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7/28/2019 Low Press Carbg and High Press Qnchg
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Furnace Atmospheres
No. 6Low pressure carburising and highpressure gas quenching.
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2 Low pressure carburising and high pressure gas quenching.
Page
Low pressure carburising and high pressure gas quenching (Intro) 4
1. Low pressure carburising 6
1.1. History 6
1.1. Dierentiation rom other carburising processes 6
1.2 Carbon transer coecient 8
1.3 State o the art today 8
1.4. Low pressure carburising principles 8
1.4.1 What is low pressure carburising? 8
1.4.2. Benets and drawbacks 10
1.4.3. Pressure range 10
1.4.4. Model o carbon transer 10
1.4.5. Reactions 11
1.5. Low pressure carbonitriding 11
1.5.1. Principles 11
1.5.2. Benets and drawbacks 12
1.6. Gases used or the LPC processes 12
1.6.1. Choice o gas or carburising 12
1.6.2. Purity o gases 13
1.7. Process parameters 13
1.7.1. Process design 13
1.7.2. Carbon mass fow 14
1.7.3. Gas fow rate 14
1.7.4. Gas type 14
1.7.5. Temperature 15
1.7.6. Pressure 161.7.6. Steel grade 16
1.8. Control o process parameters 16
1.8.1. Simulation o low pressure carburising processes 16
1.9. Hardware 17
1.9.1. Furnaces 17
1.9.2. Gas supply 18
1.10. Troubleshooting: common problems 18
1.10.1. Soot and tar problems 18
1.10.2. Near surace eect 18
2. Quenching characteristics or gas and oil 19
2.1. Quenching in oil 192.2. Quenching in gas 20
2.3. Temperature dierences when quenching in oil and gas 20
2.4 Cooling curves and heat transer coecient (HTC) 21
2.4.1. The gases 21
2.4.2. Mixture o gases 22
Content
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3Low pressure carburising and high pressure gas quenching.
Page
2.4.3. Gas recycle 232.4.4. The infuence o gas pressure and gas velocity 23
2.4.5. The eect o the gas temperature 24
2.5. Properties o the gases 24
2.6. Design o the load 26
2.6.1. Cylinder and axle 26
2.6.2. Disk and gear 27
2.6.2.1. Horizontal position 28
2.6.2.2. Vertical position 30
2.7. Distortion 30
2.7.1. Gears 31
2.7.2. Rings 31
2.7.3. Axles 32
2.8. Interrupted gas quenching 32
2.9. Equipment 33
2.9.1. Single-chamber vacuum urnaces 33
2.9.2. Two-chamber vacuum urnace 35
2.9.3. Multi-chamber vacuum urnaces 37
2.9.3.1. Continuous vacuum urnace 37
2.9.3.2. Linked multi-chamber urnaces 37
2.10. Control 39
2.10.1. Flux Sensor 39
2.10.2. QC3-Sensor 39
2.11. Hardness o dierent steel grades ater gas quenching 40
2.11.1. Hardnesses in the literature 40
2.11.2. Calculation o hardnesses 432.12. Environment 45
2.13. Quenching with high velocity gas 47
2.13.1. Principles 47
2.13.2. Heat transer coecient 49
2.13.3. Quenching a part o the component 51
2.13.4. Applications 52
3. Terminology 53
Reerences 54
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4 Low pressure carburising and high pressure gas quenching.
Low pressure carburising and high pressuregas quenching.
O the many technologies available today to improve the perormance o engi-
neered suraces, carburising is one o the most common. Carburising is enduringlypopular because it uses a higher temperature than most thermochemical proc-esses so that a deep hard layer can be ormed in a short time. The great majorityo carburising processes take place at atmospheric pressure [1] in an atmosphere
containing large quantities o carbon monoxide. The parts are subsequentlyquenched in oil. Recent developments in vacuum urnaces and steel technologyhave meant that carburising can now be carried out in a more environmentally
riendly way under low pressure [2-4].
Figure 1. Double chamber vacuum carburising urnace(photo courtesy o Seco/Warwick)
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5Low pressure carburising and high pressure gas quenching.
The process is particularly applicable to the automotive industry
because o the cleanliness o the operating environment and o the
nished product. As hydrocarbons are used directly as the source o
carbon, the volume o the exhausted toxic and/or combustible process-
ing gases is vastly reduced and relatively benign. The urnaces are
generally more ecient than the atmospheric pressure alternative.
I the steel allows, processing eciency can be urther improved by
increasing the carburising temperature. The use o gas to replace oil
or quenching ensures that the components emerge very clean, bright
and dry, and less distor ted than oil-quenched components. Improving
technologies or making steel have produced carburising steels that can
be quenched in 10 bar nitrogen (N2) [5]. Even the current lower harden-
ability carburising steels can be quenched with improved helium (He)
quenching technology [6]. Vacuum carburising has also been applied to
parts made by powder metallurgy (P/M) techniques [7]. Analysts predictan upward trend in vacuum carburising rom 1% o the market in 2000
to 13% in 2010 [1, 8].
The single chamber vacuum urnace has largely been replaced by the
double chamber unit (Figure 1) or low pressure vacuum carburising.
This type o unit has the advantage that during quenching the urnace
itsel does not have to be cooled, thus lowering the thermal load.
In addition the quenching chamber design can be optimised or the
quenching task alone, rather than the combination o vacuum carburis-
ing and quenching, and there is less contamination o the quenching
gas. The latter is an impor tant consideration i the helium or quench-
ing is to be recycled. Two-chamber urnaces are well suited or smallerthroughputs and where a very high fexibility is necessary, e.g. at
commercial heat treaters.
The next step is a modular vacuum carburising system such as that
shown in Figure 2. The automotive industry requires a higher through-
put, and two-chamber solutions are ar too expensive. In this case the
combination o several individual treatment chambers with one quench-
ing chamber is very cost eective. Depending on the case depth, a
combination o six to eight treatment chambers with one quenching
chamber is the optimum. Small, individually controlled carbur ising units
give maximum processing fexibility. The system is ully automated with
a heat-treated load leaving it every 20 30 minutes.
Figure 2. A modular vacuum carburising system at BMW (photo courtesy o ALD)
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6 Low pressure carburising and high pressure gas quenching.
1.1. History
The possibility o low pressure carburising in vacuum urnaces was
mooted more than 40 years ago [9]. Intensive investigations started
in the 70s, caused by an increase in costs o natural gas and the hope
o dramatic industrial gases savings by this method. At that time low
pressure carburising was unacceptable because o the heavy sooting
produced in the pressure ranges used, between 100 and 600 mbar, and
the diculty o achieving sucient evenness in the carburising results
[10 14].
Reducing the process pressure to values between 3 and 20 mbar so lved
these problems and allowed a denser loading o urnaces [15, 16].
Besides temperature and time, atmosphere composition, number and
length o boost and diusion steps, procedures to homogenise theatmosphere and the infow are o high importance or consistent load
results [17]. In addition to propane, acetylene and ethylene were intro-
duced as carburising gases in low pressure carburising processes
[18, 19].
Plasma carburising can be seen as a variant o low pressure carburising.
The rst hardness proles generated by plasma carburising had been
presented by Edenhoer at Hrterei-Kolloquium, Wiesbaden, 1972 [20].
Methane is the main process gas but the use o propane or mixtures o
these gases with hydrogen or argon is also reported [21 26].
1.1. Dierentiation rom other carburisingprocesses
Gas, plasma and low pressure carburising are compared in Table 1.
1. Low pressure carburising
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7Low pressure carburising and high pressure gas quenching.
Gas carburising Plasma carburising Low pressure carburising
Furnace atmosphere vacuum vacuum
Gases gas mixtures methane propane, acetylene, ethylene,
containing CO, CO2, and other hydrocarbons
CH4, H2 and N2 and their mixture [27]
Gas consumption 3 5 times urnace volume 100 l/(h*m2 load) 100 l/(h*m2 load) *1
(temperature dependent) per hour
Max. temperature 1000C 1300C 1300C
Furnace conditioning necessary not necessary not necessary
Integration in production line? no, unshielded fames, gases yes yes
Process management by gas composition, carburising time length o carburising segments, length o carburising and diusion
pulses segments, and gas fow rate
Process control by carbon potential none No atmosphere CP and its controlSurace eects internal oxidation thermal etching thermal etching
Coverage to hinder carburising cover paste mechanically *2
Carbon transer see table 2
Drillings, blind holes limited up to L/D = 25 up to L/D = 30
*1 Carburising o complex parts requires higher gas fows. Gren [28] states a required gas fow o 400 l/(h*m2) at 2 mbar and 900C to carburise blind holes.*2 The use o average cover pastes in low pressure carburising processes bear the danger that constituents o the pastes are released in the low pressure and condense in hard
layers, which have to be removed ater heat treatment by shot peening.
Table 1: Comparison o the three dierent carburi sing methods
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8 Low pressure carburising and high pressure gas quenching.
1.2 Carbon transer coecientThe carbon transer coecient gives a measure o the velocity o carbu-
rising. It is dened as the mass o carbon di used into a square metre
surace o the carburised par t per hour. It can be calculated rom the
weight dierence o small samples or, more accurately, integrated out
o carbon depth proles.
Table 2 shows values or average carbon transer coecients in d ier-
ent atmospheres and or dierent temperatures in comparison to gas
and plasma carburising.
A high carbon transer coecient is not necessarily an advantage,
because steel suraces can absorb only limited amounts o carbon. With
high carbon mass transers the sur ace o components is saturated very
rapidly. Oversaturation leads to carbide ormation, which should beavoided whenever possible. The only way to prevent carbide orming in
processes with high carbon transer coecients is to shorten the carbu-
rising segments. Segments shorter than one minute, however, increase
the inaccuracy o the carburising results.
1.3 State o the art today
Recent work indicates that carbide ormation and dissolution in car-
burising and diusion segments give rise to thermal etching eects.
Thereore low pressure carburising processes are simulated with pro-
grams using carbon transer coecients that depend on time, tempera-
ture and carbon content to obtain optimal times or the carburising anddiusion segments. With this approach, unusually good results were
achieved on low pressure carburised 18CrNiMo7-6 gears, which reached
the endurance limits o shot peened gears in the unpeened state.
1.4. Low pressure carburising principles
1.4.1 What is low pressure carburising?
The process itsel starts with evacuating the urnace, which is then
lled with nitrogen and heated rom 800C by convection to process
temperature. The heating is completed under vacuum. When the proc-
ess temperature is reached, carburising is carried out in a series o
boost and diusion segments.
Figure 3 shows a schematic illustration o a low pressure carburising
process. The carbon donator, e.g. propane or acetylene, adsorbs at the
surace and dissociates catalytically.
carbondonator(gas)
physicaladsorbtion
chemiesorbtion
recombinationof hydrogen
dissolution of carbon
diffusion
carbondonator(adsorbed)
Figure 3. Process scheme o low pressure carbur ising
Table 2: Values o average carbon transer coecient in g/m2 h in the rst 15 minutes or dierent hydrocarbons and temperatures [29] (values or carburising until thesurace is saturated shown in brackets [30])
Temperature Atmosphere Plasma Low Pressure Carburising
Endogas
Methane Propane Methane Propane Ethylene Acetylene900C 25 (25) 100 0 60 (60) 55 55 (50)
950C 35 (70) 150 0 90 (90) 80 79 (110)
1000C 80 (110) 190 0 130 (140) 120 145 (235)
1050C (155) 20 185 (195) 180 200 (335)
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9Low pressure carburising and high pressure gas quenching.
I the carbide ormation limit o the steel is exceeded, carbides can orm
in the outer surace o the components. The maximum length o carbu-
rising (boost) steps is thereore given by the carbide ormation limit o
the steel at process temperature (Figure 4).
The diusion step is carr ied out until the surace carbon content has
been lowered enough to attach another carburising segment o reason-
able duration (
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10 Low pressure carburising and high pressure gas quenching.
1.4.2. Benets and drawbacks
The ollowing advantages are oten claimed or low pressure carburis-
ing processes:
1. No internal oxidation
2. Ability to carburise drillings and blind holes
3. The possibility o using high temperatures
4. No urnace conditioning required
5. A reduction in energy and gas consumption [32]
6. Clean and sae working conditions
7. The use o only oxygen-ree gases like propane, hydrogen, argon,
and nitrogen eliminates internal oxidation.
Advantages 3 to 6 are typical eatures o thermochemical treatments in
vacuum urnaces. Furnace conditioning is known to be useul even invacuum heat treatments i there are requent changes in load require-
ments.
A drawback compared to other carburising methods is that problems
can occur with masking parts o components. Compared to gas carbu-
rising, which is controllable by measurement and adjustment o the
Carbon potential, the LPC atmosphere Carbon potential cannot be
controlled.
1.4.3. Pressure range
Low pressure carburising is nowadays carried out in the pressure rangerom 1 to 20 mbar.
1.4.4. Model o carbon transer
The ollowing simplied model describes the transer o carbon at the
steel surace (s) with acetylene as the carburising gas, divided into our
steps [33].
Step 1: Transportation o molecules o acetylene towards the
specimen. Physical adsorption on the specimens surace:
C2H2(gas) 73 C2H2(ad) (1)
Step 2: Chemisorbtion o the atoms o carbon and hydrogen during
dissociation o acetylene on the hot surace o the specimen:
C2H2(ad) + 4s 3 2(C-s)+2(H-s) (2)
Chemisorbed atoms o hydrogen orm molecules o hydrogen which are
released as gas:
2(H-s) 73 H2(gas) + 2s (3)
Step 3: Transer o chemisorbed carbon atoms into a dissolved state:
(C-s) 73 C(diss.) + s (4)
Step 4: Diusion o carbon into the metal lattice
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11Low pressure carburising and high pressure gas quenching.
1.4.5. Reactions
The reactions taking place in low pressure carburising processes are
dependent on the process gas used. The ollowing scheme shows highly
simplied reactions that occur with dierent gases.
The methane produced during pyrolysis is useless or carburising
because o its thermal stability (see above). Furthermore many dier-
ent species o gas exist in parallel. However acetylene is the only spe-
cies applicable to the carburising o steel at low pressure. The amount
o propane that must be applied to provide a homogeneous carburis-
ing depends on a sucient amount o acetylene being produced during
pyrolysis. In consequence the amount o propane has to be signicantly
higher than the amount o acetylene.
1.5. Low pressure carbonitriding
1.5.1. Principles
Unlike carbonitriding processes in gas atmospheres, low pressure car-
bonitriding is carr ied out as an integrated process o low pressure car-burising and nitriding at low pressure. There are two dierent approach-
es to obtaining sucient nitrogen in the sur ace layer. Introducing pure
nitrogen, which will dissociate at temperatures above 1000 C can do
the nitriding. In the majority o cases, however, ammonia is added dur-
ing the last diusion segment.
It is not useul to add ammonia in earlier diusion segments, since
nitrogen will immediately euse rom the surace in low pressure seg-
ments. This ollows Sieverts law, which describes the decreasing solu-
bility o nitrogen in steels as the pressure alls. For that reason the pres-
sure is typically increased up to at least 10 mbar during the adjacent
nitriding segment to provide sucient solubility o nitrogen in steel.
C3H8
CH4
C2H4
C2H6
C 3H6
C2H2
-CH4
-H2
-C2H4
-H2
-C 2H2
-CH4
2x-H2
-H2
+C 2H4/-C3H6
x2
C 6H6 carbonblack
x3 -3 H2
Figure 6. Network o homogeneous propane pyrolysis
methane
ethane
propane
ethene
acetylene
pyrolysis at 4 mbar above 1000 C
above 600 C (mainly)
under 10 mbar above 700 C (mainly)
under 10 mbar above approx. 850 C
above 800 C dissociationbelow 800 C polymerisation
(up to 940 C mainly)
(vinyl acetylene)
4C + 2Hy (at steel surface)
complex reaction
stability increases with T, C-availabity higher at lower T
The pyrolysis o hydrocarbons is always temperaturedependent. The
equations above show that ethane and propane decompose mainly to
orm methane, which will not decompose at 4 mbar at temperatures
below 1000C. At temperatures below 800C acetylene orms long-
chained hydrocarbons and aromatics. Above 800C it dissociates in a
complex reaction, whose last stage needs a s teel surace as a catalyst.
The dissociation o propane is quite complex because a variety o di-
erent components orms during the cracking processes o pyrolysis.
The existence o so many hydrocarbons and radicals leads to a complex
chain o cracking and recombination, described by Gra et al. [34] and
shown in Figure 6.
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12 Low pressure carburising and high pressure gas quenching.
1.5.2. Benets and drawbacks
The most signicant benet o a higher nitrogen concentration in steels
is that the austenite exists at lower temperatures, which leads to a bet-
ter hardenability as well as stabilised retained austenite [35]. Nitrogen-
martensite, with signicantly higher amounts o nitrogen, may also be
ormed.
Carbonitrided steel with an accumulated amount o more than 1% car-
bon and nitrogen can provide signicantly higher amounts o stable
retained austenite. This can improve the mechanical properties, espe-
cially wear resistance.
Two drawbacks are the high ammonia consumption o the process and
the technical requirements o the vacuum urnace. Ammonia dissoci-ates very rapidly at temperatures above 850C. Only small amounts o
ammonia are let to dissociate on the load. To provide a homogeneous
carbonitriding process, the quantity o added ammonia should be about
5 10 times greater than the amount o carburising gas [35].
The requirements or urnaces used or low pressure carbonitriding
are related to the special conditions or using ammonia. The gas sup-
ply system and the exhaust system must be ree o non-errous metals.
Vacuum pumps without non-errous metals are not available at present.
The use o ammonia exposes these components to a signicantly higher
risk o corrosion, which may shorten their lives.
1.6. Gases used or the LPC processesLow pressure carburising is carried out in dierent atmospheres:
x In hydrocarbons
x In a mixture o hydrocarbons and noble gases or hydrogen.
For most hydrocarbons a precondition or a low pressure carburising
process is the decomposition o the hydrocarbons at high temperatures.
This is called cracking or pyrolysis. The decomposition reactions depend
on gas type and temperature. A detailed description o possible reac-
tions is given in the doctoral thesis o Gren [28]. He gives an exten-
sive compilation o relevant data or low pressure carburising.
1.6.1. Choice o gas or carburising
Low pressure carburising can be carried out with dierent gases de-
pending on the application, the shape o the parts and the temperature.
Methane is stable up to high temperatures. Measurements by Dorn
using a mass spectrograph at IWT conrmed these results (Figure7).
Methane is generally used in plasma-assisted carburising processes
where local protection rom carburising is needed, as this can easily be
done by masking.
Propane can be used over the whole temperature range, rom low tem-
perature carburising (300 400C, used or carburising o austeniticsteels without loss o corrosion resistance [36]), to high temperature
carburising (
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13Low pressure carburising and high pressure gas quenching.
propane, parameters such as the density o loads and the ratio length/
diameter o blind holes can be increased. At higher temperatures there
is a disadvantage: the dissociation reactions change, making less car-
bon available. At lower temperatures (< 800C [19]) polymerisation
reactions take place.
Acetylene is used at a low pressure level o 2.5 mbar to suppress the
ormation o soot and short-chain hydrocarbons. Otherwise, acetylene
makes a high proportion o carbon available. This is the reason or its
good perormance in treating dense loads or complex shapes.
Propane remains popular but most new systems use acetylene.
1.6.2. Purity o gases
IWT, Bremen has collaborated with AGA AB (member o the Linde
Group) to investigate the infuence o the purity o the gases. Gases o
standard quality were compared with a gas mixture containing signi-
cant amounts o higher-chain hydrocarbons. To nd out how much soot
builds up in the urnace during the carburising processes, a ceramic
plate was xed on the most sensitive ceramic component in the ur-
nace during each process. The Institutet r Metalorskning, Stockholm,
measured the carbon uptake o these ceramic plates using a combus-
tion method. Figure 8 shows that there is hardly any di erence in the
carbon pick-up with the dierent gas qualities. The carbon content o
the ceramic plates increases slightly as the gas quality decreases. In
comparison it could be seen that, while the carbon pick-up increasesby only about a third, the carbon content o the ceramic plates is about
our times as high as in the results o plasma carburising processes. Fig-
ure 9 shows that, while the carbon pick-up decreases only slightly when
an atmosphere containing hydrogen is used, the carbon content o the
ceramic plates almost halves.
1.7. Process parameters
1.7.1. Process design
Figure 10 shows the process design schematically with the actors on
which it depends. Processes have hitherto been designed in a t rial and
error ashion through a reiterative cycle o simulation and result com-
parison.
The infuence and eects o the dierent input parameters are
described in the ollowing sections.
Figure 8. The infuence o gas quality on the average carbon pick-up and carboncontent o the ceramic plates during low pressure carburising
0
20
40
60
80
averageCpick-up[gC/m*h]
0
1
2
3
4
5
C-contentofceramicplate[gC/m]
N2 H2carrier gas
Calculated out of weight difference
Integrated from C-Curve
carbon content of ceramic plates
Low pressure carburizing
Figure 9. The infuence o gas composition (carrier gas) on the average carbonpick-up and carbon content o the ceramic plates during low pressurecarburising
Low pressure carburizing process
pressure
atmosphere
gas flow rate
batch (surface)
gas type
carbon transfer
carbon profile
temperaturesteel grade
simulation
carburizing- and diffusion segments
Figure 10. Schematic o the low pressure carburising process
0
20
40
60
80
averageCpick-up[gC/m*h]
0
1
2
3
4
5
C-contentofceramicplate[gC/m]
3.5 2.5 mixtureGas quality
Calculated out of weight difference
Integrated from C-Curve
carbon content of ceramic plates
Low pressure carburizing
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14 Low pressure carburising and high pressure gas quenching.
1.7.2. Carbon mass fow
There are two sets o parameters in operation: the parameters that
infuence the transer o carbon rom the atmosphere to the parts and
those that infuence its subsequent diusion into the part. The combina-
tion results in a carbon mass fow.
1.7.3. Gas fow rate
Figure 11 shows the eect o the process gas fow rate on the average
mass transer. The mass fow o carburising gas cannot be used directly
to control the surace carbon content or carburising depth, since under-
dosing causes a carbon fow under-supply in the load. In consequence
components that interact with the gas supply rst, because o their
position in the load, will be carburised correctly but units urther downthe line will not received enough carbon. In consequence the load will
not have homogeneous case depth and surace carbon content.
On the other hand the aim cannot be to supply as much gas as possible,
because this could result in soot ormation in the atmosphere.
1.7.4. Gas type
Investigations o the infuence o the type o process gas used on the
carbon mass fow were done by Gren [28]. During these investigations
carburising was carried out in a single process with no extra diusion
step, to allow the carburising behaviour to be characterised. No signi-cant dierence was ound between the types o gas investigated, apart
rom methane, which does not dissociate thermally at temperatures
below 1100C. Investigations by Steinbacher [38],however, did show a
dierence between acetylene and propane during carburising. Since
acetylene carburises samples directly while propane needs to decom-
pose by pyrolysis, carburising with acetylene is aster at the beginning
o the process (Figure 12). The acetylene generated by the pyrolysis o
propane is the only source o carbon. This aects how much carbon is
available locally and can cause inhomogeneous sur ace carbon con-
tents in the load.
C-quantityg/m2h
70
60
50
40
30
20
10
0
15 l/h
500 l/h300 l/h200 l/h100 l/h50 l/h
25 l/h
C2H2t = 10 min
p = 2 mbarT = 900 C16 MNCr 5
flowrate
Figure 11. The dependence o carbon mass fow on process gas fow rate [28]
0
5
10
15
20
25
30
0 1 2 3 4 5 6 7 8
time [min]
specificmassgain[g/m
2]
acetylenepropane
Figure 12. Specic mass gain o a 20MnCr5 sample carburised with identical atmos-phere parameters in propane and acetylene
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15Low pressure carburising and high pressure gas quenching.
1.7.5. Temperature
The process temperature during carburising aects the di usion and
solubility o carbon in steels. As Figure13 shows, an increase in tem-
perature reduces the process time, because the carbon diuses at a
higher rate.
In addition to the positive eect on the diusion velocity, carbon also
becomes more soluble in the s teel, as shown in Figure 14.
In consequence more carburising gas must be supplied to provide
enough carbon or the higher carbon transer (Figure 15).
0
5
10
15
20
25
30
900 950 1000 1050
Carburizing temperature C
Carburizingtime
h
0,5 mm
1.0 mm
1.5 mm
2.0 mm
3.0 mm 4.0 mm 18CrNiMo7-6Heating 3 C/minLowering to 840 CHold 840 C 30 min.CAt = 0.28 %
CR = 0.66 %
-35 %
Figure 13. Process time reduction at rising temperature
20MOCr421NiCrMo2
15CrNi616MnCr5
Ck1517CrNiMo6
10Cr4
1000
950
900
850
800
750
C
0.20 0.40 0.60 0.80 1.00 1.20 1.40 %
Mass % Carbon
Temperature
Precipitationof Cementit
G
S
S
EE
Figure 14. Maximum carbon dissolution in austenite depending on temperature
0
5
10
15
20
25
30
0 1 2 3 4 5 6 7 8
time [min]
specificmassgain[g/m2]
Steel grade (DIN-EN):Gas:Flow rate:
Pressure:
20MnCr5propane10 ml/min940 l/m2h5 mbar
Figure 15. Dependence o specic mass increase on carburising temperature
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16 Low pressure carburising and high pressure gas quenching.
1.7.6. Pressure
The eect o gas pressure on the results o carburising parts o simple
geometry is negligible. Generally or low pressure carburising a more
complex geometry is linked to areas less accessible to the gas stream,
like bores or blind holes and small gearwheels. Providing these areas
with carbon demands a lower process pressure and a dynamic gas
exchange. This is best provided by short boost and vacuum segment
series. The continuous change o pressure makes it possible or the
achievable process.
Furthermore, as mentioned beore, pressure infuences soot ormation
and polymerisation o reaction products.
1.7.6. Steel grade
The grade o steel has three dierent aspects:
x maximum carbon dissolution
x carbide ormation
x diusion velocity
The maximum amount o dissolved carbon changes with the quantity
o substitution alloy elements (see Figure 14). It is generally considered
that the more alloying elements present, the less carbon can be dis-
solved. In consequence the surace will become saturated and carbides
may be ormed earlier.Other issues related to the alloy content are the amount o carbides to
be precipitated and the type o carbide ormed. Elements like chromi-
um, molybdenum, vanadium and tungsten, which are added to accel-
erate precipitation, will orm carbides which can only be dissolved at
higher temperatures.
Some alloying elements have a strong infuence on the diusion o
interstitial elements like carbon. Most o the alloying elements that
positively infuence carbide ormation also lower the diusion veloc-
ity o interstitial elements. Figure 16 shows an example or chromium
alloyed steels. In consequence most alloying elements reduce the case
depth and accelerate carbide precipitation. To avoid the precipitation o
carbides, short boost segments should be used.
1.8. Control o process parameters
1.8.1. Simulation o low pressure carburisingprocesses
Simulation o gas carburising is well developed, but simulation o low
pressure carburising is more dicult. On one hand, process design uses
experimental data, e.g. or serial processes. On the other, institutes and
urnace constructors use programs they have developed themselves.
The problem with simulation is that there are ew data on carbon t rans-
er during the boost steps. How temperature, gas type, steel grade, sur-
ace carbon content and conditions o carbide ormation and dissolution
all depend on carbon fow are not yet precisely known. These programs
are usually run with experimentally tted data, which contain uncer-
tainties. Todays data provided or simulation are typically obtained rom
the results o carburising experiments rom which the carbon mass fow
is integrated. This carbon mass fow is highly dependent on the lengtho the previous boost step. I there is a signicant dierence between
the timing o the segments, the results may deviate rom reality.
A more convenient way to obtain the eect o the many dierent infu-
ences on mass fow data is to use thermogravimetric measurement. This
method acquires the carbon mass fow by measuring a samples weight
0
5
10
15
20
25
30
0 1 2 3 4 5 6 7 8
time [min]
specificmassgain[g/m2]
diffusiondiffusion
C-saturation of surfaceC-saturation of surface
Diffusion and
carbid formation
Diffusion and
carbid formation
Steel grade (DIN-EN):Gas:Flow rate:
Pressure:
20MnCr5propane10 ml/min
940 l/m2h5 mbar
Temperature: 1050 Cmo
Figure 17. Carburi sing o a 20MnCr5 sample: 1050C, 940 l/(m2h), propane, 5 mbar[38]
0
5
10
15
20
25
30
0 1 2 3 4 5 6 7 8
time [min]
specificmassgain[g/m
2]
30Cr6 15Cr12 30Cr12
Figure 16. The dependence o mass gain on the grade o steel
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17Low pressure carburising and high pressure gas quenching.
change during carburising. Most signicant infuences like temperature,
steel grade, gas type and their interrelation can be veried this way.
An example o one such measurement is given in Figure 17, which
shows the specic weight change o a sample o 20MnCr5 dur ing carbu-
rising in propane at about 1050C or eight minutes. Using a tted expo-
nential saturation unction, as shown in Figure 18, and dierentiating
it will give a carbon mass fow unction, which can be used to describe
the rst boost step o a sample in a diusion simulation.
A matter o special importance is the interrelation between the accu-
mulated carbon prole rom the ormer boost steps and the newly
arranged carbon mass fow unction as shown in Figure19. In act there
are two infuences that have to be considered:
x Higher surace carbon content and thereore earlier saturation o
austenite
x Change o diusion speed because o the accumulated prole and
reduced gradients.
Theoretically many experiments would be needed to obtain the exact
relationships. A simpler but quite eective approach is to obtain the
carbon mass fow unction o the rst carburising step and use it as a
basis or the subsequent ones. To account or the aster saturation and
slower diusion, a coecient can be derived, which will result in a
lower mass fow using a time shit that depends on the surace carbon
content.
1.9. Hardware
1.9.1. Furnaces
Conventional vacuum urnaces are used or low pressure carburising.
Furnace construction used to be based on a heating and carburising
chamber made o steel, which is not the ideal choice because o the
large catalytic area o the whole retort during carbur ising. These steel
retort urnaces will need a signicant higher gas supply than a urnace
with an inactive retort made o ceramics or graphite.
Most recent urnaces are equipped with a graphite chamber and graph-
ite heating, which will not interere with the carburising process by cat-
alysing a reaction o the process gas. The only drawback o a graphite
retort is that the oxygen partial pressure has to be kept low.
Todays standard vacuum urnaces can be subdivided into two major
groups:
x Single chamber urnaces
x Multi-chamber urnaces
In a single chamber urnace, carburising and quenching is done in the
same chamber. These urnaces are very oten combined with high pres-
sure gas quenching technology to quench the load. The drawback o
the combined carburising and quenching chamber is that the chamber
has to be quenched as well as the load. The result is a lower coolingrate compared with a two-chamber or multi-chamber system. The multi-
chamber system is able to combine the fexibility o using dierent,
even liquid, quenching media with a signicantly higher heat transer
rate, because the quenching chamber is cold (see section 2.9).
0
3
6
9
12
15
0 1 2 3 4 5 6 7 8
time [min]
specificmassgain[g/m2]
fitted function
measured weight gain
Steel grade (DIN-EN):Gas:Flow rate:
Pressure:
16MnCr5acetylene4 ml/min
380 l/m2h5 mbar
Temperature: 940 C
Figure 18. Fitted exponential saturation unction compared with measurement:16MnCr5, 940C, 380 l/(m2h), acetylene, 5 mbar [38]
0
200
400
600
800
0.0
0.5
1.0
1.5
2.0
0 5 10 15 20 25 30 35 40 45 50 55 60 65time [min]
0
Surfacecarboncontent[weight%]
Steel grade (DIN-EN):Gas:Flow rate:
Pressure:
20MnCr5acetylene4 ml/min
380 l/m2h5 mbar
Temperature: 1050 C
massflow
[g/m2]
Figure 19. Carbon mass fow and surace carbon distribut ion (carbon in solution)during a simulated multi-step carburising process: 20MnCr5, 1050C,acetylene [38]
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18 Low pressure carburising and high pressure gas quenching.
1.9.2. Gas supply
The gas supply equipment o a urnace used or low pressure carburis-
ing should contain no non-errous metal i acetylene is to be used or
carburising. A multi-stream supply system with multiple inlets can be
used to assist uniormity o carburising. I a carbonitriding process is
required, the exhaust system should also be ree rom any non-errous
metal.
1.10. Troubleshooting: common problems
1.10.1. Soot and tar problems
Soot orms i there is too much carbon present in the carbur ising atmos-phere. It can be observed that thermally dissociated ree carbon is
ormed i the gas fow rate is too high respective to the total surace
o the load. In the 1970s, when relatively high process pressures were
used, soot sensors (photo sensors) were used to detect soot by measur-
ing the adsorption o light by the soot og [12]. The process gas fow rate
was controlled as a means o controlling the rate o sooting.
Soot can be minimised by adapting the fow rate to the total surace o
the load and also by limiting the pressure. Tar (long chained hydrocar-
bons) can also orm by complex polymerisation processes, which have
not been suciently investigated up to now. Hydrocarbons and soot are
oten ound in cold parts o plants. Processes that run continuously arereported to produce especially high amounts o tar and soot.
1.10.2. Near surace eects
Internal oxidation is a well known damaging eect in gas carbur ising
processes. It reduces the amount o dissolved alloying elements and
thereore the hardenability in the outer region. The oxides ormed
especially on grain boundaries reduce the atigue strength through
notch eects.
Components carburised at low pressure show no signs o internal oxida-
tion, but other eects are reported, including:
x Eusion o elements, especially manganese
x Formation o carbides on grain boundaries, i the carburising
parameters are less than optimal
x Etching at austenite grain boundaries during the carbur ising step[39], which can be considered as notches.
Recent research work indicates that element eusion and carbide or-
mation and dissolution during the low pressure carburising process
ampliy thermal etch eects. Optimised simulation o the carburising
process led to a marked increase in atigue resistance [40, 41].
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19Low pressure carburising and high pressure gas quenching.
2. Quenching characteristics or gas and oil
Heat treatment operation or hardening steels consists o heating and
quenching processes. Although both are important or the resulting
characteristics, the quenching sequence is generally the more critical. It
must be carried out at a controlled cooling rate in order to achieve the
correct hardness and structure. A cooling rate that is too high generally
results in higher strength and hardness. At the same time a quenching
process with a high cooling rate is associated with greater distortion,
and maybe even cracking.
The rate o cooling must thereore be suited to the type o material and
to the shape and dimensions o the component. Oil is today the most
common quenchant, especially or carburised components, but the use
o high pressure gas quenching, HPGQ, is increasing.
2.1. Quenching in oil
The quenching process [42] in oil can be divided into three phases:
x Vapour phase
x Boiling phase
x Convection phase
Figure 20 shows a schematic representation o the three phases during
quenching. The heat transer in each phase ollows a di erent mecha-
nism and each phase plays its part in the nal result.
In the vapour phase, the surace temperature o the component being
hardened is so high that the liquid quenching media, oil, is rapidly
vaporised and a thin, thermally insulating lm o oil vapour orms over
the entire part. This vapour phase must not last too long i undesirablephase changes to errite and pearlite in the steel are to be avoided. The
actual length o time varies considerably, depending on actors such as
the oil itsel and its latent heat o evaporation, the surace condition o
the component and the packing pattern o the load.
1000
900
800
700
600
500
400
300
200
100
0
1007550250
2015105 5
Cooling rate [C/S]
Time [s]
Temeperature[C]
0
Vapourblanket
Boiling
Convection
Cooling rate
Figure 20. Typical cooling curve or oil quenchants
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20 Low pressure carburising and high pressure gas quenching.
During the boiling phase, the oil comes into direct contact with the hot
surace and is immediately boiled away, increasing the rate o heat
removal. In most cases, or ecient cooling o any particular grade o
steel, the rate o cooling must be highest over the same temperature
range as the errite and pearlite nose or the material in the time tem-
perature transormation (TTT) diagram.
The convection phase begins when the surace temperature o the com-
ponent alls below the boiling point o the oil. During this phase, the
fow velocity and the temperature o the oil primarily determine the rate
o cooling. A low boiling point results in a high cooling capacity.
2.2. Quenching in gas
The quenching process in gas consists o only one phase [43], the con-vection phase, which starts at the beginning o the quenching process
(see Figure 21). During this phase, the fow velocity, pressure and tem-
perature o the gas primarily determine the rate o cooling. In theory
heat is also removed through radiation to the surrounding walls and
between the components, but in practice this has very little eect com-
pared with the convection, so it is usually ignored.
Figure 21 shows the dierences between the two quenching media. For
most gases in common use under typical conditions the maximum heat
transer coecient or the oil is two or three times higher than or gas.
It can also be seen that the nal temperature or gas quenching is lower
than that or oil. That is quite natural as the gas temperature at the endo the quenching is about 30 50C while the oil temperature might be
80 120C.
2.3. Temperature dierences when quenching
in oil and gasWhen a component such as a cylinder [44] is quenched in oil, it is rst
surrounded by the vapour phase. The vapour phase collapses ater a
short time, and is replaced by the boiling phase. Ater urther cooling
the convection phase begins. Normally all three phases co-exist or a
period, see Figure 22 at let, until nally only convection remains.
The centre section o Figure 22 shows how the heat transer coecient,
a , is calculated or oil and water. The maximum a-value or oil is almost
5000 W/m2C, which is normal or ast quenching oil.
While the three phases coexist there is a large temperature dierence
between the surace and the core and in the axial direction o the cyl-inder. To the right in Figure 22 the uneven temperature within the cylin-
der can be seen. The maximum temperature is 750 C and the minimum
temperature is less than 200 C at the sur ace. This uneven temperature
causes stresses that deorm the component and urther distortion also
arises because the transormation to martensite starts at a dierent
time.
Gas quenching will have a convection phase only and give a constant
heat transer coecient e.g. 1000 W/m2C along the cylinder, see
Figure 23.
Because the heat transer coecient is constant, the axial temperaturegradient within the cylinder shown to the right in Figure 23 is small.
This type o quenching gives more homogenous stresses and thereore
less distortion. When the gas fow is perpendicular to the cylinder, as
in Figure 23, it results in an uneven heat transer coecient around the
cylinder.
0
100
200
300
400
500
600
700
800
900
0 20 40 60
Time, s
Temperature,
C
0
100
200
300
400
500
600
700
800
900
0 1000 2000 3000 4000 5000
Heat Transfer Coefficient, W/m2 C
Tenmperature,
C
Figure 21. Typical cooling curve or gas (red), in this case helium at 10 bar. Forcomparison the curve or a hot quenching oil is also shown (blue). [43]
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21Low pressure carburising and high pressure gas quenching.
However, during normal quenching the fow direction is parallel to the
cylinder, as usually long thin cylinders are charged into the urnace ver-
tically. Here the heat transer coecient decreases along the cylinder,
see Figure 24.
2.4 Cooling curves and heat transer
coecient (HTC)As Figure 21 shows, the quenching characteristics o oil and gas are
quite dierent, which should be remembered when reading this sec-
tion. The heat transer coecient, HTC, is an important input parameter
or simulation o the hardness, distortion and stresses o a component.
It also characterises the quenching properties o quenchants.
For oil, the three phases are quite distinct . For gas the HTC, ater a
short temperature drop, stabilises at an almost constant value, which
depends on the type o gas or mixture, the pressure and gas velocity as
well as the geometry o the component and its orientation.
2.4.1. The gases
An average value or the HTC can be calculated rom the theory and the
calculation ormulae developed or a heat exchanger when the gas fow
is perpendicular to the tubes [45]. Figure 25 shows the HTC and how it
varies with pressure and gas velocity.
The curves have been calculated or the our most commonly used
gases.
x Argon (Ar) is used or components whose surace would react with
any other gas.
x Nitrogen (N2) is used most oten in this context, because it is cheap
and widely available.x Helium (He) has better cooling properties than N2 but is much more
expensive and is thereore used less.
x Hydrogen (H2) has the best cooling capacity and is cheaper than He.
Because hydrogen in combination with oxygen may orm a combus-
tible mixture, however, all hydrogen installations are subject to spe-
cial saety precautions and are, so ar, very little used.
Figure 23. Heat transer coecient and temperature distribution with perpendicu-lar gas quenching o a cylinder
h1
h2
h3
h1 > h2 > h3
Figure 24. Heat transer and temperature distribution during parallel gas quench-ing o a cylinder (where h is the heat transer coecient).
Figure 22. Heat transer and temperature distribution in oil quenching a cylinder
However, the eects o dierences in the heat transer coecient are
small in comparison to the larger dierences occurring with oil quench-
ing. Thus gas quenching normally causes less distortion. Both axial andperpendicular fows cause di erences in the heat transer coecient
along the component; sometimes it would even be more benecial to
quench in a perpendicular direction in order to get a more even heat
transer (Figure 36).
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22 Low pressure carburising and high pressure gas quenching.
The gas speed and pressure are the main parameters aecting the cool-
ing characteristics, as well as the gas composition. Figures 21 and 23
illustrate that quenching is done by convection only. An increase o gas
pressure, and thereore velocity, means that the HTC rises. As Figure 25
shows, this results in aster quenching.
2.4.2. Mixture o gases
A mixture o gases has an optimum composition or heat transer. Figure
26 shows the infuence on the HTC o adding He to an N 2 atmosphere,
compared with the addition H2. For both mixtures the maximum value o
the HTC is reached at about 80%.
1.5
1.4
1.3
1.2
1.1
1
Coe
cent
0 1004020Helium content
8060N
2He
0 1004020Hydrogen content [%]
8060H
2
1200
900
600
300
0Heat-transfer-coefficient[W/m2K]
Figure 26. Heat transer coecient or gas mixtures in a nitrogen atmosphere. For the H2-N2 mixture the points S1 to S7 indicating the dierent positions in the load.
3000
2500
2000
1500
1000
500
0 352015105
Cylinder 12.5 mm
Gas velocity [m/s]
h
[W/m2K]
3025
H2
He
N2
Ar
3000
2500
2000
1500
1000
500
0 352015105
Cylinder 12.5 mm
Pressure [bar]
h
[W/m2K]
3025
H2
He
N2
Ar
20 bar 15 m/s
Figure 25. Relationship between the heat transer coecient at 500 C or pressure and gas velocity
With a mixture o He N2 the HTC will remain the same as or 100% He
[46] even when the He content is 60 70%. This will reduce the cost o
the quenching gas. However, when quenching with pure helium, the
helium recycling system should always be implemented (see Section
2.4.3 or urther details). For the H2 N2 mixture [47] the content o H2
can be 30-40%, which is comparable to 100% H2. In this case it is advis-
able to use a mixture o 70 80% o H2 in order to take advantage o
the higher HTC, about 20 30% compared to 100% H2.
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23Low pressure carburising and high pressure gas quenching.
2.4.3 Gas recycle
Recycling o nitrogen is not economically attractive, but i helium is
used, experience shows that recycling can reduce the cost (Figure 27).
However, careul consideration needs to be given to actors such as the
purity required in the output gas, the pressure and the time available to
carry out the recycle. Because o the high capital cost o the equipment
and the gas losses, the amount o cost saved by the use o a properly
optimised helium-based quenching system depends on the gas quality
required rom the recycling system. A simple helium recycling system
with minimal clean-up, and hence minimal losses, on a typical vacuum
carburising installation with one urnace, can reduce helium costs by at
least hal [48].
2.4.4. The infuence o gas pressure and gasvelocity
The ollowing expression shows the relationship between the HTC, pres-
sure and gas velocity [49].
h = C. pm . vn
h = Heat trans er coecient, W/m2 C
p = Gas pressure, bar
v = Gas velocity, m/s
C, m, n = Constants, depending on the chamber, load conguration and compo-
nents. For a perpendicular gas stream, m and n are equal to 0.6 0.8
In a quenching chamber the gas velocity is controlled by the an speed.
A lower an speed gives slower cooling, (see Figure 28 [50]). Cooling in
He at 20 bar, with the an running at 75% o maximum speed, provides
a cooling capacity equal to that o He at 10 bar and 100% an speed.
Higher gas velocities bring more gas molecules per unit o time into
contact with the surace o the component and remove heat at a aster
rate.
The eect o gas pressure or He and N2 on the cooling rate [51] is
shown in Figure 29. When the quenching changes rom N 2 at 10 bar
to He at 10 bar, the maximum rate increases by about 50 70%. An
increase to 20 bar He gives an increase o 40% in comparison with 10
bar He. A urther increase to 40 bar gives another increase o 40%. 40
bar is however not practical as yet, but is shown here as a possibility.
Figure 27. A helium recycle system (photo courtesy o ALD)
0
900
800
700
600
0 240150120Time [s]
210180
Temperature
[C]
906030
500
400
300
200
100
20 bar He, 25 100 %
10 bar He, 100 %
25 %
50 %100 %
75 %
Figure 28. The eect o an speed on cooling. He at 10 and 20 bar using a 30 mmtest piece o Inconel 600 with the thermocouple in its centre. Coldquenching chamber at IVF. [50]
0
900
800
700
600
0 10050Cooling rate [C/s]
75
Temperature
[C]
25
500
400
300
200
100
Figure 29. Cooling curves or dierent pressures o He and N2. Cold quenchingchamber at IVF.
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24 Low pressure carburising and high pressure gas quenching.
2.4.5. The eect o the gas temperature
The gas temperature is one o the parameters needed to calculate
the HTC. Very oten a constant value is assumed, but in an indus-
trial quenching chamber the gas temperature varies over the time o
quenching. The actual gas temperature at any time is needed in order
to get the most accurate value. However, the
temperature o the inlet gas is always lower
than the outlet gas as it heats up passing
through the load. The solution [52] is to use
the average temperature between the inlet
and outlet temperature (see Figure 30).
During the starting phase o quenching the
inlet temperature rises about 40C and theoutlet temperature increases by about 100C.
This means that components at the top and
the bottom o the load are quenched at a slightly dierent temperature.
The calculated HTC is however a mean value or the whole load.
2.5. Properties o the gases
x The rate o heat transer by convection is governed by: the gases
and their thermophysical properties (see Table 3)
x the body geometry
x the average gas velocity, pressure and its turbulence.
In order to calculate the heat transer coecient, h, the well-known key
values such as Nusselt, Reynolds and Prandtl values must be known,
see ormulae below.
Nu = h d /l (1)
Re = U d /u (2)
Pr = ur Cp /l (3)
h = heat transer coecient, W/m2Cd = characteristic measure, e.g. the diameter o an cylinder or axle, ml = gas thermal conductivity, W / m KU = gas velocity, m/su = kinematic viscosity, m2/sr = gas density, kg/m3
Cp = gas specicity heat capacity, kJ/kg K
0
150
125
100
75
0 200140120Time [s]
180160
Temperature
[C]
1008060
50
25
Gas outlet
4020
Mean value of gas temperatures
Gas inlet
Figure 30. Gas temperature during quenching at 10 bar He in a cold chamber.
Table 3: Physical properties o the gases at 15C and 1 bar [53].
Properties Argon Nitrogen Helium Hydrogen
Density, kg/m3 1.67 1.17 0.17 0.08
Spec heat capacity, kJ/kg K 0.52 1.04 5.19 14.30
Thermal conductivity W/m K 0.017 0.026 0.154 0.191
Dynamic viscosity Ns/m2 23 x 10-6 18 x 10-6 20 x 10-6 9 x 10-6
Kinematic viscosity, m2/s 0.14 0.15 x 10-4 1.19 x 10-4 1.06 x 10-4
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25Low pressure carburising and high pressure gas quenching.
These three key values (1 3) have the ollowing correlation:
Nu = C Rem Prn (Pr/Prs )r (4)
Pris the Prandtls value in the gas volume and Prs is the value close to
surace o the component.
C, m, n and rare constants. These constants vary with the design o the
quenching chamber, conguration o the load, position and geometry o
the components and so on. Mostly the value o n is about 0.3 0.4 and
value o r is around 0.25. However, the values o Cand m depend on
the magnitude o the Re value [54] (see Table 4). Similar results have
also been reported by R. Wiberg [55].
From Equation 4 it is possible to calculate the heat transer coecient,
h, using the suggested values or the constants n and rand the m value,
which normally is ~ 0.7.
h = C U0.7
d-0.3
l0.7
u0.4
r0.3
Cp0.3
(5)
The calculated value o h is an average or a component similar to a cyl-
inder or an axle. Its important to keep in mind that the h value varies
over the surace o the component (see 2.6).
Now the heat transer coecient is known, the time, t, it takes to
quench rom one temperature to another can be calculated.
(6)
W = weight o component, kgA = surace area o component, m2
T = average temperature o gasT1 = start temperature or componentT2 = end temperature or component
The physical properties in Table 3 are given or 15 C and 1 bar. When
the temperature and, especially, the pressure are higher, some proper-ties will change. For a more qualied and more exact simulation it can
be valuable to use the corrected values as shown in Figure 31 and 32.
Figure 31 shows the variation in the kinematic viscosity with tempera-
ture at 15 bar or nitrogen. It illustrates that, or example, an increase in
temperature rom 20C to 100C increases kinematic viscosity by 60%.
When this and other temperature-dependent changes are taken into
consideration, the heat transer coecient decreases rom 391 to
355 W/m2C, a reduction o about 10%. In this case the gas velocity is
10 m/s.
Figure 32 shows the change in kinematic viscosity versus pressure at100 C or nitrogen. An increase o pressure rom 10 to 20 bar decreases
the kinematic viscosity by about 50%.
The change in the kinematic viscosity that comes with a pressure
change rom 10 20 bar increases the heat transer coecient rom 355
to 480 W/m2 C.
0
3,0
2,5
2,0
1,5
0 300150100Gas temperature [C]
250200Kinemati
cviscosityx0,0
00001m2/s
[C]
50
1,0
0,5
Figure 31. Kinematic viscosit y versus gas temperature at 15 bar nitrogen.
0
5,0
4,5
4,0
3,5
0 301510Pressure [bar]
2520Kinemati
cviscosityx0,0
00001m2/s
[C]
5
3,0
2,5
2,0
1,5
1,00,5
Figure 32. Kinematic viscosity versus pressure at 100C or nitrogen.
Table 4: Constants and exponents in Equation 4
Re C m
1 to 40 0.750 0.4
40 to 1000 0.510 0.5
1000 to 2 x 105 0.260 0.6
2 x 105 106 0.076 0.7
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26 Low pressure carburising and high pressure gas quenching.
2.6. Design o the load
2.6.1. Cylinder and axle
In the previous sections the heat transer coecient used was an aver-
age value around a test probe, a cylinder or a component. However,
during gas quenching o any component the local heat transer is o
major importance to the nal hardness, uniormity and distortion o
the component. Even or a component as simple as a cylinder there is a
variation both along its length and its circumerence, depending on gas
quenching conditions.
Two major parameters are the turbulence and the Reynolds number
[55]. In a test in a wind tunnel, with axial fow along a cylinder, it wasshown that with a turbulence o 0.3%, which is nearly a laminar fow,
the HTC had the highest value at the back part o the cylinder, see Fig-
ure 33. The same gure also shows how the heat transer coecient
(proportional to the Nusselt number) increases with higher Reynolds
numbers. The Reynolds number is proportional to the gas velocity.
(Note: Nu=d/land when Nu is known rom Figure 30, then h can be
calculated; d is the critical dimension, in this case 0.15 m, where the
trials were made or a cylinder with a diameter o 0.15 m [56]. lis the
gass heat transer capacity, in this case 0.026 (see Table 3). The value
o h is then 175 when Nu is 1000. When Re is 300 000 then the gas
velocity is 30 m/s).
However, with increasing turbulence up to and over 6.7% the HTC over
the cylinder has shited so it has it highest value at the ront part along
the cylinder sur ace (see Figure 33). The turbulence was increased by
inserting a disk with a diameter 1/3 o the cylinder diameter, and one
diameter up in the upstream gas.
Figures 33 and 34 illustrate that with increasing Reynolds number, i.e.
a higher fow velocity, the HTC value also increases. With the actual
parameters the HTC value is about twice as high at the ront o the cyl-
inder as it is at end o the cylinder.
In industrial vacuum urnaces there is a high degree o turbulence. The
normal consequence is that the ront part o a cylinder surace has the
highest HTC value along its length. This has also been noted in other
reported results [56, 57].
A more in-depth analysis o axial fow along a cylinder has been made
with dierent congurations [56] (see Figure 35). In conguration A
there is a ree fow o gas along the cylinder axis which gives a higherheat transer at the ront end o the cylinder. Figure 36 shows the heat
transer coecient over the cylinder or all congurations. The HTC is
high at leading edge o the cylinder, between 0 and 40 mm. Beyond
40 mm the heat transer is more uniorm. This is in good agreement with
the result in Figure 34.
In conguration B where the cylinders are supported with holding bars
there is an increase in the heat transer at the supporting points at 50
and 100 mm. The heat transer coecient is increased locally by 25%,
because turbulence is higher.
In congurations C and D the heat transer coecient is more uniorm.The heat transer coecient appears to vary between 0 and 40 mm
rom the leading edge o the cylinder. Beyond 40 mm, the heat trans-
er is almost uniorm. In conguration C the heat transer coecient
is somewhat higher still. This is in good agreement with results rom
experimentally veried tests.
a
d
b
c
Figure 33. The heat transer coecient (Nusselt numbers) along the cylindersurace. The distance a b is the ront end; b c is the cylinder side; andc d is the rear. The turbulence is 0.3%. (The heat transer coecient isproportional to the Nusselt number.)
d
c
b
a
Figure 34. The heat transer coecient (Nusselt number) along the cylinder sur-ace. The turbulence is 6.7%. The turbulence disk is seen in the ront othe cylinder.
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27Low pressure carburising and high pressure gas quenching.
When the fow o gas is perpendicular to a cylinder axis there will be an
uneven HTC around the cylinder (see Figure 37). Also in this case the
level o the Reynolds number has an infuence. With increasing Rey-
nolds number the HTC has a minimum at 0 degrees (see Figure 37), and
will be rising towards the impingent point at an angle o 90 degrees.
At the same time the HTC will also increase.
Industrial tests o perpendicular gas fow against a cylinder or axle
have shown a higher HTC at the cylinder surace turned into the fow in
comparison with the ar side. One test [56] in an industrial urnace with
about 15 m/s gas fow gave 20% higher HTC at the ront side. Another
test [58] with a very high gas velocity gave a dierence between the
ront and back o a cylinder o 4 6 times higher HTC at the ront side.
In a load with more than one layer, the highest HTC is always ound at
the top layer when the gas fows rom top to bottom. The highest values
are ound in the top layer where the cold and ast gas rst impinges on
the components. The heating up o the gas leads to smaller HTC in the
middle and bottom layers. The reduction depends mainly on the design
o the load. Examples in the literature have reported reduction values
rom 50% [47] and 30% [59].
2.6.2. Disk and gear
Common components that industry needs to manuacture are gears or
the automotive industry. With the increasing use o vacuum carburising
combined with gas quenching it is important to optimise the design o a
load in order reduce distortion as much as possible. An extensive study
[60] has been made, simulating gas quenching o disks and gears, bothin horizontal (lying down) and vertical (hanging) positions (see Figure
38). The simulated gears were plain disks without teeth, but with a cen-
tral hole. The gear has an outer diameter o 25 cm and a central hole o
15 cm. The thickness is 5 cm. This gives the gear a square cross-section
with sides o 5 cm.
a) Configuration A b) Configuration B
c) Configuration C c) Configuration C
Figure 35. Four quenching basket congurations are delineated. (a) No basket,the cylinders stand alone in the quenching chamber; (b) basket madeo bars, currently used in industrial gas quenching processes; (c) basketmade o 3 mm thick plates; (d) basket made o tube with 3 mm wallthickness.
0
800
700
600
500
0 1206040Length [mm]
10080
Hea
ttransfercoefficient[W/m2]
20
400
100
300
200
A
B
C
D
Figure 36. Heat transer distribution over the cylinder surace or all congurations.
0
800
700
600
-90 90300Angle [degrees]
60-30-60
500
400
300
200
100
Simulated
Measured
Heattransfercoefficient[Wm2K-1]
Gas flow -90 deg.
0 deg.
0 deg.
90 deg.
Figure 37. An example o a typical pattern or the HTC around a cylinder.
Cross section
Figure 38. Schematic view o the conguration or two types o load
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28 Low pressure carburising and high pressure gas quenching.
2.6.2.1. Horizontal position
Figure 39 shows the simulated velocity eld over horizontal stacked
gears (the rst and th) with an axial distance o 5 cm between the
gears. The gas velocity is 20 m/s at a pressure o 20 bar. Starting with
the rst gear shown in F igure 39a, the typical fow conguration is:
1. stagnation fow on the upstream surace, accelerating rom the centre
towards the gear corners
2. separation at the corners and change o direction to axial fow
3. ast fow over the outer and inner diameter o all the gears
4. a much slower type o circulation between the gears indicted by the
dark blue arrows to the right o the shown cross-section.
I the distance between the gears is increased, the velocities between
them also increase.
For the rst gear, the gas velocity at the corners is about 16 18 m/s,
while it is lower, about 6 9 m/s, at the ront side and somewhat less,
4 5 m/s, at the ar side. Along the inside and outside the velocity is
more uniorm at about 15 19 m/s. For the th gear, the velocity at the
ront side is lower than or the rst gear, at about 4 5 m/s.
Figure 39. Velocity eld or (a) rst gear upstream; (b) th gear. The distancebetween the gears is 5 cm, and the gas pressure is 20 bar at 20 m/s. Thegas stream is coming rom the let.
a) b)
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29Low pressure carburising and high pressure gas quenching.
Figure 40 shows the variation o the Nusselt value or the rst and the
th gear. The upstream surace or the rst gear is shown in Figure 40a
or all simulated distances between the gears. Figure 40b shows the
same or the th gear.
Figure 41a shows that the distance between the gears has no infu-
ence on the Nusselt number. The upstream gas is undisturbed when it
impinges on the rst gear, which is the reason the Nusselt number stays
the same. The Nusselt number has a minimum almost in the middle o
the surace and is about six times higher at the corners than in the mid-
dle o the ront surace.
The prole o the Nusselt numbers or the th gear is the same over the
ront surace as or the rst gear. The scatter or the dierent distances
is higher but the relationship between minimum and maximum in this
case is only three times.
A similar pattern as in Figure 40b exists or all the other sur aces. Aver-
age Nusselt numbers have been summarised or each gear and are
shown in Figure 41.
The Nusselt numbers are the highest or the upstream rst gear and
then they drop or gears 2 to 5. However the most even Nusselt num-
bers are obtained with the spacing 5 cm apart rom the rst gear,
although the Nusselt numbers are the lowest in this case.
In gas quenching the dierences in HTC over the surace and between
gears and disks are small compared to the dierences in HTC orquenching in oil, where a typical value is 10 20 times higher. This has
a benecial infuence in reducing distortion.
The divergence between the rst gear and disk can be used in a posi-
tive way by replacing it by a thin dummy disk or spoiler, creating a more
uniorm gas fow downstream. This conclusion has been conrmed in
other work.
2
1,5
1
0,5
00 10,40,2
Distance from inner diameter
Nu
x
10-4
0,80,6
5 cm
10 cm
15 cm
20 cm
2
1,5
1
0,5
00 10,40,2
Distance from inner diameter
Nu
x
10-4
0,80,6
5 cm
10 cm
15 cm
20 cm
Figure 40. The calculated Nusselt number over the ront surace, (a) or the rstgear and (b) or the th gear.
a) b)
10,5
8
7,5
7
6,50 521
Cylinder 1 is the first in the f low and 5 is the last
Average
Nu
percylinder
x
10-4
43
5 cm10 cm
15 cm20 cm
10
9
8,5
9,5
Figure 41. Area averaged Nusselt numbers or all gears and all distances.
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30 Low pressure carburising and high pressure gas quenching.
2.6.2.2. Vertical position
For this simulation only three gears were used. Because it includes a
gear located between two others and one that has only one gear next
to it, the results should be adequate to describe the fow and Nusselt
number behaviour or any number o parallel gears in a vertical posi-
tion.
In vertical fow, large dierences in the fow are less likely because o
the direction o the fow and the placing o the gears. Higher Nusselt
numbers are reached in vertical fow, compared to horizontal position
more because o the smaller amount o material, than because o the
hole. This is what makes it easier or the gas to fow through the load,
rather than geometrical reasons. Figure 42 shows the fow or 10 cm
spacing. The eddies inside the cylinder holes, and how the directionchanges and goes upstream inside the hole, can both clearly be seen.
In Figure 43 the area-averaged Nusselt numbers or the three cylinders
are displayed in the same way as in Figure 40. The Nusselt numbers
or the three gears are much the same in comparison with gears in the
horizontal position, and this results in more even hardness and lower
distortions. With the exception o the gear placed in the centre in the
10 cm case, which obtains the highest value, the more separated the
gears, the lower is the cooling, although the dierences are very small.
This is because when as the gears are separated urther apart, the
velocities between two adjacent gears decrease.
2.7. Distortion
Gas quenching is oten claimed to reduce the amount o distortion.
While theoretically valid, this is also true in most practical cases. During
quenching, oil passes through three di erent phases: a vapour phase;
a boiling phase; and a convection phase. All three phases have dier-
ent HTCs (see Figures 20 and 21). The quenched component is thereore
subjected to a dierent HTC at dierent positions on the component at
the same time. This leads to uneven quenching and inhomogeneous
phase transormation in the steel component, which causes uneven
stresses and distortions. In gas quenching, only the convection phase
is present and, consequently, more homogeneous phase transorma-
tions within the quenched component can be assumed, resulting in
more even stresses and less distortion. In practice, however, during
gas quenching the HTC also diers around a component depending onits geometry, its position in a load and the fow conditions dictated by
the perormance and geometry o the quenching chamber. But, com-
pared with oil quenching the di erences in HTC are much smaller when
quenching in gas.
In gas quenching one actor to consider is the distortions, such as ovali-
ty and fatness, that cannot be corrected. These distor tions are very crit-
ical and important to reduce. Distortion in diameters and, sometimes, in
conicity can be adjusted by sot machining beore hardening. However
it is then impor tant to minimise scatter.
Figure 42. Velocity plot or gears with 10 cm distance.
9800
8800
8600
0 32
Number of cylinder. 1 is the left and 3 is the right
A
verage
Nu
percylinder
5 cm10 cm15 cm20 cm
9600
9200
9000
9400
Figure 43. Area-averaged Nusselt number or all gears and all distances.
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31Low pressure carburising and high pressure gas quenching.
2.7.1. Gears
Automotive transmission synchronizer gears were gas quenched, ater
being vacuum carburised, with 20 bar helium [61]. The load consisted
o about 340 gears placed horizontally in nine layers. Compared with oil
quenching, use o high pressure gas quenching provided a signicant
reduction in gear distortion (see Figure 44).
The lower distortion values were consistent and repeatable so the sot
and hard machining tolerances could be decreased. Other transmission
parts such as sun gears, ring gears, pinions, and shats have also been
quenched in 20 bar helium with good results.
Extensive testing with gas- and oil-quenched gears has shown [62]
that gas quenching gives lower distortion. For example, a 30% reduc-tion in out-o-fatness was recorded. Since out-o-fatness is o crucial
importance to the tooth fank deviation, any improvement is particularly
important. Loading the gears in a vertical position also gave a reduction
o 10-20% in distortion compared to the horizontal position. It also gave
slighter higher hardness. This agrees well with the simulation discussed
in Section 2.6. As mentioned previously, the geometry o the gear also
has a noticeable infuence on distortion. With a small reinorcement o
the gear the distortion decreased by a urther 30%. According to Altena
[35] the reinorcement o such components has a large infuence, up to
50%, on the distortion and it must not be neglected.
There are other published results, which also show the comparisonbetween quenching in oil and gas where the gas gives lower distortion
[44, 48].
2.7.2. Rings
The geometric orms o gears and rings are relatively similar. While most
gears are made o carburising steel, most rings are made o ball bearing
steel. Rings o 100Cr6 steel were quenched in gas and two ast-quench-
ing oils [63] respectively (Figure 45). The gas was helium at 10 and
20 bar in a cold chamber. The distortion was determined by comparing
the diameter, ovality and conicity.
Both oils gave a higher distortion and scatter, compared with gas.Quenching at 20 bar gave less scatter, arising rom the act that the
10 bar quenched rings were not ully hardened because the cooling
capacity o the gas was too low.
In other published results, which also show the comparison between
quenching in oil and gas, the gas gives lower distortion [64, 65].
Figure 44. Less distortion is a major advantage o high pressure gas quenchingover oil quenching. These ovality or roundness data are or (a) 50 oil-quenched and (b) 50 gas- quenched synchronizer gears.
0,06
0,01
0
10 barHe
O
valityofOuterDiameter[mm] Average and
Standard Deviation0,05
0,03
0,02
0,04
20 barHe
Oil A Oil B
n = 127
12
6Oil A: Houghton
Quench A
10 bar HeCold Chamber
20 bar He
Oil B: Bellini Fn
}
Figure 45. Change in ovality or the ball bearing steel 100Cr6 with outer diameter70 mm, inner diameter 60 mm and height 15 mm, cooled in gas and oils.
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32 Low pressure carburising and high pressure gas quenching.
2.7.3. Axles
Gears and rings can be loaded both horizontally and vertically, but axles
are normally loaded vertically. Pinions in a load o 500 kg were carbu-
rised and quenched in both oil and gas with the same charge pattern.
Figure 46 reveals that the median straightness has decreased rom 100
to 50 m (4/1000 to 2/1000 in), a reduction o 50%.
It is clear that the scatter also is s trongly reduced, which reduces subse-
quent grinding or straightening.
In the same investigation long slender drive shats were oil- and gas-
quenched. The straightness decreased by 60% when quenching in gas.
A shorter and more stable axle decreased in straightness by only 15%
[48].
2.8. Interrupted gas quenching
Temperature gradients during quenching cause stresses and uneven
phase transormations and hence distortion and uneven hardness.
One way to control these deects is to lower temperature gradients by
decreasing the HTC. This can be done either by lowering the pressure
or by lowering the fow rate by reducing the an speed. It is crucial to
know when the interruption starts and by how much the HTC will be
decreased.
Quenching in a salt bath results in very similar cooling characteris-
tics and low distortion. But the possibility o doing the same with gas
quenching avoids the detrimental eect on the environment that salt
entails.
12
8
4
0621
Straightness 1/1000
in
Frec.
43
20
16
5
Gas carburizing & Oil quench
Vacuum Carburizing & Gas quench
Figure 46. Change in straightness or pinions o SAE 8260, quenched in oil and20 bar helium.
Temperature[C]
Time [s]
Fan stop Fan restart
conventional
dynamic
Figure 47. Eect o interrupted quenching, by turning o ventilator or 20 s.
left flank
right flank
Quenchingin oil
Conventionalgas quenching
Dynamic gas quenching(20 sec. fan turn off)
60
0
10
20
30
40
50
m
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33Low pressure carburising and high pressure gas quenching.
As a general rule the interruption in gas fow ought to start at or just
above the martensite temperature, which depends on the carbon
content o the steel. How much and or how long the HTC should be
decreased depends on the hardenability o the steel and the dimen-
sions o the component. The HTC or the urnace and the load congu-
ration must be both known or the calculation. The cooling curves are
calculated rom the HTC to determine the optimal curves that give the
correct hardness at a reduced cooling rate. Figure 47 shows the result
or a gas-quenched carburised SAE 5115 (16MnCr5) gear, compared with
oil quenching.
The quenching was interrupted at about 350C by turning o the an or
20 s and then turning it on again. The pressure remained unchanged.
The scatter o the helix slope distortion was strongly reduced. This, in
turn, reduced the subsequent grinding operation. This technique is com-mon industrial practice used to reduce distortion.
Salt bath quenching is typically used or austempering, but can be used
where low distortion is needed. However, salt baths create environmen-
tal problems.
2.9. Equipment
The gas quenching technique has seen rapid development through-
out the last 25 years. The rst vacuum urnaces were equipped with
nitrogen quenching at 1 2 bar. This combined a brazing process and
hardening o air hardening steel such as high alloy tool steel and highspeed steel [66]. Figure 48 shows how the gas quenching technique has
developed rom 1960 to the present. In about 1981/82 the rst single-
chamber vacuum urnaces with gas quenching at 5 6 bar were devel-
oped. The improved quenching power then allowed hardening o hot
working tool steels, small cold working steel components and the rough
hardening steel components in medium sizes.
The use o lighter gases, such as helium and hydrogen, together with
a gas pressure o 20 bar, gave a large increase in the HTC in the gas
quenching development sequence. A urther increase o the gas pres-
sure to 40 bar has been tested in a small cold chamber. This urther
improved quenching power, but in practice today the limit is 20 bar or
both technical and economical reasons. The 20 bar vacuum urnace has
an HTC o more than 1000 W/m2 C, which corresponds to normal oil
quenching or hot oil quenching. This gives sucient core strength and/
or hardness or carburising steel, through hardening steels in larger
dimensions, or lower alloyed steels. One goal is to develop the cold
chamber and its fow pattern urther to increase HTC without the need
to increase the pressure.
2.9.1. Single-chamber vacuum urnaces
In single-chamber urnaces heating and quenching both take place in
the same chamber. The design o a single-chamber vacuum urnace is
a compromise between the demands on the heating and quenching
systems. During quenching the heating elements and the wall insula-
tion material are cooled together with the load, oten to room tempera-
ture. The urnace can be built so that the fow o the gas can change
direction during the quenching period as well. The drawing to the let in
Figure 49 shows such a urnace where the load is quenched rom below
[67]. By changing the guiding plates the gas fow can be alternatedrom below and rom above. In the drawing to the right in Figure 49, the
guiding plates are adjusted so that the gas fow comes rom the let.
This mode is useul i the layers are tightly packed, making it dicult or
the gas to fow in a vertical direction.
Figure 48. Development o gas quenching technology
1 5 10 20 40
100 350 1000 1600
1960
1970
1980
1990
2000
Steel Grades3high-alloyed
tool steel3high performance
cutting steel3air hardening steel3gas quenching of
case hardening steel3soldering processes
(W/m2K)
+ hot working steel3quenched and tempered
steel (medium cross section)3cold working steel
+ case hardening steel3quenched and tempered
steel (larger cross section)3low alloyed steel
Yearpressure (bar)
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34 Low pressure carburising and high pressure gas quenching.
In single-chamber urnaces there is lot o space between the load and
the wall. As a result all the gas will not be orced to pass through the
load, instead some o the gas will pass outside load, see Figure 50 [62].
The distance between the load and the wall ought to be as small as
possible, but in prac tice the gap is usually 30 50 mm. When all other
conditions are the same it normally takes less time to ll a cold cham-
ber with gas because its volume is smaller. The lling time depends on
the buer chamber, pressure and volume, and the piping between the
buer tank and the quenching chamber, but 5 7 s is normal.
The same eect has been ound through simulation, see Figure 51 [57].
The simulation also showed that the heat transer coecients or the
outer plates on the side acing the urnace wall were 30% lower than
or the three plates in the centre.
The same simulation development work has also shown that the inlet
duct should have the same opening area as the load itsel or the
quenching chamber. I the inlet duct is too small the fow pattern will
be less avourable and give a less even heat transer coecient around
the load.
Figure 49. Single-chamber vacuum urnace: let, gas fow rom below; right, gasfow rom let [68].
Figure 50. Dierences in g