Forming & Fabricating Community of SMEhttp://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 Vaidyahttp://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:

Professor Susil K Putatunda

Department of Chemical Engineering and Materials Science and

Engineering,

Rozalia Papp

Business Development Specialist / Heat Treatment

rozalia.papp@airliquide.com

www.us.airliquide.com

Frederick J. (Rick) Diekman

President and Founder www.metal-wear.com

Controlled Thermal Processing, Inc.

Deep Cryogenic Treating (DCT) of Metals,

an Emerging Technology

Rozalia Papp

Sr. Business Development Specialist (Heat Treat & SPAL)

Frederick J. Diekman

President

Susil K. Putatunda

Professor, Department of Chemical 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

0ºC

http://wikis.lib.ncsu.edu/images/9/95/CH434_binardsc.gif

-273ºC?

Fe-C Phase Diagram

Fig 1: Microstructures of samples Fig 1: Microstructures of samples austemperedaustempered at 550at 550°°FF

--BainiticBainitic ferrite and austenite with graphite nodules.ferrite and austenite with graphite nodules.

--very fine scale ferrite and austenitevery fine scale ferrite and austenite

Fig.2: Microstructure of the cryogenically treated Fig.2: Microstructure of the cryogenically treated sample showing the presence of carbide.sample showing the presence of carbide.

The Effect Of Cryogenic Processing On The Mechanical Properties Of

Austempered Ductile Cast Iron (ADI)

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.

- 320ºF

- 297ºF

- 302ºF

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

Hold or Soak

Room Temp

Ram

p D

ow

n

Ram

p U

pTem

per R

amp

Up Temper Hold

Tem

per R

am

p D

ow

n

Time

Temperature

MEI machine uses spraybartechnology

Insulation is a mineral wool.

300 Below uses electric refrigeration compressors to -100ºF, then spraybars

Insulation is polyurethane foam

Cryo - Processors

Vacuum Insulated Machines by Applied Cryogenics Heat Exchanger TechnologyCapable of -320ºF to +320ºF

LN2 Consumption at -300ºF 7 liters/hour

Cryo - Processors

InsulationPrice versus Performance

• R5 or R1500, its your (extreme) choice• Overall Efficiency, four basic factors:

1. Thermal conductivity2. Vacuum level ($$$)3. Cost of labor ($$) and materials ($)

Source:http://lartpc-docdb.fnal.gov/0002/000217/001/Cryogenic_Insulation_Technology.pdfCryogenic Thermal Insulation Systems, James E. Fesmire, Stan D. Augustynowicz

MATERIAL High Vacuum

Medium Vacuum No 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

Representative k Values (mW/mK)

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 steel2. Cooling the inside of the machine .25L/pound of steel3. Heat infiltrating through the insulation insulation and construction

dependent4. Heat created by air circulation 1.5 L/hour/horsepower

Performance Experiments

Effects of Cryogenically Treated Steel

Comparison of wear-resistance ratios for five high-carbon steels soaked at -84°C and -190°C

(-120 and -310°F). Soaking temperatures below -84°C does not significantly change the

hardness of the material.

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.

(Source: ASM Handbook, Vol. 4, Heat Treating, ASM International, 1991, p 205

Heat Treating Progress: Volume 2, Number 49, December 14, 2007)

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 0°C.

All the samples were first heat treated as per standard norms and re tempered after cryogenic treatment. The samples were treated at 0°C, -20°C, - 40°C, -80°C and -190°C.

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• Milling Cutters• Die Casting Dies• Stamping Dies• Knives• Forging Dies

• Molds• Extruding Dies• Forming Rolls• Broaches

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 Victoria’s 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 0ºK (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?