HEAT TREATMENTS

Mechanism and Applicability of Heat

Treating at Cryogenic Temperatures
By PETE PAULIN
300'Below Inc.
Decatur, IL

Durability is the most important

criterion used to define the quality of
a tool steel. Cryogenic treatment and
tempering of metals has been ac
knowledged for almost thirty years
as an effective method for increasing
durability, or wear life and de
creasing residual stress in tool steels.
Deep cryogenics (below -300F) is cre
ating many new applications in sci
ence. High temperature superconduc
tors, the super-conducting super col
lider, cryo-biology, magneto-hydrodyn
amic drive systems for ships, and low
temperature physics have all devel
oped recently.
The deep cryogenic treatment and
tempering process for metals is eco
nomical. It is a one time permanent
treatment, affecting the entire part,
not just the surface. The treatment
may be applied to new or used tools,
sharp or dull, and resharping will
not destroy the imparted properties.
Benefits achieved from subjecting
tools to this treatment include: in
creases in tensile strength, tough
ness, and stability through the re
lease of internal stresses. The excep
tional increase in wear resistivity,
generally exceeding 200% is the great
est benefit.
Steel surfaces requiring wear resis
tance, such as in the cases of drill
bits, end mills, surgical scissors, bear
ings, racing engines, slicers and gran
ulator knives, all benefit from the in
expensive treatment. New applica
tions are being discovered continu
ously.
BASIS FOR IMPROVED PROPERTIES

A research metallurgist at the Na

tional Bureau of Standards in Boul
der Colorado, states, When carbon
precipitates form, the internal stress
in the martensite is reduced, which
minimizes the susceptibility to microcracking. The wide distribution of
very hard, fine carbides from deep
cryogenic treatment, also increases
wear resistance. The study con
cludes: ...fine carbon carbides and
resultant tight lattice structures are
24

Deep cryogenic treatment and tempering machine with Squid nitrogen cylinder is newly
designed for highly efficient thermal transfer in processing.

precipitated from cryogenic treat

ment. These particles are responsible
for the exceptional wear characteris
tics imparted by the process, due to a
denser molecular structure and re
sulting larger surface area of contact,
reducing friction, heat and wear.
There have been skeptics of the
cryogenic process for Bome time, be
cause it imparts no apparent visible
changes to the metal. Since proper
heat treating can transform 85% of
the retained austenite to martensite
and the deep cryogenic process only
transforms an additional 8 to 15%,
the deep cryogenic treatment has
been considered an inefficient pro
cess. While these percentages are cor
rect, the conclusion drawn from them
is inaccurate. In addition to the trans
formation to martensite, the sub
jected metals also develop a more
uniform, refined microstructure with
greater density. Although known to
exist, this type of microstructure was
only recently quantified scientifically.
Particles known as binders are
coupled with the precipitation of the
additional microfine carbide fillers.
The fillers take up the remaining
space in the micro-voids, resulting in
a much denser, coherent structure of
the tool steel. These particles are

identified and counted in the above

study cited, using a scanning electron
microscope with field particle quanti
fication (an automatic particle count
er). It is now believed that these par
ticles are largely responsible for the
great gains in wear resistivity. The
permanent irreversible molecular
change created is uniform throughout
the tool, unlike coatings, and will
last the life of the tool, regardless of
any subsequent finishing operations
or regrinds.
Fig. 1 shows two photomicrographs
(lOOOx) representative of samples from
the same S-7 bar stock. The first is
untreated S-7. The second was deep
cryogenically treated. Both samples
initially were conventionally heat
treated; that is, austenitized and oil
quenched. The deep cryogenic treat
ment consisted of varying ramp with
pause at -150F for 1 hr, at -270F for
2 hr and soaking for 8 hr at -310F,
followed by tempering at 300F for 1
hr, AC to room temperature and tem
pering at 225F, AC. In this micro
stru ctu re, note the con sid era b ly
greater number of fine particles cou
pled with fine carbides in comparison
with the untreated sample. The martensitic transformation is readily
apparent.
Industrial Heating August. 1992

Fig. 1 Photomicrographs (1000X) of non-cryogenically treated and tempered S-7 steel (left) and deep cryogenically treated S-7 steel (right).
Superior properties developed by the latter treatment are attributed to increased transformation of austenite to martensite and a more uniform,
refined microstructure with greater density (precipitation of additional microfine carbides).

FIELD TESTING PROVES DEEP CRYOGENIC

TREATMENT POTENTIAL

The cryogenic cycle is an extension

of standard heat-treatment, and cre
ates many outstanding increases in
durability. Some examples are as
follows.
A major aircraft manufacturer test
ing deep cryogenic treatment found
that with only six different tools
treated, the savings in tool purchases
could exceed $5 million.
An Arizona State study conducted
by Laurel Hunt, used deep treated
C-2 deburring tools on INCONEL al
loy 718, achieving a 400% improve
ment based on weight, after five cuts
of .003 in. (.007 cm) on this alloy.
This deep cryogenic treatment of an
8% cobalt end mill has made dramat
ic improvements in two important
ways. The number of milling cuts
was increased from three before deep
cryogenic processing, to 78 cuts after
processing (26 times the wear life).
Resharpening the end mills after
deep cryogenic treatment required
only 1/3 the amount of stock removal
to restore the tool geometry.
Rockwell, a major aircraft manu
facturer, using C-2 carbide inserts to
mill epoxy graphite, doubles their
output after deep cryogenic treatment
of the inserts. In a second test, a
400% improvement was achieved upon
milling 4340 stainless steel with cryo
genic treated tool.
Other applications include: Leading
national stock car drivers who pre
viously raced only 4-8 races between
equipment teardowns, drove in 40+
races before teardown after cryogeni
cally treating block, crank, cam, pis
tons and heads.
Fig. 2 Standard heat treating, austenitizing,
oil quenching and tempering, compared to
cycles with added cryogenic ( - 7 CPC) and
tempering cycles. (Source: Jassy
Polytechnique InstitutelAlexandru).
Industrial Heating August, 1992

LAB RESULTS CONFIRM HELD TESTS

Shallow Cryogenic Cycles

The latest research data on cryo

genic and tempering cycle confirms
the long standing theory that cryo
genic treatment significantly enhanc
es cutting tool life. Dr. loan Alexan
dra and Dr. Constantin Picos of the
Polytechnic Institute of Jassy, Roma
nia, utilized the latest scientific equip
ment available, a JEOL IXA-5A Elec
tron Probe, a DRON-1 X-ray Diffracto
meter, a Quantimet 720 Quantitative
Microscope, and a Chevenard Differ
ential Dilatometer to supply the fol
lowing results from the extensive
study.
The study involved 7 samples (AN, Fig. 2) each subjected to a differ
ent heat/cool cycle as noted. Each
sample was the equivalent of M2
steel. The carbide particles were phys
ically counted, both before and after
the deep cryogenic treatment. The

team then measured the samples

with the equipment above, and with
standard metallurgical evaluative
testing. The results confirm with tan
gible evidence the carbon participa
tion in cryogenic processing.
The results of the testing, Fig. 3,
comparing standard heat treating to
heat treating with the addition of a
shallow cryogenic soak (-7 0 C ) are
summarized as follows: austenite de
creased from 42.6% to 0.9%; martens
ite increased from 66% to 81.7%; car
bides increased from 6.9% to 17.4%;
mean number of carbides counted @
lmm sq increased from 31,358.17 to
83,529.73; number of carbides less
than 1 |un increased from 23,410.24
to 69,646.09; Rockwell increased from
60.10 to 66.10; tensile strength in
creased from 86.0 to 244.46; bending
tensile rate increased from 0.65 to
1.85; KCU (resiliency) increased from
.0668 to 1.18; HRC after 20 minutes
hold at 675C: 56.88 to 62.25.

t00
1200
1000

S'

00

f.
CJ 600
=
o
SL 400
E

200
0
-200

A: Hart Mat aaly ( im M

fc Hart M ( M feMla Mapar fC M M n q k | .
C :H M M M M k t a | ) p ie c | d ( M l
M M i f e M M i B m M k d m ltM p .

H: HMt M rife f pa A m it r t w nynM lt cjet a iM .

I t HMt kaat ( M taapai A m M t a v
cyda Km
tu * .
It HmI Mat Him
uyapatc tpda Am
l i Mp ir , m t M li cycta M i

U n M n aptos w m M m k m M m H al M c k M l It * s q k A n t e * m c a a p h tf t t . % C; .3 Mk
-M S ; 4.1Cr, 5 .1 %
.m i - , t r w * . t m pH i v a n d H aah naM il| it n h r i teat k a a M @ 12MC A m - i ------ it
F av i< k a piacM v a n A m Mbfadad ta M o p t M l c q d a @ - 7 K a n M q la i l i B p n r t M afcr

M U*

25

Fig. 3 Cryogenic and tempering cycle

doubles durability, decreasing austenite while
doubling microfine carbides.

0.00-^
Sample 10

Durability in terms of length of

cutting time increased from 20 min
utes to 45 minutes with a shallow
cryogenic cycle.
Fig. 2 illustrates the seven sepa
rate heat/cool cycles used to temper
the lathe cutting tools. The tools
were then used to cut 0.5% structural
carbon steel (see Table I). Durability
was established by measuring the
radical component of wear.

Table I Parameters for Lathe Cutting

Tools in Wear Resistant Test
Intensive Speed @33.6m/min.
Depth 5mm; Feed - 0.62mm per rev.
Relief angle - 8 Deg.;
hake angle - 5 Deg.: Plan - 45 Deg.

1.2 to 2 times depending on the al

loy. This is consistent with the Jassy
findings. However, the deep cryogenic
treatment in liquid nitrogen at 317F
soak improved wear resistance by
even greater ratios running from 2 to
6.6 times.
PROCESS ADVANCEMENT THROUGH NEW
EQUIPMENT AND COMPUTERIZATION

The deep cryogenic process has had

an Achilles heel. It has been incon
sistent. In the past, improvements to
cutting tools would vary from little
improvement to over 1000% increased
in useful life. The key to effective
improvements consistently is proper
processing. If a cutting tool is drop
ped in liquid nitrogen, without tem
perature control, the tool could shat
ter. Metals require specific cooling
rates; temperature changes must be
controlled exactly to obtain the opti-

mal cooling curve. The computer pro

cessor solves the problem, since it al
lows exact duplication of the optimal
cooling curve, repeatedly.
The older cryogenic tanks did not
have adequate controls. A relatively
new cryogenic system (model 2953,
lead illustration) achieves consistent
results.
The new cryogenic machines oper
ate with controlled dry thermal treat
ment. Controlled simply means
that the process is performed accord
ing to a precise prescribed time table.
A process controller (Yokogawa UP
25) operates the descent, soak and
ascent modes (see Fig. 5). Generally,
the material is cooled slowly to -317F,
held for 20-60 hr then raised to
+300F, and slowly returned to room
temperature. The machine switches
over to the electrical resistance mode
for the tem pering operation. The
dry process prevents the metals
from being subjected to liquid nitrogen,
and eliminates the placing of an item
in the freezer and pushing a button.
A breakthrough in system insula
tion has been achieved as a result of
the space program. The system is de
signed to accomplish thermal trans
fer, and the more efficient the better.
It is essential to transfer therms
from the liquid nitrogen to the metal
parts being treated, without losing
the therms to the outside. Thus, the
vacuum chamber is designed for threelevel insulation. Walls of the cham
ber are 3 in. stainless steel. On the
inside wall are 125 wrapped layers of
aluminized polyester film. Inside the
chamber itself is 2 in. polyisocyan ur
ate high density foam which is coat-

Deep Cryogenic Cycle vs Shallow

Cryogenic Cycle

Separate laboratory testing has

been accomplished by Dr. Randall F.
Barron at Louisiana Tech University.
The results by Dr. Barron more than
substantiated the Jassy study. In one
series of tests compared were five
common steel alloys (see Fig. 4).
First they were wear tested as pro
cured, then as chilled to -120F and fi
nally tested after treating at -317F.
In all cases the cold treatment im
proved wear resistance; the colder
the treatment, the more favorable
the results. The -120F (dry ice) treat
ment improved ratios ranging from

Fig. 4

Wear improvement due to shallow

cryogenic ( - 12CPF) treatment vs.
improvements due to deep cryogenic
(-317 F) treatment

26

52100

Industrial Heating August, 1992

ed with Ceramaseal amorphous vapor

barrier 'comprised of microspherical
ceramic globes. A 93% increase in
processing ability is accomplished
with the space shuttle insulation
in the vacuum walls, providing con
siderable savings in processing and
making the treatment economical for
a variety of items in addition to
tooling.
ADVANTAGES FOR HEAT TREATERS AND
IN INDUSTRIAL PRACTICE

Potentially every tool heat treated

is a candidate for the additional ser
vice of cryogenic treatment and tem
pering. It is economical to provide
the additional improvement of any
perishable item.
There are more than a handful of
large tooling manufacturers utilizing
the process today for manufacturing
a premium line of cutting tools.
More than 200 heat treaters pro
vide cold cryogenic services. Howev
er, 95% of these are only utilizing
-120F (dry ice) treatments. Only a
handful of companies provide cryo
genic treatment below -300F, which
results in much more impressive re
sults and accompanying benefits.
A small Massachusetts firm has
been processing items for 12 years.
The strings on a piano which was
previously tuned every six months
were treated. The piano has not been
tuned for five years. Musicians who
play guitar and violin firmly believe
that the strings are brighter in sound.
Oscilloscopes confirm a shift after
treatment.
A firm in Michigan has been pro
cessing with the method for 27 years.
They also specialize in stress relief of
the plastic material used in contact
lenses, among other items. A cryo
genic treating company in Phoenix
treats many aerospace parts. Another
processor in Ohio treats many car
bide tools. The treatment is gaining
acceptance nationwide. The process is
used in Europe and Australia under
the trade name CryoTough, a BOC
treatment.

Fig. 5

Instrumentation for control of the cryogenic treatment and tempering cycle.

When a specific tool receives wear

extension, there is a 95% certainty
similar tools will respond consistently
in the future to the same exact cycle.
Among the properties which define
the cutting qualities of a tool steel,

durability is the highest importance.

Results in this regard are decisive in
establishing the benefits of cryogenic
treatment and also answer the decades
long question, what happens when
parts are tested in this manner?

CONCLUSION

While not a Magic-Wand which

will extend the life of everything,
over 100 tools such as reamers, taps,
dies, broaches, drills, endmills, slicers
and cutting knives do respond consis
tently to this process. Cryogenic ser
vice can create a premium more
profitable tool line for a manufactur
er. It is also saving considerable tool
expense for the end user. The process
is effective throughout the tool un
like a coating, so tools can be resharp
ened and retain the benefits of the
treatment until completely worn out.
The process also works with TiN
coatings.
Industrial Heating August. 1992

Tell us about your requirements, we'll

suggest practical and economical solutions.
For objective and helpful atmosphere
control recommendations, not sales
talk...it makes no difference if you're a
do-it-yourselfer or prefer engineered
c o n tro l system s. W e'll su p p ly the
know-how and atm osphere furnace
controls.

Choose any of the following approaches:

Control carbon, temperature, time
Control carbon only
Control endothermic generators
Computer monitoring and data
acquisition
Write or call: (216)349-7220

Q
Division of Zircoa, Inc., 31711 Solon Rd., Solon, OH 44139 FAX (216) 248-8864

Circle #124
27