriding, black oxide coating is used on outwardly visible components like slides, barrels, and muzzle devices including flash hiders, muzzle breaks, and compensators. It can be applied to any carbon steel component, but it will not adhere to stainless steel.

Specifications for Black Oxide Coating

Unlike nitriding and HIP, we rarely encounter standard specifications when it comes to black oxide results. However, as a best practice we work with customers to establish boundary samples for each part number treated with black oxide so we can compare our results to what both sides agreed upon as a desirable appearance.

High Pressure Gas Quenching

High pressure gas quenching can be performed in a vacuum furnace as an alternative to oil quenching for any firearms components that are near net shape or completely finished—or where distortion is a chief concern. In high pressure gas quenching, parts are austenitized under vacuum. Then, the chamber is backfilled with inert gas, which is heavily agitated by powerful motors.

High pressure gas quenching results in cleaner parts than oil quenching, but it has other benefits that can prove highly valuable for firearms components. This process can take a conventional 4140 alloy and make it achieve the same properties as a vacuum arc remelted (VAR) 4340, a much higher quality nickel-based material. This can allow firearms manufacturers to see similar hardness and strength results in everyday components as those they would expect from an extreme duty material like 4340.

Handling and Traceability for Firearms Components

No heat treater should make a habit of losing any type of parts, but the implications for serialized firearms components are more severe than any other mass-produced components. Serialized components are what the U.S. government considers the firearm—it refers to the part that features the serial number, usually the lower frame assembly and sometimes the barrel or slide.

Firearms components to be treated with gas nitriding that have AMS 2757 or AMS 2759/12 identified as the standard are also subject to the recordkeeping guidelines outlined in the specification. AMS 2757 requires that documentation includes the equipment and approved personnel’s identification, date of processing, number of parts, alloy, lot identification, and actual thermal processing times and temperatures at a minimum.

Proper handling of firearms components by heat treaters is essential to keep the supply chain running smoothly. Improperly heat treated parts will either wind up in the scrap bin or require reprocessing, and lost parts can result in an ATF audit or investigation. At our company, we’ve engineered our process to prevent issues from occurring in the first place. Here are a few examples of how we do it:

  • Electronic tracking. Each lot of parts is assigned a barcode that links to electronic records of all relevant information about the job—process parameters, specifications, shop orders, etc. The process parameters on the parts’ barcode are integrated with equipment, so when parts are scanned for processing, the furnace will be automatically set to the proper parameters according to the parts’ recipe. This helps us prevent parts from being improperly heated or subject to the wrong process altogether.
  • Secure storage. In Paulo plants that process firearms, we use locked cages and secure vaults to protect serialized components. All access to these areas is monitored and recorded to maintain accountability and, if applicable, adhere to AMS specifications.
  • Specialized handling. To give our firearms customers more peace of mind and to safeguard against errors in our process, we’ve also engineered secure fixturing for many components that allows them to remain locked throughout the entire heat treatment and finishing process.

In addition to a Federal Firearms License (FFL), heat treaters should also have a documented quality management system in place. Choosing an ISO 9001-certified supplier can help give manufacturers confidence in a heat treating partner’s ability to maintain quality operations. Maintaining other certifications such as IATF 16946 and CQI-9 is also a good sign that your partner is well equipped to handle firearms work.

Conclusion

The firearms industry relies on its thermal processing partners to sustain its growth. Proper heat treatment and metal finishing results in better performing, longer lasting firearms for our military and law enforcement, which helps keep our country safe. In uncertain times, the firearms industry represents a bright spot in the U.S. economy that we are proud to support.

About the Author: Rob Simons is manager of metallurgical engineering at Paulo where he leads the commercial heat treating industry’s largest in-house metallurgy team. Rob continuously spearheads research and innovation at Paulo that lead to advanced capabilities and better results for the company’s customers. Rob holds a bachelor’s degree in Metallurgical Engineering from the Missouri University of Science & Technology.

About Paulo: Founded in 1943, Paulo is one of the largest providers of thermal processing and metal finishing solutions in North America. Headquartered in St. Louis, Paulo operates six divisions servicing the United States and northern Mexico.

[1] https://www.azom.com/article.aspx?ArticleID=6769

[2] https://www.azom.com/article.aspx?ArticleID=971

[3] https://www.azom.com/article.aspx?ArticleID=970

[4] https://www.azom.com/article.aspx?ArticleID=6772

[5] https://www.azom.com/article.aspx?ArticleID=4220

[6] https://www.ssisintered.com/materials/low-alloy-molybdenum-nickel-steels

[7] https://www.azom.com/article.aspx?ArticleID=972

(photo source: william isted at unsplash.com)

All other images are provided by Paulo.

Article updated on Thursday 4/29/2021 at 3:22pm.

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Process Innovation to Reduce Distortion During Gas Quenching

“High-pressure gas quenching (HPGQ) attempts to reduce temperature nonuniformities by reducing the cooling rate; however, this is generally not sufficient to eliminate shape change. Shape change can be predicted by heat treatment simulation software, but it is difficult to reproduce the exact same cooling conditions in the vessel for each batch. Therefore, the distortion of the components will not be consistent from batch to batch.”

Read the case study to see one response to this issue in this original content from Heat Treat Today by Justin Sims, lead engineer at DANTE Solutions.

This article first appeared in the latest edition (March 2020) of Heat Treat Today’s Aerospace Heat Treating magazine.


Distortion is generally described by a size change and a shape change. In heat treatment of steels, size change is unavoidable and is mainly due to the volumetric difference between the starting microstructural phase and the final microstructural phase. Shape change of steel parts from heat treatment is due to nonuniform thermal and nonuniform microstructural strains as a result of nonuniform cooling or heating, alloy segregation, poor support of the component while at high temperature, thermal expansion or contraction restrictions, or residual stresses from prior forming operations. Nonuniform cooling or heating can be as fundamental as the temperature gradient from the part surface to its core, or as complex as the flow of fluid around a component feature. Both can result in nonuniform strains, resulting in a shape change. If the stresses causing these strains exceed the yield strength of the material, then permanent shape change will occur. Size change can be anticipated and is predictable, while shape change, or distortion, is usually unanticipated and more difficult to predict.[1-2] 

Justin Sims,
Lead Engineer,
DANTE Solutions

Most thermal processes try to control these nonuniformities using methods of low complexity such as part orientation and rack design. Quenching systems, for example, are generally designed to remove as much thermal energy from the work pieces as possible and to do this as quickly as possible. High-pressure gas quenching (HPGQ) attempts to reduce temperature nonuniformities by reducing the cooling rate; however, this is generally not sufficient to eliminate shape change. Shape change can be predicted by heat treatment simulation software, but it is difficult to reproduce the exact same cooling conditions in the vessel for each batch. Therefore, the distortion of the components will not be consistent from batch to batch.

In response to this issue, a prototype gas quenching unit capable of controlling the temperature of the quench gas entering the quench chamber was devised. With the DANTE Controlled Gas Quench (DCGQ) unit, it is possible to have control of the thermal and transformation gradients in the component by controlling the temperature of the incoming quench gas, thereby significantly reducing, or eliminating entirely, the shape change caused by quenching. In doing so, the size change can easily be predicted by heat treatment simulation software, and post-hardening finishing operations can be reduced or eliminated. This process is ideal for thin parts or components with significant cross-sectional changes. Atmosphere Engineering (now part of United Process Controls) in Milwaukee, Wisconsin constructed the unit and provided the logic to control it. All experiments with the unit were conducted at Akron Steel Treating Company in Akron, Ohio. The project was funded by the U.S. Army Defense Directorate (ADD).

Figure 1 (left) shows the front of the unit, while Figure 1 (middle) shows the back of the unit. The back of the unit contains the human machine interface (HMI), shown in Figure 1 (right), where process parameters can be modified and DCGQ recipes entered. The prototype unit has a working zone of nine cubic ft. and is capable of quenching loads up to 100 lbs. at one atmosphere of pressure.

Figure 2. Comparison of quench gas temperature entering the
quench chamber versus the recipe setpoint temperature for
two different DCGQ process recipes

The ability of the unit to maintain continuity between the recipe setpoint temperature and the actual temperature entering the quench chamber is absolutely paramount. Figure 2 shows two schedules, one aggressive and one conservative, comparing the recipe setpoint (Chamber Inlet SP) to the actual quench gas temperature (Chamber Inlet PV). Figure 2 also shows that the prototype unit has good control of the quench gas temperature between 752°F (400°C) and room temperature, the martensite transformation range for most high hardenable steel alloys. There is some deviation between the two temperatures below 392°F (200°C) for the aggressive schedule as the setpoint reaches its set temperature, due to the relatively small temperature difference between the quench gas and the shop air. This small temperature difference makes it slightly difficult for the air-to-air heat exchanger used in the design to keep up with the rapid drop in temperature, but overall there is very good control of the quench gas temperature.

Figure 3. Micrograph of DCGQ (left) and HPGQ (right) processed coupons, mag. 1000X
There is a copper layer on the surface of the DCGQ processed coupon.

Microstructural examination was conducted on Ferrium C64 coupons processed using the DCGQ process and coupons processedusing a 2-bar HPGQ. C64 was chosen for this study due to its extremely high hardenability and its high tempering temperature. Figure 3 compares the microstructures of the two processes at a magnification of 1000X, and no significant difference is detected. The DCGQ coupons required two hours to complete the transformation, whereas the HPGQ coupons transformed in a few minutes. There is no indication that the slow rate of transformation damaged the microstructure or mechanical properties in any way. Tensile and Charpy properties were equivalent between the two processes.

Distortion coupons, thick disks with eccentric bores, were designed and manufactured with the goal of evaluating the distortion response when subjected to a DCGQ process, and then compared to coupons subjected to a standard 2-bar HPGQ operation. All coupons were manufactured from the same Ferrium C64 bar stock. All coupons were cryogenically treated and tempered at 595°C for eight hours after quenching.

Figure 4. Nomenclature and locations used for out-of-round measurements on the distortion coupon

Figure 4 shows a distortion coupon with the nomenclature and locations used for measuring the out-of-round distortion of the eccentric bore. Due to the uneven mass distribution, the north-south direction will generally be larger than the east-west direction. Five measurements were then made along the axis of the coupon using a Fowler Bore Gauge.

Table 1. Out-of-round distortion measurements of the distortion coupon for a DCGQ and HPGQ process

Table 1 shows the results from four coupons; two hardened using the DCGQ process and two processed using the standard 2 bar HPGQ for C64. The individual measurements (EW1, NS5, etc.) are relative and are dependent on the reference value used for the bore gauge. The individual measurements give an indication of the variation in distortion in the axial direction. The out-of-round measurements are actual values, as they are the difference between the actual measurements. The DCGQ process gave significantly less distortion than the HPGQ process.

While the values reported show a 50% reduction in out-of-round distortion for the DCGQ process, a larger gain could have been realized if two other conditions were addressed. First, the coupon for DCGQ was placed directly into a 1832°F (1000°C) preheated furnace since the prototype unit does not have austenitizing capabilities. Controlled heating, just like controlled cooling, should be utilized to realize the full potential of this process. Second, the DCGQ schedule was designed for another coupon geometry that was processed together with these distortion coupons. Therefore, the schedule was not optimum for this coupon geometry.

Table 2. DANTE simulation results comparing HPGQ and DCGQ using the experimental conditions and a DCGQ with optimized heating and cooling schedulesMARCH 2020

Table 2 compares the DCGQ simulation results in which the two processes executed on the experimental coupons were compared to an optimized process, including controlled heating and cooling schedules designed for this coupon. The optimized schedule predicts an order of magnitude reduction in out-of-round distortion. Comparison of the measurements from the HPGQ and DCGQ experiments in Table 1 to the model predictions in Table 2 shows that the model predictions agree closely with the experimental results.

Simulating the application of the DCGQ process to a gear geometry, the predicted warpage of a bevel gear was examined. The simulation looked at the differences between an oil quench, 10 bar HPGQ, and a 10 bar DCGQ process. From Figure 5, it is clear that the HPGQ process is predicted to produce the most distortion. Even though the 10 bar gas quench has a slower cooling rate than the oil quench, less distortion is not guaranteed since a slower rate does not guarantee a more uniform phase transformation.[3] In this case, both heating and cooling were controlled for the DCGQ simulation.

Figure 5. Comparison of oil quench, HPGQ, and DCGQ processes for a bevel gear

In summary, a prototype gas quenching unit has been constructed with the ability to accurately control the temperature of the quench gas entering the quench chamber. Experimental results have shown that mechanical properties and microstructure are equivalent between the DCGQ process and a 2-bar HPGQ process for Ferrium C64. Thick disks with eccentric bores were machined and then heat treated using DCGQ and HPGQ. It was shown that the DCGQ process reduced distortion in these disks by 50%. Simulation using DANTE then showed that the distortion could be reduced further if controlled heating and cooling are used. Finally, a comparison was made between an oil quench, HPGQ, and DCGQ processes for a bevel gear. This comparison showed that the HPGQ process was predicted to cause the most distortion. HTT

References

[1] Prabhudev, K.H., Handbook of Heat Treatment of Steels, Tata McGraw-Hill Publishing, 1988, p.111-114

[2] Sinha, Anil Kumar, ASM Handbook, Vol. 4: Heat Treating, ASM International, 1991, p.601-619

[3] Sims, Justin, Li Zhichao (Charlie), Ferguson B. Lynn, Causes of Distortion during High Pressure Gas Quenching Process of Steel Parts, Proceedings of the 30th ASM Heat Treating Society Conference, ASM International, 2019, p.228-236

 

About the Author: As an analyst of steel heat treat processes and an expert modeler of quench hardening processes, Justin Sims was the lead engineer for designing and building the DANTE Controlled Gas Quenching (DCGQ) prototype unit. This system was developed to minimize distortion of quenched parts made of high hardenability steels, while still achieving the required properties and performance.

For more information, contact Justin at DANTE Solutions

 

Process Innovation to Reduce Distortion During Gas Quenching Read More »

Testing Underway for Innovative Gas Quenching Unit

 

A Cleveland-based heat treatment software and engineering firm, specializing in metallurgical process engineering and thermal/stress analysis of metal parts, recently announced that mechanical and fatigue testing is underway on an innovative gas quenching unit designed to minimize component distortion during the hardening process.

The DANTE Controlled Gas Quenching (DCGQ) unit is capable of quenching single components following a time-temperature schedule designed for a specific component and steel alloy using the DANTE software.

DANTE Solutions proposed the concept of the process and the DANTE Controlled Gas Quench (DCGQ) unit and collaborated with Milwaukee-based Atmosphere Engineering (now part of United Process Controls), which built the unit, and Akron Steel Treating. The project is funded by the US Army Defense Directorate (ADD), and the aim market is aerospace, where high hardenability steels are used for gears, bearings, and shafts.

Justin Sims, mechanical engineer, DANTE Solutions

According to Justin Sims, a mechanical engineer with DANTE Solutions, the project began with Phase 1, wherein the team had to “make sure that a relatively slow cooling rate through the martensite transformation did not degrade material properties.”

“Phase 1 showed that we had comparable results for hardness, tensile properties, Charpy impact properties, and bending fatigue to the standard quenching practice for Ferrium C64,” said Sims. “We then initiated Phase 2 and had a unit built that was capable of controlling the temperature of the incoming quench gas to within +/- 5°C.” Phase 2 will end December 2018 after two years. The Phase 1 process currently has a patent pending.

Mechanical & Fatigue testing is currently underway at Akron Steel Treating Company where the unit is installed, and samples have been processed to compare the DCGQ process to standard HPGQ of high alloy steels. The current steel under investigation is Ferrium C64. Sims noted that DANTE is overseeing the processing of the test materials, and commercial metallurgical testing companies are performing the tests.

Tensile Testing Metallurgical Laboratory completed the hardness, tensile and Charpy impact testing, and the results are similar for conventionally hardened C64 samples and DCGQ processed samples. IMR Test Labs is conducting the bending fatigue tests. The US Army at Fort Eustis will conduct the rolling contact fatigue tests.

“We have hardness, tensile, and Charpy impact results from the unit we can share with anyone who is interested,” said Sims. “Distortion, bending fatigue, and rolling contact fatigue are currently being evaluated and the results will be available before the end of 2018.”

“We believe that the DANTE Controlled Gas Quench (DCGQ) process, patent pending, has the potential to change the way heat treating is performed on high hardenability steels,” added Sims. “By controlling the temperature of the incoming quench gas, components experience a near uniform transformation to martensite. This near-uniform transformation has the potential to eliminate post-heat treatment correction operations by minimizing part distortion and allowing designers to account for the size change distortion in the initial design of a component. To date, mechanical and dynamic properties for Ferrium C64 processed using the standard hardening process and the DCGQ process has been identical. Bend fatigue and rolling contact fatigue are currently being evaluated.”

 

All images provided by DANTE Solutions.

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Enhancing Energy Efficiency of Thermochemical Vacuum-Processes and Systems

BOTW-50w  Source:  Heat Processing

“The energy optimization of thermoprocessing equipment is of great ecological and economical importance. Thermoprocessing equipment consumes up to 40 % of the energy used in industrial applications in Germany. Therefore it is necessary to increase the energy efficiency of thermoprocessing equipment in order to meet the EU’s targets to reduce greenhouse gas emissions. In order to exploit the potential for energy savings, it is essential to analyze and optimize processes and plants as well as operating methods of electrically heated vacuum plants used in large scale production. For processes, the accelerated heating of charges through convection and higher process temperatures in diffusion-controlled thermochemical processes are a possibility. Modular vacuum systems prove to be very energy-efficient because they adapt to the changing production requirements step-by-step. An optimized insulation structure considerably reduces thermal losses. Energy management systems installed in the plant-control optimally manage the energy used for start-up and shutdown of the plants while preventing energy peak loads. The use of new CFC-fixtures also contributes to reduce the energy demand.”

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Improved Materials and Enhanced Fatigue Resistance for Gear Components

BOTW-50w Source:  Thermal Processing for Gear Solutions

“When trying to improve fatigue properties, two important areas need to be addressed: improvements of material and improvements in heat treatment technology.”

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