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Materials Science Forum Vol.

710 (2012) pp 113-118


Online available since 2012/Jan/24 at www.scientific.net
© (2012) Trans Tech Publications, Switzerland
doi:10.4028/www.scientific.net/MSF.710.113

Development and Characterization of Ti5Al2.5Sn-ELI Alloy


Hemispherical Domes for High-Pressure Cold Helium Tanks

Satish Kumar Singh1,a , Pravin Muneshwar2,b , K. Naresh Kumar3,c ,


Bhanu Pant4 , K Sreekumar5 and P. P. Sinha6
Materials and Mechanical Entity, Vikram Sarabhai Space Centre, Trivandrum-695022, India
a
satish_kumar@vssc.gov.in, bpravin_muneshwar@vssc.gov.in, cnaresh_kurnala@vssc.gov.in,
d
bhanu_pant@vssc.gov.in

Keywords: Ti5Al2.5Sn-ELI alloy, closed-die forging, microstructure, mechanical properties, multi-


point necking

Abstract Titanium alloys are used for high-pressure gas bottles / propellant tanks and structural
applications owing to their high specific strength, good fabricability / weldability and compatibility
with various working fluids. For these applications at ambient temperature, the workhorse Ti6Al4V
alloy is extensively used. For the applications at low temperatures, two ELI grades of titanium
alloys namely Ti6Al4V and Ti5Al2.5Sn are used as these retain toughness down to 77K and 4K
respectively. Due to this inherent advantage, Ti5Al2.5Sn-ELI alloy has been selected as high
pressure helium gas bottle submerged in liquid hydrogen (20K temperature). The gas bottle is
spherical in shape and is made by electron beam welding of two machined hemispherical shells of
500 mm nominal diameter. The hemispherical shells for the difficult-to-forge Ti5Al2.5Sn-ELI alloy
are developed through controlled closed-die forging operations. Shells are subsequently
characterized for microstructures and mechanical properties at ambient temperature. Substantial
increase in tensile strength with reasonably good ductility with respect to ambient temperature is
achieved at 20K temperature. Multi point necking is observed at 20K. The present paper briefly
outlines the process control devised for development of these domes and discusses the various
characterization results obtained on forged hemispherical shells.
Introduction
Titanium alloys find extensive application in aerospace industry due to high strength to weight
ratio, excellent corrosion resistance and high fracture toughness. Among the various Ti alloys,
Ti6Al4V alloy, the workhorse of the titanium industry, finds application as gas bottles, propellant
tank and motor cases for room temperature applications in aerospace due to its high strength to
weight ratio, good forgeability /formability, good response to heat treatment to achieve wide range
of mechanical properties, good weldability and fracture toughness. For low temperature
applications, two alloys namely Ti6Al4V-ELI and Ti5Al2.5Sn-ELI are used.
Ti5Al2.5Sn-ELI, due to its inherent ability to maintain toughness down to liquid helium
temperature, is selected for storage of cold helium gas at high pressure at 20K. Upper stage of
launch vehicle uses 500 mm nominal diameter spherical gas bottle submerged under liquid
hydrogen environment. Ti5Al2.Sn-ELI alloy has aluminum, which is an alpha phase stabilizer,
improves the strength of the alloy by solid solution strengthening. Tin (neutral element) is added to
improve its strength further by solid solution strengthening. The total content of the alloying
elements in the alloy should not exceed the aluminum equivalent value as given in the following
empirical relation:
Aluminium Equivalent = Al + Sn/3 + Zr/6 + 10(0) ≤ 9.0
The alloy is rated among the difficult to forge alloys and is characterized by need of high
unit pressure, due to higher aluminum equivalent in the alloy and is prone to cracking during
processing [1]. Higher flow stress coupled with tendency for cracking below the alpha transus,
narrow alpha-beta temperature range and scatter in mechanical properties for processing above beta
transus temperature require precise control of processing parameters during closed-die forging of
Ti5Al2.5Sn-ELI alloy.

All rights reserved. No part of contents of this paper may be reproduced or transmitted in any form or by any means without the written permission of TTP,
www.ttp.net. (ID: 130.113.151.253, McMaster University, Hamilton, Canada-18/03/15,19:20:10)
114 Advances in Metallic Materials and Manufacturing Processes for Strategic
Sectors

The paper brings out the processing methodology adopted for development of 500 mm
nominal diameter, 25 mm thick hemispherical domes required for liquid hydrogen submerged gas
bottles. Results of acceptance tests like dimensional, mechanical properties evaluations at ambient
temperature, microstructural observation, NDT carried out on hemispherical domes are included in
the paper. Tensile test results achieved at lower temperatures with two cross head speeds have been
included and effect of cross head speed on tensile properties at 77K has been highlighted.
Development and characterization procedure
The raw material (billets) of 225 mm diameter and 68 kg reference weight required for
conversion into hemispherical domes was processed by M/s Midhani, Hyderabad. Chemistry of
billet, mechanical properties and microstructural evaluation on samples, ultrasonic test to class A
level & Dye penetrant test on each billet were carried out for accepting the billets. The mechanical
properties and microstructure were evaluated on 100 mm square forged and annealed sections
realized from 225 mm diameter billets. The tensile strength and impact strength at ambient
temperature were evaluated as per ASTM E8 and E23 respectively.
The hemispherical domes were developed using 10T hammer at M/s BFL, Pune through
closed-die forging technique. The gas-fired furnace maintained under oxidizing atmosphere was
used for soaking of billets/semis. The hemispherical domes from the billets were forged in 1005°C
to 900°C temperature range in three steps, namely pan-caking, buster, and finish forgings in well
lubricated and pre-heated dies. Surface cracks observed during forging were removed by grinding
before next stage forging operation. The hemispherical dome developed has been included in Fig. 1

Fig. 1 Ti5Al2.5Sn-ELI alloy hemispherical dome.


Forged domes were annealed at 800°C for two hours and then cooled in air. Annealed
domes were descaled using shot blasting technique. Each hemispherical dome was inspected for
inner diameter, wall thickness, total height, end boss diameter, end boss height etc. Ultrasonic test
as per AMS 2631 to class A1 level and dye penetrant test were carried out on each dome to ensure
its soundness. One forged dome was destroyed for extensive mechanical properties evaluation.
Specimens from top, middle and bottom locations and from circumferential (longitudinal) and
radial (transverse) directions were taken for tensile and impact properties evaluations. The sample
was taken from the destroyed dome for microstructural and tensile properties evaluations at 20K
and 77K. Low temperature property evaluation was carried out at two cross head speed of 2
mm/min. and 0.5 mm/min. and using two types of specimen with 6.4 and 4 mm gauge diameters.

Results and Discussions


Chemical composition of Ti5Al2.5Sn-ELI alloy billets used for development of forged dome is
included in Table 1. The mechanical properties evaluated on 100 mm square forged and annealed
section are included in Table 2.
Materials Science Forum Vol. 710 115

Table 1 Chemistry of Ti5Al2.5Sn-ELI alloy billets used for processing of hemispherical dome
Elements Al Sn C Fe O N Fe+O H Ti
[wt%]
Specified 4.7- 2-3 0.05 0.25 0.12 0.035 0.32 0.0125 Balance
6.5 (Max) (Max) (Max) (Max) (Max) (Max)
Achieved 5.3 2.78 0.021 0.044 0.0855 0.0087 0.1325 0.008 Balance

Table 2 Mechanical properties obtained for Ti5Al2.5Sn-ELI alloy billets (in annealed condition, on
100 mm square forged and annealed blocks at 300K) for hemispherical dome
Type UTS 0.2%YS El RA Impact strength
(Charpy V Notch)
[MPa] [MPa] [%] [%] [Kg-m/cm2]
Specified (Minimum) 690 620 10 15.0 2.8
Achieved -Longitudinal 827-857 742-752 19-21 46-53 7.6-8.1
Achieved-Transverse 832-833 761-769 20 47-48 6.0-8.3

From Table 1, it can be seen that elements are within the specified limits. It is also seen that
impurities like iron, oxygen and nitrogen are controlled well below the specified limit. The
aluminum equivalent for Ti5Al2.5Sn-ELI alloy billet used for dome development is 7.11, which is
well below the specified limit of 9%. From Table 2 it can be seen that tensile and impact properties
meet the specified requirements.

Table 3 Dimensions achieved on dome


Type OD at Boss Total Height. Wall Inner
52.5mm Ht. Diameter. thickness radius
[mm] [mm] [mm] ]mm] [mm]
Specified 511.0 155 360 25 230.5
Minimum (+6.3, -0.0) (+5.0,-10.0) (+6.3/-0.0) (+0.0, -
4.0)
Dome-1 514.0/515.0 156.5 362.5 27.5 / 28.8 OK,
Achieved Dome-2 514.0/516.0 156.5 362.5 27.0 / 29.2 measured
Dome-3 514.5/515.0 156.0/156.5 362.0 26.6 / 27.2 with
Dome-4 512.0/516.5 155.0/156.0 362.0 26.2 / 28.8 template

Table 3 shows the dimensions achieved on the domes. It can be seen that domes meet the specified
requirement. Also, variations in dimensions from dome-to-dome are minimal. Pan cake and buster
forging operations are completed in one heat each while last stage of forging operation (finish
forging) is completed in 12-20 re-heats. Table 4 includes tensile and impact properties achieved at
300K on forged and annealed dome. As seen in Table 4, variation in longitudinal / transverse tensile
and impact properties at different locations on forged dome is minimal indicative of uniform flow
of material. The forged dome has met minimum specified mechanical properties. Forged dome and
billet sample tensile properties are comparable even though mechanical working on 100 mm square
section is less than 25 mm thick forged dome with same 225 mm diameter as input material. 100
mm square section sample has been forged in single heat where as multiple re-heats are experienced
during forging of dome. Properties achieved in the alloy are related to strain, strain rate and
temperature of deformation. Even though strain rate during closed-die forging operation through
hammer is high, multiple re-heats during closed-die forging has reduced the strain introduced per
heat to the dome and due to this increase in tensile strength on 25mm thick dome as compared to
100 mm square section is not observed.
116 Advances in Metallic Materials and Manufacturing Processes for Strategic
Sectors

Table 4 Mechanical properties achieved on forged and annealed Ti5Al2.5Sn-ELI alloy


hemispherical dome at 300K
Dome location 0.2%YS UTS EL RA Impact strength
(Charpy V Notch)
[MPa] [MPa] [%] [%] [Kg-m/cm2]
Top-Trans 760-775 822-840 17.0-19.0 31.3-47.0 4.5-4.8
Top-Long 789-793 829-833 17.0-17.5 43.0-43.2 5.2-5.5
Middle- Trans 769-777 816-826 17.0-19.5 36.0-47.0 4.1-4.7
Middle- Long 762-784 820-842 19.0-20.0 43.2-47.0 4.7-5.2
Bottom- Trans 760 -798 822-853 17.5-18.5 43.2-43.8 4.0-4.1
Bottom- Long 776-811 829-846 16.5-17.5 39.4-47.5 4.5-4.8
Where: Long and Trans stand for longitudinal and transverse direction respectively

Domes have met ultrasonic test requirement of Class A1 (1.2 mm diameter FBH) level. The
microstructure obtained on dome is shown in Fig. 2. It contains primary alpha in transformed beta
matrix resulting from below beta transus processing of the alloy.

30µm
Fig. 2 Microstructure observed on dome
From Table 5 it is seen that increase in tensile strength and 0.2%YS at 77K with respect to ambient
temperature is around 51.5 % and 55% respectively. Increase in tensile strength and 0.2%YS at 20K
with respect to ambient temperature is around 82.6 % and 72.5 % respectively. The increase in
strength with decrease in temperature is due to increase in resistance to dislocation movement.
Also, % reduction in area at 77K is nearly three times the % elongation indicative of load carrying
capability of the alloy even after necking (localized deformation). But at 20K, difference between %
elongation and % reduction in area is negligible. This implies that % elongation at 20K has more
contribution from uniform elongation than necking (non-uniform) elongation. The table also
includes tensile properties achieved on 4mm gauge diameter specimen and it is observed that tensile
properties are comparable to 6.4 mm gauge diameter indicating that there is no variation in tensile
properties for the gauge diameters included in the study.
Materials Science Forum Vol. 710 117

Table 5 Tensile properties achieved on Ti5Al2.5Sn-ELI alloy forged specimens at 77K and 20K for
production batch forgings for specimen gauge diameter of 6.4 mm
Sr. Identification Temperature UTS 0.2 %YS Tested with cross EI RA
No Details [MPa] [MPa] head speed [%] [%]
1 Smooth-1 1290 1230 2mm/ min. 10.0 29.0
2 Smooth-2 77K 1250 1200 11.0 34.0
3 Smooth-3 1240 1210 10.0 32.0.
4 Smooth-1 1536 1352 15.0 19.0
5 Smooth-2 1471 1336 16.8 18.2
6 Smooth-3 1545 1396 0.5mm/min. 14.0 16.5
7 Smooth-4* 20K 1536 1352 11.4 11.5
8 Smooth-5 1520 1337 12.4 16.4
9 Smooth-6 1477 1324 14.0 17.0
10 Smooth-7** 1533 1351 16.0 17.0
11 Smooth-8** 1530 1314 16.0 18.6
* Specimen failed at the end of gauge length, ** Specimen tested with 4 mm gauge diameter
Tensile test results achieved on 4 mm gauge diameter specimens with cross head speed of
2mm/min. and 0.5 mm/min. is included in Table 6 and it is seen that the strength values achieved
with two cross head speeds are similar while there is variation in % elongation with cross head
speed. Testing with 0.5 mm cross head speed reduces the gap between % elongation and %
reduction in area as observed in 20K testing. However, the gap between the two at 77K temperature
is more than that observed at 20K testing. Also, it is observed that percentage elongation is more for
specimen tested with cross head speed of 0.5 mm/min.

Table 6 Effect of cross head speed on tensile properties


Sl No UTS 0.2% YS El RA Cross head Test temp
[MPa] [MPa] [%] [%] speed
1 1230 1153 9.7 23 2mm/min 77K
2 1244 1201 9.5 27 2mm/min 77K
3 1269 1126 17.7 23.7 0.5mm/min 77K

Stress–strain diagram obtained at 20K for two specimen’s configurations are included in Figs 3a
and 3b. Serrations (multiple decrease and increase in stress) are observed in both the stress-strain
diagrams. These serrations results from multiple necking induced in the specimens due to
deformation couple with adiabatic heating during testing at 20K. Necking (load drop) occurs when
strain hardening becomes lower than softening observed during testing Condition for load drop
(instability in flow curve) has been reported as [2] :

(∂б/∂ε)-б≤(∂б/∂T)(б/ρCp) (1)
Where
(∂б/∂ε)-б = increase in strength due to deformation
(∂б/∂T)(б/ρCp) = decrease in stress due to rise in temperature
Б, ε, T, ρ and Cp are flow stress, strain, temperature, density and specific heat respectively.
At lower temperature, flow stress increases while there is substantial decrease in specific heat
compared to ambient temperature. The above points make flow softening more than strain
hardening and hence establish the condition for load drop at lower temperature due to adiabatic
heating. Due to rise in temperature, load falls and there would be a decrease in stress. During the
decrease in stress, strain hardening and decrease in specimen temperature due to heat flow from the
surrounding lead to increase in stress and this shifts the deformation and load drop at another
location in the specimen. Specimens with 6.4 mm diameter requires more time to achieve the
temperature for the rise in flow stress as compared to 4 mm diameter specimens and due to this
reason fall in stress is less and number of serrations are more in smaller diameter specimens.
118 Advances in Metallic Materials and Manufacturing Processes for Strategic
Sectors

(a)

(b)

Figs. 3: Stress strain diagram at 20K for specimen gauge diameter of (a) 6.4 mm and (b) 4 mm

Conclusions
1. Processing parameters for hot-forging of hemispherical dome from qualified Ti5Al2.5Sn-ELI
alloy billets through closed-die forging are developed using 10T hammer
2. Forged domes have met dimensional, NDT and mechanical properties requirements.
3. Substantial increase in tensile strength at lower temperature with respect to ambient
temperature is observed.
4. Strength achieved at 77K is not affected by cross head speed but % elongation is observed to
more at lower cross head speed.
5. Multi-point necking is observed during testing at 20K.
6. Both % elongation and % reduction in area are observed to be close to each other for tensile
test at 20K indicative of maximum contribution of uniform elongation to total elongation.
Acknowledgements
We acknowledge M/s Midhani, Hyderabad support in realizing Ti5Al2.5Sn-ELI alloy billets of
stipulated quality required for development of forgings and M/s Bharat Forge Limited (BFL), Pune
for providing support in developing the hemispherical domes of stipulated quality. Facility support
provided by MCD for characterization of the specimens and by CTF/LMF for testing at low
temperature, Quality support provided by QC/MMG & QCI/MME for the forged domes are
acknowledged. Authors are indebted to Director, VSSC for granting permission to publish/present
this work.
References
[1]Mathew J. Donachie, Jr., Titanium A Technical Guide, 2nd edition, ASM International, Metal
Park Ohio, 2000.
[2]George E Dieter, Mechanical Metallurgy, Third edition, McGraw-Hill Book Company, 1986.
Advances in Metallic Materials and Manufacturing Processes for Strategic Sectors
10.4028/www.scientific.net/MSF.710

Development and Characterization of Ti5Al2.5Sn-ELI Alloy Hemispherical Domes for High-Pressure


Cold Helium Tanks
10.4028/www.scientific.net/MSF.710.113