Low-Pressure Carburising Systems: A Review of Current

Technology
S. Bruce & V. Cheetham
Edwards, UK UK
BOC Edwards,
P.F. Stratton
BOC, Huddersfield, UK

ABSTRACT: Although the great majority of carburising is still carried out at

atmospheric pressure, recent developments in vacuum furnaces and steel technology
have meant that carburising can now be carried out in a more environmentally friendly
way under low pressure. The range of material types being carburised under vacuum is
increasing with a strongly upward trend towards vacuum carburising evident in many
areas. In choosing a suitable carburising process, three main choices have to be made:
- which carburising technique and gas (or gases) to employ; which type of vacuum
pump system to install; and which quenching gas to use. In particular, the selection of
carburising gas has a significant impact on the efficiency and cleanliness of the
process, and on deciding the most appropriate vacuum pump system. This paper
describes the current state of the art and practical experiences with low-pressure
carburising techniques and examines the various options within these three essential
choices. It also considers the safety and environmental implications of these choices.

1. INTRODUCTION
Of the many technologies available today to improve the performance of engineered
surfaces, carburising is one of the most common. Carburising is enduringly popular
because it uses a higher temperature than most thermochemical processes so that a
deep hard layer can be formed in a short time. The great majority of carburising takes
place at atmospheric pressure in an atmosphere containing large quantities of carbon
monoxide. The parts are subsequently quenched in oil. Recent developments in
vacuum furnaces and steel technology have meant that carburising can now be carried
out in a more environmentally friendly way under low-pressure.

Low-pressure carburising processes are carried out in

vacuum furnaces like the one in Figure 1.
Hydrocarbons are used directly as the source of
carbon. Emissions are low in volume and relatively
benign. The oil has been replaced by gas quenching.
The parts emerge very clean, bright and dry, and less
distorted than oil-quenched components. Improving
technologies for making steel have produced
carburising steels that can be quenched in 10 bar
nitrogen (N2). Even the current lower hardenability
carburising steels can be quenched using improved
helium (He) quenching technology. Vacuum
carburising has also been applied to parts
Figure 1. Double chamber vacuum made by powder metallurgy (P/M)
carburising furnace (photo courtesy of techniques. Analysts predict an upward trend
Seco/Warwick) in vacuum carburising from 1% of the market
in 2000 to 13% in 2010.
However, many issues still need to be considered at the design stage of any low-
pressure carburising system. The first is the carburising technology to be used – which

Edwards Ltd, Crawley Business Quarter, Manor Royal, Crawley, West Sussex, RH10 9LW, UK. T: +44 (0) 1293 52 88 44
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 hydrocarbon to choose, is plasma needed to activate it, and how will the hydrocarbon
be supplied? The second is the choice of vacuum pumps – which pumps will eliminate
any potential problems, optimise reliability and performance, ensure safety in operation
and minimise the costs of ownership. The third question is what quenching gas to use
– nitrogen, argon (Ar) or helium, at what pressure, and is recycling possible?

2. CARBURISING TECHNOLOGY
In low-pressure carburising (LPC), the vacuum furnace is evacuated after charging.
When the pressure has dropped below 10Pa, the furnace chamber is effectively free of
oxygen and the heating cycle can start. The charge is heated to between 790 and
1040°C in up to three stages, depending on the carburising temperature and the
sensitivity of the components. Once the whole charge has reached the carburising
temperature, the first carburising phase is initiated by admitting the hydrocarbon into
the furnace at pressures between 10 and 1000Pa. Carbon transfer is so effective that
the austenite is saturated with carbon after only a few minutes. The first carburising
phase must therefore be stopped after a relatively short time by interrupting the gas
supply and evacuating the furnace.

This sets
off the first
diffusion
phase.
Carbon
transferred
during the
carburising
phase
diffuses
into the
steel and the carbon content at the surface
Figure 2. A typical LPC cycle (screen shot Figure 3. Vacuum carburising simulation
courtesy of Seco/Warwick) (courtesy of Seco/Warwick)
decreases accordingly. Depending on
the case depth specified, further carburising and diffusion phases follow the first,
building up the case with each cycle. The length of the carburising phases decreases
with increasing case depth. A typical cycle is shown in Figure 2, which clearly shows
the pulses of carburising gas. The sharp rise in surface carbon produced by each
pulse is illustrated in Figure 3. Once the specified case depth has been obtained, the
temperature is reduced to the hardening temperature and the charge is gas quenched,
either in the same chamber or a separate one. Depending upon the hardenability of
the steel, the quenchant can be high pressure nitrogen or helium. Finally the
components are tempered in the usual way at a temperature determined by the
properties required and the steel used.

A range of hydrocarbon gases and gas mixtures has been used and promoted for LPC.
Originally propane (C3H8) was the principle hydrocarbon gas because it was used in
atmospheric carburising. Used in excess, propane can produce good metallurgical
results as it readily dissociates above 600oC, breaking down into free carbon atoms,
hydrogen (H2) and methane (CH4). However this generally occurs before the gas
comes in contact with the steel surface, and consequently there is time for the carbon
atoms to recombine with other propane fragments in a radical polymerisation process
to form tars and soot. This reaction is in direct competition with the desired
carburisation reactions. Uncontrolled soot formation results in poor carbon transfer to
the part and loss of productivity through the need for additional maintenance of the

Edwards Ltd, Crawley Business Quarter, Manor Royal, Crawley, West Sussex, RH10 9LW, UK. T: +44 (0) 1293 52 88 44
© Edwards Limited 2009. All rights reserved. Registered in England and Wales No. 6124750
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 heat treatment system. The production of tars and soot within the chamber and pipe
work is also a major problem for the vacuum pumping system, as will be discussed
later.

Other saturated hydrocarbon gases have been used for LPC, although they can also
be prone to heavy tar formation. Methane is nearly non-reactive at these low
pressures, and requires a temperature of at least 1040°C or activation with a plasma
(called Plasma-Aided LPC), although it appears to have lost some popularity recently.
Isobutane (i-C4H10) also leads to heavy tarring. Better results are reported using
unsaturated hydrocarbon gases, such as ethylene (ethene, C2H4) (although this still
gives some tar), and especially acetylene (ethyne, C2H2) – currently the most popular
LPC gas. The reason is understood to be the higher decomposition rates of such
molecules under LPC conditions, and their significantly lower tendency towards the
polymerisation reactions that lead to tar formation. Other hydrocarbons and mixtures of
gases are being widely investigated, to find the optimum feed gas compositions to
produce the best metallurgical results with the least generation of soot and tar.
Cyclohexane (C6H12) vapour is reported to produce excellent results, and specific
mixtures of ethylene, acetylene and hydrogen are also promoted as giving highly
effective carburising together with very high cleanliness.

The keys to good results are therefore maximising the efficiency of hydrocarbon
decomposition to make the most of the available carbon atoms, while minimising the
formation of vinylic free radicals that promote rapid polymerisation to soot and tar. The
particular popularity of acetylene as the key LPC gas illustrates these features.
Acetylene tends to dissociate only at the metal surfaces of the load, it penetrates well
into blind holes and around complex geometries and it dissociates into two active
carbon atoms without vinylic fragments (compared to the one carbon atom plus
fragments produced by dissociation of either propane or ethylene). It does not form any
non-reactive methane and produces comparatively little soot. This is illustrated in
Figure 4, which shows similar installations running acetylene and propane after one
year of operation.

Figure 4. Comparative cleanliness of LPC hydrocarbon gases (Photographs courtesy of Ipsen

International)

The LPC process is controlled more by experiment than by theory, and the case depths
achieved depend on temperature, furnace pressure, hydrocarbon flow rate and time.
However, computer control using these empirical functions is possible, as shown in
Figure 3.

On a practical note, acetylene is shipped in a cylinder packed with a porous solid and a
liquid solvent, commonly acetone. Acetylene dissolves in the acetone solution and
disperses throughout the porous medium. When the valve of a charged acetylene

Edwards Ltd, Crawley Business Quarter, Manor Royal, Crawley, West Sussex, RH10 9LW, UK. T: +44 (0) 1293 52 88 44
© Edwards Limited 2009. All rights reserved. Registered in England and Wales No. 6124750
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cylinder is opened, the acetylene comes out of solution and passes out in gaseous
form. There is a maximum draw-off rate that cannot be exceeded without entraining
acetone into the acetylene. Although the overall acetylene requirement is low in LPC,
instantaneous flow rates can be high, so several cylinders must be manifolded together
to provide the required flow.

3. VACUUM PUMPING SYSTEM

The LPC process clearly introduces issues for the vacuum pump system:
x if substantial amounts of soot and tar are formed, the gas flow will carry them
over into the vacuum pumps
x the resulting vacuum pump contamination, by tars in particular, can lead to
operating problems such as oil degradation, poor lubrication, increased pump
wear, internal blockages and difficulty in re-starting pumps
x the hydrogen and residual hydrocarbon in the pumped gases can make them
flammable.

There are two types of vacuum pumping system that overcome these issues and are
used successfully in LPC applications. The choice of system depends essentially on
whether the process uses propane, or other hydrocarbons generating significant
amounts of soot and tars, or whether it uses acetylene (ethyne) or other cleaner
mixtures. In all cases the processing pressure needed requires a mechanical vacuum
booster (a “Roots” booster) to be installed in series with the primary vacuum pump. The
important choice to be made is the type of primary (backing) pump, which must be
either an oil-sealed (“wet”) rotary piston pump or a dry mechanism claw pump.

A typical system with an oil-sealed rotary piston pump is shown in Figure 5. This uses a
standard reliable rotary piston pump of 500m3/h capacity behind a mechanical booster
of 2600m3/h displacement. The booster is run by a variable frequency drive, giving
good operational flexibility as it can assist in initial pump down right from atmospheric
pressure. The booster is fitted with a fine oil spray injection system, using the seal /
lubricating oil from the primary pump itself. This maintains a thin film of oil over the
whole internal surfaces of the booster pump and the following pipe work during
operation, flowing right into the primary pump. This is highly effective in preventing
internal adhesion of soot and tars from propane-based and other “dirty” LPC systems,
because all such contaminants reaching the vacuum pumps are trapped in the oil film
and washed into the oil of the primary pump. To prolong the useful life of this oil, the
primary pump is fitted with a pumped external oil filtration system, which supplies
filtered, clean oil constantly to both primary pump and booster oil spray. Clearly, such
systems demand regular oil changes.

In the ”wet” pump system, safety does not permit any compressed air supply or air-
breathing gas ballast system to be connected to the primary pump, because of the
hydrogen and hydrocarbon gas content of the pumped gases. A nitrogen gas ballast
supply must be fitted instead, with the nitrogen flow calculated and controlled to dilute
the flammable gas in the primary pump at all times to a safe margin below the lower
explosive limit (LEL), even when the process is generating the highest levels of
flammable gases. This will then ensure that exhaust gas reaching the air from the final
exhaust pipe remains outside the flammable region under all circumstances.

The
alternati
ve
system
shown in
Figure 6

Figure 5. A LPC vacuum pump set using

an oil-sealed “wet” primary pump, and a Figure 6. A LPC vacuum pump set using a
Roots mechanical booster, with a dry claw primary pump, and a Roots
pumped oil purification and injection mechanical booster, with an oil injection and
system circulation system
 has an industrial dry claw vacuum pump of nominal 600m3/h capacity behind a
mechanical booster of 2600m3/h displacement. The booster may be run by a variable
frequency drive or a low-maintenance hydrokinetic drive, both of which give good
operational flexibility and can assist in initial pump down right from atmospheric
pressure. Once again the booster is fitted with a fine oil spray injection system, but the
flushing oil is aspirated under vacuum into the booster inlet from a separate external oil
reservoir. This system also maintains a thin film of oil over the whole internal surfaces
of the booster pump, the following pipe work and the dry claw pump during operation.
When the oil is then evacuated from the exhaust of the dry claw pump, it is trapped by
a large external filter / coalescer and drained back down into the external oil reservoir.
This is very effective in preventing internal adhesion of smaller quantities of soot and
tars from acetylene-based and other “cleaner” LPC systems, as the circulating oil traps
any contaminants reaching the vacuum pumps. This system also allows the use of low-
maintenance dry claw pump technology, without any requirement for an additional oil
circulation pump, and hence a potentially lower overall cost of ownership.

In the dry claw pump based system, the usual dry pump shaft seal purge must be
supplied with inert nitrogen, and safety does not permit any compressed air supply or
air-breathing system to be connected to this purge, or to the gas ballast inlet, because
of the hydrogen and hydrocarbons in the pumped gases. The amount of seal purge
and gas ballast purge nitrogen supplied to the dry pump must be calculated and
controlled to ensure that the flammable gas is always diluted to a safe margin below
the lower explosive limit (LEL), even when the process is generating the highest levels
of flammable gases. This will also ensure that exhaust gas reaching the air from the
final exhaust pipe remains outside the flammable region in all circumstances.

GAS QUENCHING
Gas quenching in vacuum furnaces is an increasingly attractive option because of its
low environmental impact and minimal distortion of the parts being treated. Whilst
nitrogen is by far the most common quenching gas, helium is a viable option when
higher cooling rates are required, particularly for carburised components. Very recently
steel makers have come to recognise the potential for carburising steels that will
quench to full hardness using the “standard” 10 bar nitrogen quench. One such steel is
15NiMoCr10 that is compared to some typical low alloy carburising steels in Table 1.

Table 1. The diameter of cylinders that can be quenched in various gaseous media to achieve
a 300 Hv core hardness

Steel Cooling Bar Heat Quenchant

ISO SAE rate Diameter Transfer Gas Pressure
(ºC/s) (mm) Coefficient (bar)
(W/m2ºK)
16MnCr5 5115 15 20 800 N2 10
30 1150 N2 20
40 1500 He 20
20MoCr4 4118 RH 23 20 1250 N2 20
30 1800 He 30
15NiMoCr10 40 800 N2 10

Recycling of nitrogen is not economically attractive, but if helium is used, recycling can
reduce the cost. However, careful consideration needs to be given to factors such as
the purity needed in the output gas, its pressure and the time available to do the
recycle. The amount saved by the use of a properly optimised helium-based quenching
system depends on the gas quality required from the recycling system because of the

Edwards Ltd, Crawley Business Quarter, Manor Royal, Crawley, West Sussex, RH10 9LW, UK. T: +44 (0) 1293 52 88 44
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Edwards and the Edwards logo are trade marks of Edwards Limited.
 high capital cost of the equipment and the high losses. It has been shown that a
simple helium recycling system with minimal clean-up, and hence minimal losses, on a
typical vacuum carburising installation with one furnace can reduce helium costs by at
least half.

4. SAFETY AND ENVIRONMENTAL GUIDELINES

The process operator always has the responsibility to conduct a proper risk
assessment of any potentially hazardous process, and to operate the process safely.
The following comments are made for general guidance only.

There are two safety concerns, the furnace atmosphere itself and the vented gases.
Because the LPC process uses hydrocarbon gases and typically generates quantities
of hydrogen as a by-product, it is clearly essential to rigorously exclude air or any other
source of oxygen from the furnace to prevent any potentially flammable mixtures. This
will typically require routine leak checking and / or pressure-rise testing of the chamber
and system. The pump system must have controls to ensure that pumped gas
concentrations remain at a safe margin below the LEL (lower explosive limit) for
hydrogen (4 vol.%) wherever the gas pressure is above 60 mbar, based on the
maximum possible hydrogen process flow and the nitrogen gas ballast (and nitrogen
shaft seal purge flow if fitted) required to dilute it. These dilution measures should be
interlocked to stop the process if they fail, for example by using a flow sensor to alarm
and switch off the process gases if the nitrogen purge flow drops below an acceptable
level. A recommended safe margin for below-LEL operation is <= 25%LEL.

In processes with a very high hydrogen concentration, it is permissible to operate

above the UEL (upper explosive limit) but only after taking professional safety advice.
Essentially, the pump system must incorporate measures to ensure that pumped gas
concentrations remain at a safe margin above the UEL concentration for hydrogen
(75.6 vol.%) wherever the gas pressure is above 60 mbar, based on the minimum
hydrogen process flow and allowing for any gas ballast or shaft seal nitrogen flow
required. This will involve measures and safeguards to ensure: that air cannot leak into
the system or into the vacuum pumps during operation; that there is a proper
maintenance regime including routine replacement of shaft seals on oil-sealed pumps;
and that mechanical vacuum boosters with hermetic shaft seals are used. This
approach will also require inert purging of the exhaust line so that air cannot mix with
the above-UEL gases before the final vent. A recommended safe margin for above-
UEL operation is <= 60% of the residual oxygen concentration which would be present
at UEL.

At the end of the cycle, the furnace itself will be full of inert gas, usually nitrogen. It is
recommended that the furnace is flushed through with air so that the oxygen level
exceeds the critical 19% before the door is opened to avoid any risk of asphyxiation.
From an environmental perspective the key issues to be considered and dealt with are:
x consumption and disposal of oil (mostly from oil-sealed pump systems)
x protection from flammable risks in the system and exhaust lines
x ensuring safe chamber access by avoiding asphyxiation risks.

5. CONCLUSIONS
A great deal of experience has now been gained operating LPC systems around the
world with various process parameters, different modes of operation and types of
vacuum pumping equipment. The problems that arise are familiar and can be resolved
by selecting the right approach for the given process type. For relatively clean LPC
systems, dry-based primary vacuum pumps are well proven and offer the lowest overall
cost of ownership. However, for typical LPC furnaces using propane and generating a

Edwards Ltd, Crawley Business Quarter, Manor Royal, Crawley, West Sussex, RH10 9LW, UK. T: +44 (0) 1293 52 88 44
© Edwards Limited 2009. All rights reserved. Registered in England and Wales No. 6124750
Edwards and the Edwards logo are trade marks of Edwards Limited.
 lot of soot and tar, operating reliability can be assured by using “wet” type oil-sealed
vacuum pumps with recirculating oil flushing systems. Many LPC carburised
components can be designed so that they can be quenched with high pressure
nitrogen. Where this is not possible, high pressure helium must be used with a recycle
system.

6. BIBLIOGRAPHY
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Luiten C.F., Limque F. & Bless F. (1979), Heat Treatment ’79, Birmingham, UK
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Prunel G. & Stauder B. (2004), Proceedings of the 14th IFHTSE Congress, Vol.1, pp.364-369.
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Shivanath R. et al. (2001), Industrial Heating, May, pp.37-39.
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Edwards Ltd, Crawley Business Quarter, Manor Royal, Crawley, West Sussex, RH10 9LW, UK. T: +44 (0) 1293 52 88 44
© Edwards Limited 2009. All rights reserved. Registered in England and Wales No. 6124750
Edwards and the Edwards logo are trade marks of Edwards Limited.