Superplastic forming of titanium

European Titanium Conference 2009

Parallel Session D: 11.10am 11.35am
Dr Richard Curtis PhD, DIC, CEng, CSci, FIMMM, FADM Chair, IOM3 Superplasticity Committee, UK. Department of Biomaterials, Biomaterials, Biomimetics and Biophotonics Research Group.

Acknowledgements
Dan Sanders, Boeing Inc Bill Swale, Aeromet Ltd Peter Stewart, BAe Systems Mike Wallis, Rolls Royce Werner Beck, Formtec AG. Colleagues at Kings College London, University of Wales Swansea, University of Kentucky.

A community..
....of superplastic forming practice has emerged: - Euro SPF meetings, 2001, 02, 04, 05, 07, 08, 2010 (Bilbao / San Sebastian) - Euro SPF website - UK IOM3 Superplasticity Committee - USA Superplastic Forming Committee - ISO, ASTM and Standards

SIM-O-SPF - what are the

objectives..?
SIM-O-SPF will provide a forum to share knowledge and experience about SPF process in general and Simulation of SPF in particular. Will identify limitations of current Simulation capabilities and recommend future developments Will create an effective partnership amongst all members from different background (academia, commercial software and industry) Providing immediate access to well established simulation tools that are used by various parties for SPF applications in Aerospace, Rail and Automotive Introduce Simulation-based approach to SPF that would result in higher quality components, improved design, optimized manufacturing parameters and a more cost effective approach Enhance the capabilities of existing Simulation tools by further developments and diversity in applications For further details contact: rajab.said@esi-group.com
Copyright ESI Group, 2009. All rights reserved.

The Euro-SPF group is a community federating European industries and universities involved in SuperPlastic Forming. It promotes exchanges between the members as well as the SPF technology. It also informs about the meetings directly or indirectly linked to SPF and about the positions offered in the universities and in the companies

SPF technology in aerospace

SPF technology in automotive

SPF for Medical Prostheses

Titanium alloys have some of the best biocompatible properties of all metallic alloys and for this reason many dental and medical implants and devices are manufactured from both the commercially pure and the Ti6Al4V alloy forms.

ceramic die

argon gas Ti-6Al-4V sheet Induction coil heating

Ti-6Al-4V Alloy formed sheet

Die chamber pre-heated to 900oC inside the press

Ceramic die

Orbital Floor Fracture

Upper face trauma usually results in fractures of the internal orbit, usually termed Orbital Blowout Fracture. Patients usually present with pain, swelling & often double vision is experienced. Bones in the orbital region play a vital role in the normal function of the eye. Therefore, accurate realignment or anatomic reconstruction of the bony orbit is essential in maintaining normal function. Recent advances in diagnosis & treatment of internal orbital fractures: CT scanning greater ability to improve implant design and production.

Aeromet Forming Division, established in 1985 produces Airframe and Engine Components from Titanium Sheet and Plate by Superplastic, Hot Forming, Chemical Milling and & Laser Trimming. Aeromet makes a minimum of 150 different SPF components on a production basis

Superplastic Forming Press

5 Axis Laser Trimming

Chemical Milling Plant

Superplastic Forming
Superplastic Forming at 900C Four components in one pressing Ti6/4 2,0mm thick

Complex assembly
Spherical & Conical shapes produced by SPF

Size:-600mm diameter x 300mm deep x 0.81mm skin thicknesses. Material - Ti 6/4

Assembly of Nine SPF Details

Tail Cone Section

Superplastic Forming at 900C Two products Ti6/4 0,8mm and one at 1,6mm thick. Size 800mm sq.

Tail Cone Section

Superplastic Forming at 900C from 2.2mm thick Ti6/4 Size 800 x 600 x 300mm Deep.

Product Examples

Various Firewalls & Assemblies made from Superplastically Formed components.

Typhoon
Tunnelskin Panel

Keel Panel

General view of two sheet SPF/DB keel panel in part assembled rear fuse of Typhoon. (NB. Single sheet tunnel skins also present) (Courtesy BAe Systems)

Typhoon
Top sheet

Core sheets

Lower sheet

Segment of four sheet X core configuration of SPF/DB Typhoon fore-plane.

(Courtesy BAe Systems)

Cellular structure

~1100mm

Four sheet DB/SPF/DB six cell demonstration piece.

(Courtesy BAESystems and MOD)

Rolls-Royce Barnoldswick
DB/SPF fan blade - internal structure

Section > 80% Hollow

Superplastic line core

Membrane Panel

Diffusion Bond

An SPF cell with the latest generation of presses at Rolls-Royce Barnoldswick

ARIANE V, SPF Hemispheres Ti6-4

Membrane thickness s=0,8 -0/ +0,2mm Pole/equator zone thickness = 1,8 / 2,2mm Roundness tolerance D= 483 0,2mm Final strength= 1020 N/mm

Replacement of forged shells No final surface machining Thickness formed to final shape Schedule reduction Cost savings ~30% from Ti-scrap reduction Production effort
08.05.28_ISC Forum.ppt
The information contained herein is proprietary to FT and shall not be reproduced in whole or part or used for any purpose except when such user processes direct written authorisation from FT.

22

Ti 6-2-4-2 Closing Shell

Closing shell ri./ le. with weird shape Process and forming tools fully functional SPF parameters Ti 6-2-4-2 from FT database Cycle time ~10 mins

08.05.28_ISC Forum.ppt
The information contained herein is proprietary to FT and shall not be reproduced in whole or part or used for any purpose except when such user processes direct written authorisation from FT.

23

Silent Helicopter Exhaust

Materials data beyond current max application temperature, Ti6-4, Ti6-2-4-2 and Ti beta21S Temperature simulation Stress simulation Design process = f (low mean + peak stresses, heat flow, heat radiation, temperature dissipation) Process development Prototype articles Engine bench test

08.05.28_ISC Forum.ppt
The information contained herein is proprietary to FT and shall not be reproduced in whole or part or used for any purpose except when such user processes direct written authorisation from FT.

24

SPF Standards

SuperPlastic Laser Integrated Component Equipment (SPLICE)

LASER

Cutting Blanks from Sheet Stock

Welding and/or Diffusion Bonding

Surface Preparation

SPF/DB

Fatigue Enhancement

Hole Drilling

Removal of Surplus Material

In Process Inspection

Laser Induced Superplasticity (LIS)

Raw Material All Content of this presentation, copyright LISTechnology Ltd. Finished Component
26

Laser Induced Superplasticity (LIS)

Double Sided Forming

All Content of this presentation, copyright LISTechnology Ltd.
27

Benefits of the Technology Being Pursued

Quicker
Process should allow a Massive Compression in SPF/DB Cycle Times
Long Cycle Time
Material Preparation 75% Reduction Heat-up 90% reduction Forming Cool Down Finishing Operations 15% 95% 50% reduction reduction Reduction

Short Cycle Time

Saving of 66%
28

All Content of this presentation, copyright LISTechnology Ltd.

Superplastic Prosthetic Forming

patient prostheses SP forming

Simpleware solution

log

die
Ti-6Al-4V
log &

In this case, Simpleware software allows conversion of 3D images into high quality meshes which can be used for FEA, CAD and RP. Enabling implant design and manufacture. FE meshes Said & Curtis et al. KCL

Pressure cycle FE-SPF simulation

Provision of Maxillofacial Implants

Cranioplasty Orbital Floor Reconstruction Malar Augmentation

(Wehmller et al, 2004)

Trevor Coward and Richard Curtis, KCL

Contamination in titanium
The alpha case is generally known to be developed by the interstitials such as carbon, nitrogen and especially oxygen dissolved from mould materials
from the synthesis of the microstructure, the hardness profile, EPMA mapping and TEM, it could be confirmed that the alpha-case is formed by not only interstitial oxygen atoms but also substitutional metal atoms dissolved from mould materials.
Materials Science and Engineering A 405 (2005) 173177

Die-Ti-6Al-4V surface modification

Forming conditions: 180 minutes @ 900C

100 m Quartz substrate

Ammonium Biflouride etch

100 m Croform investment substrate

32
Atwood & Curtis et al. KCL

Depth of interaction zone

150
Croform-WB Rematitan Ultra Alumina 800 C 850 C 900 C

Depth (um)

100

Zirconia Silica

50

0 0
33
Atwood & Curtis et al. KCL

50

100 Time (min)

150

200

Bending Ductility Tests

Determine the ductility or strength of a material. Aim - produce results of either pass or fail. Clause 6 Shall not show any cracking on the outside surface of the test piece strip should be bent through an angle of 105 around a mandrel. Failure of the test piece plastic deformation or crack initiation may be attributable to one mode only. In the case of a three-point bend test, it is most likely to be due to the tension on the lower, convex surface. Instron 1193 machine - produce results (Load vs Deflection graphs).
Ditta & Curtis et al. KCL

V-block bend test

Load vs Deflection graph

Load (N)

Deflection (mm)
Ditta & Curtis et al. KCL

Bending Test Samples

- specimens 1 - 3 = die-side in tension.

- specimens 4 - 6 = gas-side in tension.

Ditta & Curtis et al. KCL

Furnace Samples
Furnace 20
500
Specimen number

400

Load (N)

300

1 2 3 4 5 6

}die }gas

200

100

Overlap of graphs

0 0 2 4 6 8

Deflection (mm)

Ditta & Curtis et al. KCL

SPF Samples
SPF 30 - (Guys 422)
500
Specimen number

400

Load (N)

300

1 2 3 4 5 6

}die }gas

200

100

4-6 : able to withstand greater load before failure.

Ditta & Curtis et al. KCL

0 0 2 4 6 8

Deflection (mm)

1-3 : failed earlier than 4-6.

Effect of time on mechanical properties: furnaced samples.

Furnace 120 no plastic region on graphs brittle behaviour.
Furnace 20 VS Furnace 120 : Specimens 1-3 (die-side)
500 Specimen number 400 F 20 - 1 F 20 - 2 F 20 - 3 F 120 - 1 F 120 - 2 F 120 - 3

Load (N)

300

200

Furnace 20 obvious plastic region on graphs ductile behaviour.

100

0 0 2 4 6 8

Deflection (mm)

Ditta & Curtis et al. KCL

Bioactivity assessment by immersion in SBF using SEM and EDX:

Ti64 (Sanded) SP700 (Sanded) Ti64 (NaOH) SP700 (NaOH)

D1

D3

D7 D7
Ti Ti P Ca Ca Ti Ca P Ca Mg Ca Ca Ti

EDX (D7)

V Ti Al

V Ti

V Ti Al

V Ti

Omar & Curtis et al. KCL

SEM and EDX:

Ti64 (Degu 900C) Ti64 (Wiro 900C) SP700 (Wiro900C)

D1

D3

D7

Ti

P Si

Ti Ca Ca

P Ca Ti

P Ca

Ti

EDX (D7)

Ca

Mg Si

Mg

Omar & Curtis et al. KCL

Day 3

Cp-1
Cells: primary human osteoblasts

Ti64

G417 20min TCP control

Nunclon tissue culture plate

TCP: tissue culture plastic no disk G416 120min CP-1: unalloyed titanium Ti64: Ti64-G417 (SPF 900C) Ti64-G416 (SPF 900C) PVC control: Portex +control strips
42
Atwood, DiSilvio & Curtis et al. ongoing project, KCL

PVC toxic control

Alamar Blue proliferation - indicates metabolic activity affected by the number of cells
human osteosarcoma cells

0.3 Arb. Units

0.2

0.1

120 min

SP700

20 min

CP1

Ti64

43

Superplastic Prosthetic Forming samples: g417 (20 min) / g416 (120 min)

Atwood, DiSilvio & Curtis et al. ongoing project, KCL

tcp2

pvc

tcp

0.0

Alkaline phosphatase produced by cells associated with bone forming tissue (differentiation)
ALP expression in cell lysate distrupted cell membranes represents differentiation

44
Atwood, DiSilvio & Curtis et al. ongoing project, KCL

Alkaline phosphatase released from cells on surfaces in media

Alkaline Phosphatase in Supernatant Solution 0.18 0.16 0.14 0.12 0.1 0.08 0.06 0.04 0.02 0
Supernatant meaning fluid from around/above cells however, cells could be withdrawn from the fluid influencing the results. NB. cells may not be adhering to surface of the disk.

Average sample set 1 sample set 2 sample set 3

arb units

Ti64

g417

sp700

g416

cp-1

tcp

..the activity of the enzyme ALP reaches a peak at day 7 on SPF titanium alloy (g417) suggesting that the presence of reaction products on the surface have a stimulatory effect

Sample type

tcp = tissue culture plastic (no sample) pvc = polyvinyl chloride toxic control disk m = medium alone (no cells) b = buffer alone (no cells)

27 disks: 3 of each type of disk - each point is 4 measurements

pvc

Cell Proliferation
-Alamar blue to measure cytotoxicity, proliferation or activation Classical proliferation profile

Omar & Curtis et al. KCL

Recent advances in the understanding of the chemistry of investment materials?

Scrimgeour et al., (2007) with 31P solid-state MASNMR spectroscopy on phosphate bonded investment: (a) Deguvest -- setting struvite, amorphous orthophosphate farringtonite, Mg -- burn-out (900C) metaphosphate (b) Wirovest -- setting struvite, amorphous orthophosphate -- burn-out (1050C) pyrophosphate (dominant), amorphous orthophosphate.

What is known about the titanium alloy surface?

Titania (TiO2) of 7 8 nm forms a passive and corrosion resistant film on the alloy surface Titania is an n-type semiconductor that can be doped with other elements to modify its electronic properties. e.g. Nb5+ ions or P5+ ions Titania exists in three different crystalline allotropic forms, brookite, anatase and rutile although it may also be amorphous

Rutile titania
http://www.fis.unipr.it/phevix/img/tot_disorder.jpg

http://zqlin.public.iastate.edu/TiO2%20Raman%20Spectra.jpg

For Ti-6Al-4V alloy the transformation to rutile is suppressed

Omar, Festy & Curtis et al. KCL

Shapes produced by Superplastic Prosthetic Forming

Juszczyk & Curtis et al. KCL