Forming & Fabricating Community of SME

http://sme.org/ffc/

The Forming & Fabricating Community focuses on key metal forming and
fabricating technologies. The community also engages members as technical
experts and manufacturing practitioners. They support the sharing of
manufacturing knowledge and solutions through professional networking.

Community Advisors: Brian Peshek, Dean Philips, Jon Brouwer,

Charles Caristan (your host today), Bob Iossi, Eric Kam, Viwek Vaidya
http://sme.org/ff-advisors/
Housekeeping Rules

1.5 hour webinar + 30 min. Q&A

All participants will be muted during the webinar

During the presentation, you can log along your

questions in the Q&A window of the WebEx screen.

Q&A session immediately following the presentation: all

participants will be unmuted

The whole presentation is recorded and a web link to

the recording will be emailed by SME to all attendees.
 Meet the Presenters:
Controlled Thermal Processing, Inc.
Frederick J. (Rick) Diekman
President and Founder
www.metal-wear.com

Rozalia Papp
Business Development Specialist / Heat Treatment
rozalia.papp@airliquide.com
www.us.airliquide.com

Professor Susil K Putatunda

Department of Chemical Engineering and Materials Science and
Engineering,
 Deep Cryogenic Treating (DCT) of Metals,
an Emerging Technology

Frederick J. Diekman Rozalia Papp Susil K. Putatunda

President Sr. Business Development Professor, Department of Chemical
Specialist (Heat Treat & SPAL) Engineering and Materials Science
and Engineering,

Controlled
Thermal Processing, Inc.
 Presentation Objectives

Define Deep Cryogenic Treating (DCT)

Metallurgical timeline and development
Discuss the Process
Show Some of the Research
Show Some of the Possible Economic Impacts of the
Process
The future of DCT science
 Deep Cryogenic Treating (DCT) is:

The Creation of Structural and Mechanical Changes

in Materials By Exposing Them to Cryogenic
Temperatures.
The Cryogenic Society of America

Considers Cryogenic Temperatures to be

Temperatures Below 1200K
(-2440F, -1530C)

(00K= Absolute Zero)

 Why is it not more well known?

Man has been changing materials with heat for many

thousand years.
Man has been using heat to treat metals for 7500
years.
Man has had cryogenic temperatures for only ~100
years.
 Why DCT Not Well Known?

This image shows average temperatures for the period from 1961 to 1990.
 Phase Diagrams Rarely Show Phases Below
Zero Degrees Celsius

0C

?
-273C

http://wikis.lib.ncsu.edu/images/9/95/CH434_binardsc.gif
Fe-C Phase Diagram
 The Effect Of Cryogenic Processing On The
Mechanical Properties Of
Austempered Ductile Cast Iron (ADI)

Fig 1: Microstructures of samples austempered at 550550F Fig.2: Microstructure of the cryogenically treated
-Bainitic ferrite and austenite with graphite nodules. sample showing the presence of carbide.
-very fine scale ferrite and austenite
The Effect Of Cryogenic Processing On The
Mechanical Properties Of
Austempered Ductile Cast Iron (ADI)
 Air Separation Plants

The gases from the air, nitrogen (N2), oxygen (O2) and argon (Ar) are
produced from the fractional distillation of air.

- 302F

- 297F

- 320F
 Wkipedia Says

A cryogenic treatment is the process of treating workpieces

to cryogenic temperatures (i.e. below 190 C (310 F)) to
remove residual stresses and improve wear resistance on steels.

The process has a wide range of applications from industrial tooling

to improvement of musical signal transmission. Some of the benefits
of cryogenic treatment include longer part life, less failure due to
cracking, improved thermal properties, better electrical properties
including less electrical resistance, reduced coefficient of friction,
less creep and walk, improved flatness, and easier machining.
 Kinetics of Cryogenic Treatment
(ASM Handbook Volume 4 Heat Treating, 1991 and last revised in 2001)

There are several theories concerning reasons for the effects of cryogenic
treatment. One theory involves the more nearly complete transformation of retained
austenite into martensite. This theory has been verified by x-ray diffraction
measurements. Another theory is based on the strengthening of the material
brought about by the precipitation of submicroscopic carbides as a result of the
cryogenic treatment. Allied with this is the reduction in internal stresses in the
martensite that happens when the submicroscopic carbide precipitation occurs. A
reduiction in microcracking tendencies resulting from reduced internal stresses is
also suggested as a reason for improved properties.
The absence of a clear-cut understanding of the mechanism(s) by which cryogenic
treatment improves performance has hampered its widespread acceptance by
metallurgists. Nonetheless, it is important to review the studies done to determine
the effects of cryogenic treatment on the performance of steel in a variety of
applications.
 What Cryogenic Metallurgy Does

Relieves Residual Stresses (All Metals)

Refines the Crystal Structure (All Metals) (Unproven Theory)
Modifies Point Defects in the Crystal Structure (All Metals)
Precipitates Fine Eta Carbides (Steels With Carbide
Forming Elements Only)
Converts Retained Austenite to Martensite (Hardened
Steels Only)
Refines the Crystal Structure (All Metals)
(Unproven Theory)
Basic Metallurgy Teaches

For all temperatures above 0oK, there is

a thermodynamically stable
concentration of vacancies and
interstitial atoms. Introducing a point
defect into a crystal increases its
internal energy vis-a-vis a perfect
crystal. (Italics added).
Russell, Alan M., and Lee, KOK Loong, STRUCTURE-PROPERTY
RELATIONS IN NONFERROUS METALS John Wiley and Sons 2005
Page 18
 Results of Deep Cryogenic Treating

Increased abrasion and wear resistance

Increased fatigue life
Increased ductility
Reduced residual stresses
Mild increase in tensile strength
A change in vibration characteristics
 Typical Cycle Steps in Cryogenic
Metallurgy
Temper Hold

p
pU

Tem
m
Ra

per
er
mp

Ram
Te
Ra

pD
m

Room Temp
pD

ow n
Up
ow

Time
mp
n

Ra

Hold or Soak Temperature

 Cryo - Processors

MEI machine uses spraybar 300 Below uses electric refrigeration

technology compressors to -100F, then spraybars
Insulation is a mineral wool. Insulation is polyurethane foam
Cryo - Processors

Vacuum Insulated Machines by Applied Cryogenics

Heat Exchanger Technology
Capable of -320F to +320F

LN2 Consumption at -300F

7 liters/hour
 Insulation
Price versus Performance

R5 or R1500, its your (extreme) choice

Overall Efficiency, four basic factors:

1. Thermal conductivity
2. Vacuum level ($$$)
3. Cost of labor ($$) and materials ($)

Source:http://lartpc-docdb.fnal.gov/0002/000217/001/Cryogenic_Insulation_Technology.pdf
Cryogenic Thermal Insulation Systems, James E. Fesmire, Stan D. Augustynowicz
 Representative k Values (mW/mK)
MATERIAL High Medium Vacuum No Vacuum
Vacuum
High Vacuum .5 to 5

Nitrogen gas at 200 18.7

Fiberglass, 16 kg/m 2 14 22

PU foam, 32 kg/m 21

Cellular glass foam, 128 kg/m 33

Perlite powder, 128 kg/m 1 16 32

Aerogel beads, 80 kg/m 1.1 5.4 11

Aerogel composite blanket, 125 kg/m 0.6 3.4 12

MLI, foil and paper, 60 layers, 79 kg/m 0.09 10 24

! LCI, 30 layers, 78 kg/m3 0.09 1.6 14

Source: http://lartpc-docdb.fnal.gov/0002/000217/001/Cryogenic_Insulation_Technology.pdf
 Cooling Cost Factors in Deep Cryogenic
Processing

The Major Cost is the Liquid Nitrogen

1. Cooling the Load .25L/pound of steel

2. Cooling the inside of the machine .25L/pound of steel
3. Heat infiltrating through the insulation insulation and construction
dependent
4. Heat created by air circulation 1.5 L/hour/horsepower
 Performance Experiments
Effects of Cryogenically Treated Steel
(Source: ASM Handbook, Vol. 4, Heat Treating, ASM International, 1991, p 205
Heat Treating Progress: Volume 2, Number 49, December 14, 2007)

Theories about the reasons for the effects of

cryogenic treatment include a more nearly
complete transformation of retained austenite
into martensite; precipitation of submicroscopic
carbides; and a reduction in internal stresses
in martensite that occurs when the
submicroscopic carbide precipitation occurs. A
reduction in microcracking tendencies resulting
from reduced internal stresses is suggested as
a reason for improved properties.
Comparison of wear-resistance ratios for five high-
carbon steels soaked at -84C and -190C
(-120 and -310F). Soaking temperatures below -84C
does not significantly change the
hardness of the material.
Army Aviation & Missile Command Research
With Illinois Institute of Technology Research
Institute

Study of wear resistance under

Hertzian contact stresses of 9310
steel.
50% extra pitting resistance
5% more load carrying capacity
400F to 600F higher tempering
temperature
Wind Turbine Gear Boxes

Failure is biggest
maintenance cost.

5 year predicted life

Many fail earlier

Replacement cost of
$500,000

Current installation rate is

approximately 2900 turbines
/year.
University of Trento, Trento, Italy/GKN Corp.
Effect of Deep Cryogenic Treatment of the Mechanical Properties of
Tool Steels
(A. Molinari, M. Pellizzari, S. Gialanella, et al. 2001 Journal of Materials Processing
Technology.)

Studied M2 & H13.

Improved hardness homogeneity.
Led to 50% cost reduction.
Increased toughness on H13.
No significant changes to microstructure except reduction in retained
austenite.
Need to study the sub-microstructure for mechanism.
Cryogenic Treatment of M1, EN19 and H13 Tool Steels to
Improve Wear Resistance
(IE(I) Journal-MM, Vol 86, October 2005 pages 64, 65, 66; P Sekhar Babu,
Member, P Rajendran, Non-member, Dr K N Rao, Fellow)

Cryogenic treatment is said to improve wear resistance of tool and die steels and
implemented at many places for that purpose. Although it has been confirmed that
cryogenic treatment improves wear resistance and tool life, the process has not
been standardized with inconsistent results varying from researcher to researcher.
In this work the authors have studied the improvement in wear resistance of M1,
EN19 and H13 tool steels after cryogenic treatment. The materials were tested for
improvement in abrasive wear resistance after cryogenic treatment at different
temperatures below 0C.
All the samples were first heat treated as per standard norms and re tempered
after cryogenic treatment. The samples were treated at 0C, -20C, - 40C, -80
C and -190C.
It was observed that the wear resistance improved for all the samples from
315% to 382% depending on the material.
Tool Steel Tooling Accounts for up to 20% of
the cost of production of things we buy.
Annual Market for tool steels is 32,000,000 Kg

Drills Molds
Milling Cutters Extruding Dies
Die Casting Dies Forming Rolls
Stamping Dies Broaches
Knives
Forging Dies
 Brakes
Lab Tests indicate up to 7 times life.

Specified by the US Postal Service after extensive testing.

California County Sheriff fleet of 450 Ford Crown Victorias saving over
$650,000/year based on a one year practical test.

United States Commercial & Government Fleet --31,600,000 Vehicles

Proven environmental benefits

 Copper Welding Electrodes Last Longer

(Sub-zero Treatment of Steels Technology/Processes/Equipment, Linde AG | Linde

Divison/82049 Hollriegelskreuth/Germany).

Cryogenic treatment of copper welding

resistance electrodes increases their life by
a factor 2 to 9.

These electrodes are used by the hundreds

of thousands in automotive and appliance
industries.
 CARBIDE

Carbide cutting tools have been shown to last up

to 6 times as long.
 Cryogenic Treatment of Cutting Tools
(Andrew Yong A thesis submitted in 2006 for the degree of Doctor of Philosophy,
Department of Mechanical Engineering National University of Singapore)

Cryogenic treatment significantly alters the microstructure of tungsten

carbide.

Cryogenic treatment increases the hardness of the tungsten carbide tools.

Cryogenically treated tungsten carbide tools in continuous cutting

operations show a marked decrease in tool wear during the initial duration of
cutting as compared to untreated tools.

Cryogenically treated tungsten carbide tools perform well in intermittent

cutting operations, such as milling operations.
 Other Areas of Use

Electronics
Stereo Equipment
Chip Manufacturing
Plastics
Stabilization of Metals
Springs
Sports Equipment
 The Cryogenic Society of America

CSA is a non-profit technical society serving all those

interested in any phase of cryogenics, the art and
science of achieving extremely low temperatures
almost absolute zero.
www.cryogenicsociety.org
 Cryogenic Research Database

Joint effort between ASM & CSA

Papers & Articles reviewed by a committee of experts
Complete papers published where possible
Available to the public

www.cryogenictreatmentdatabase.org
 ASM Cryogenic Processing Sub
Committee

Educate Markets
Encourage and Coordinate Research
Discourage Frivolous Claims
Create a Research Database
Review Cryogenic Processing in ASM Publications
Provide Peer Review of Research
 To Conclude

DCT can further change structure and properties of metals.

DCT can improve mechanical properties and reduce production
costs.
Research & practical testing have proven the process in many cases.
Next steps in the DCT science shall include but not be limited to:
Understand phase changes down to 0K (absolute Zero)
Determine the best processing parameters for each material )metallic and
non-metallic)
Develop a specification driven, industry approved process for each
material and each application
Include the new scientific advancement in the teaching system
THANK YOU FOR YOUR ATTENTION!

Questions?