BEHAVIOUR OF

MATERIALS SUBJECT
TO DEEP SUBZERO
TEMPERATURES –
PRELIMINARY FINDINGS
AND IDEAS
 GENESIS
• Sub Zero Processing for Tool
Steels up to – 40oC
• Improve Dimensional Stability
• Eliminate Retained Austenite
 NEED FOR SUB ZERO
PROCESSING
• Instabilities Developed During
Manufacturing Process
• Unstable / Quasi Stable / Meta
Stable Phases Developed during
Hardening
• Eliminate Hardness Drop during
Tempering
 MATERIAL
CHARACTERISTICS
• ALL ALLOY AND TOOL STEELS
• PH HARDENING STEELS
• SUPERALLOYS
• COPPER & COPPER ALLOYS
• ALUMINIUM AND ALUMINIUM ALLOYS
• PLASTICS AND POLYMERS
• PRECIOUS METALS
• CARBIDES AND SINTERED MATERIALS
 DEEP SUB ZERO
TECHNOLOGY
• Operation at low temperatures (-
195OC)
• Long Residence times for
homogenization
• Slow cooling and heating rates
 THEORY
• Deep Sub Zero Processing based on Third
Law of Thermodynamics
• Stress Relieving at Atomic Level
• Elimination of Point & Line Defects
• Low Temperature Provides adequate G
for transformation
BENEFITS IN TOOL
AND ALLOY STEELS
MANUFACTURING PROCESS
FOR TOOL STEELS
• Rough Machining
• Stress Relieving
• Finish Machining
• Hardening
• Deep Sub Zero Processing
• EDM, Grinding & Polishing
HARDENING & TEMPERING
 THEORY
• Annealed steel C & Alloy elements as
Carbides
• Ni & Co in solid solution
• Heat to dissolve Carbides
• Avoid grain coarsening & embrittlement
 THEORY
• Ferrite -- Austenite
• Lattice parameters change
• Carbon & alloy elements occupy lattice
points
• Austenite -- Martensite
• No time for C to reposition
• High microstress -- high hardness
 RETAINED AUSTENITE
• Incomplete Austenite -- Martensite
Transformation
• Increase with
– Increased Alloy content
– Higher Hardening Temperature
– Longer Soaking Times
 TEMPERING
• Reheating to relieve inherent stresses
• Prevent Cracking
• Transform Retained Austenite -- Martensite
• Immediately after hardening
• Microstructure consists of
– Tempered Martensite / Martensite
– Carbides / Retained Austenite
• Tempering Dependent on Tool Steel
 PRACTICE
• Stress Relieving
• Hardening / Quenching
• Tempering
 STRESS RELIEVING
• After Rough Machining
• Y. S. low so unable to resists stresses
• Stress Relieved, lower distortion
• Right Sequence
– Rough Machining
– Stress Relieving
– Finish Machining
 HARDENING
• Vacuum / Salt Bath / Muffle Furnace /
Fluidized Bed
• Protection against Decarburisation
• 1-2 Preheat steps
• Holding for temperature equalization
 QUENCHING
• Oil
• Salt Bath
• Air
• Cooling rate depending on Hardenability
• Avoid Bainite Formation
 TEMPERING
• Immediately after job cooled to 50 0C
• Temperature depends on
– Hardness required
– Toughness required
– Dimensional stability
DEEP SUB ZERO
PROCESSING
 WHY DEEP SUB ZERO
PROCESSING
• Minimize Retained Austenite
• Improves Toughness with no change in
Tensile Properties
• Hardness Profile Correction
 R. A. CONVERSION
• Conversion of Retained Austenite in situ to
Temper Martensite.
• Stress relieving provides driving force for
transformation.
• Hardness Correction across cross section
 THEORY
• Athermal Conversion of Austenite to Martensite
• Volume Change accompanies Phase
Transformation
• Structural Integrity of Steel prevents complete
transformation
• Tempering precipitates Carbides leading to
Stress Relief & further Transformation
• Prolonged Tempering leads to complete
relieving of stresses but drop in hardness
 CARBIDE PRECIPITATION
• Eta Carbides precipitated
• Sub micron size particles characterized by
shape
• “Concrete Effect”
• Toughness Increases, Catastrophic
Shattering decreases significantly
 THEORY
• Alloy Element Solid Solubility decreases
with decreasing temperature
• No preferred Precipitation Site
• Precipitation over entire matrix
• Very high Specific Surface
• Approx 10% of Total Carbide Volume
 THEORY –
“CONCRETE EFFECT”
• Eta Carbide Particles act as Binder
between Matrix & Primary Carbides
• Establish Coherency in Steel
Microstructure
• Reduce Stress Concentration around
Primary Carbides
• Minimise Chipping Tendency by promoting
Abrasive wear
 THEORY –
CATASTROPHIC SHATTERING
• Minimise Stress Concentration leading to
delay in Crack Initiation
• Secondary Carbide Particles provide
barrier for Crack Propagation
• Crack Growth rate decreases leading to
minimisation of Catastrophic shattering
PH HARDENING
STEELS
MANUFACTURING PROCESS
FOR PH HARDENING STEELS
• Rough Machining
• Stress Relieving
• Finish Machining
• Solution annealing
• Deep Sub Zero Processing
• Finish Tempering
• EDM, Grinding & Polishing
 THEORY
• Steels hardened by precipitation of
dispersed phase due to instability in parent
phase
• Solutionising for homogenisation of
phases
• Deep Sub zero processing for uniform
precipitation of nuclei
• Finish tempering for growth of precipitate
phase
 THEORY
• Lower tempering temperatures possible
• Alloys exhibit uniform distribution of
phases and much higher physical
characteristics
• Dimensionally stable and fully transformed
phase distribution in finished component
 NON FERROUS
MATERIALS, SUPER
ALLOYS AND
SINTERED
MATERIALS
• Solid Solution Strengthening
• Inter atomic distances (Bragg distances)
reduced
• Atomic packing density increased
• More Uniform Dispersion of nucleation
sites in PH alloys
• Increased Mechanical Properties due to
more ordered structure.
• Effects more dramatic in Single Phase
Alloys as compared with Multi Phase
Alloys
• Preferably carried out in finished
components as ductility & malleability
decreases significantly
• Pure metals show better results as
compared to alloys
• Even applicable in Noble Metals such as
Au, Ag, Pt, etc.
• Sintered carbides and other Powder
metallurgical components exhibit varying
degrees of improvement based on metallic
nature of the product.
 OTHER IMPROVEMENTS
• Long Range order established
• Corrosion Resistance increased
• Thermal, Electrical Conductivity & Hot Hardness
improved
• Dimensional stability, structural compactness
improved
• Grain Shape and Size refined.
• Vacancies erased, Dislocations and Stacking
Faults eliminated by forming fresh grain
boundaries.
 CONCLUSIONS
• EXPOSURE OF MATERIALS TO DEEP
SUB ZERO TEMPERATURES CAUSES
PERMANENT IRREVERSIBLE
CHANGED IN THE MICROSTRUCTURE
OF THE METALS
• PHENOMENON BEING EXPLORED AND
SCIENTIFIC BASIS FOR THE
IMPROVEMENTS BEING ANALYSED
 CONCLUSIONS
• BENEFITS QUANTIFIABLE IN THE CASE
OF ALLOY STEELS.
– PRODUCT LIFE INCREASES (50 - 700%)
– UNIFORM WEAR PATTERN ESTABLISHED
– AMOUNT OF REGRINDING/REDRESSING
MINIMIZED
• HARDNESS INCREASE DETECTED IN
NON FERROUS MATERIALS
 CONCLUSIONS
• DIFFERENT PROCEDURES FOR
DIFFERENT MATERIALS AS WELL AS
AT DIFFERENT STAGES IN THE
MANUFACTURING PROCESS
• OPTIMUM PROCEDURES STILL UNDER
STUDY FOR VARIOUS MATERIALS
• REAL AND TANGIBLE BENEFITS SEEN
THOUGH EXACT REASONS FOR THE
SAME ARE UNDER INVESTIGATION