ongoing development the · 2018. 4. 14. · tiro™ intermediate product (poppy seed) • small...

Christian Doblin, Ongoing development of the TIRO™ processOctober 7‐10, 2012 • Atlanta, Georgia, USA

Ongoing development of the TiRO™ process

Continuous direct titanium powder production


CSIRO Titanium Technologies ‐ from ore to moreCSIRO Titanium Technologies ‐ from ore to more

Titanium Technologies

MetalProduction

Powder to Product

ManufacturingVictorian Direct Manufacturing

Centre

TiROAlloys ProcessNovel Alloys

SheetWireExtrusionsBilletPowder Prep

Cold SprayAustralian Additive Manufacturing Init.

Machining Technologies

We pull resources from the overall pool of 6,500 dedicated employees of CSIRO. The Titanium Technologies group taps into the skills of 70 CSIRO scientists and engineers. We strive to build a titanium industry that is more efficient and affordable.


Mg

TiCl4

•Ti Powder

Ar

MgCl2

Process Intermediate (MgCl2/Ti composite)

Fluidised Bed Reactor

Vacuum DistillationSeparator

Electrolytic cell

TiRO™ ProcessTiCl4(g) + 2Mg(l) → Ti(s) + 2MgCl2 (s)

TiRO™ Process 3


TiRO™ 2.5 kg/h Ti equiv. FBRFBR freeboard

Exhaust

FBRfurnaces

Product pot

Control panel

TiRO™ Process4


TiRO™ intermediate product (from FBR)• The FBR product is near spherical particles (d50 ≈ 300 µm) comprising a continuous

MgCl2 matrix with much smaller uniformly dispersed Ti particles• Evidence of agglomeration occurring

Particle size distributions of FBR product

0

10

20

30

40

50

60

70

80

90

100

0 50 100 150 200 250 300 350 400 450 500 550 600 650 700 750

% C

umul

ative

Particle Size, µm

TF101025 - seed bed

TF101025-2hr

TF101025-4hr

TF101025 final bed

ESEM micrograph of “poppy seeds”

Photograph of intermediate“poppy seeds”

TiRO™ Process 5


TiRO™ intermediate product (poppy seed)• Small titanium particles dispersed throughout a MgCl2 substrate (d50 = 1.7 µm)• Some voidage and unreacted Mg in cores

0

10

20

30

40

50

60

70

80

90

100

0.1 1 10

size, µm

Cum

ulat

ive

vol%

0

2

4

6

8

10

12

Dife

rent

ial v

ol%

Cumulative vol%

Differential vol%

Particle size distribution of Ti particles in intermediate

Ti

ESEM micrograph of “poppy seed”

TiRO™ Process 6

Micro CT scan particle voidage (dark areas) unreacted Mg (bright spot) at the cross‐hairs


TiRO™ poppy seed chemical composition• Nominally 20 wt% Ti, 80 wt% MgCl2 (Based on reaction stoichiometry)• O


TiRO™ Continuous Vacuum Distillation Unit (CVDU‐X)

Ti discharge

3 temperature zone furnace

Feed hopper

Condensing side arm

Vacuum off take

Vacuum filter


Continuous vacuum distillation of “poppy seed”• Serves two purposes

• Separates MgCl2 from Ti• Sinters Ti to reduce specific surface area & hence

limit formation of surface oxide layer and limit O content to


TiRO™ vacuum distilled titanium biscuit• Lightly sintered• Limited mechanical strength, Very friable• Residual Cl = f(process conditions)

• Routinely achieve


TiRO™ vacuum distilled titanium product• Low density partially hollow spheres

• Free flowing powder when ‐‐‐‐‐‐broken up/ ground

TiRO™ “Biscuit” treatment d10[µm]

d50[µm]

d90[µm]

Bulkdensity,[kg/m3]

Tapdensity,[kg/m3]

Mortar and pestle ≈250 1.45 1.73Ring milled for 2 min 106 211 348 2.23 2.59Ring milled for 5 min 735 177 311 2.05 2.57


Techno‐economics of TiRO™ Source: Annual Reports, various

• Greenfield Comparison:– Median Kroll Plant Capital Cost US$ 35k/tpa– TiRO™ ‘Worst Case’ Capital Cost US$ 15k/tpa

• Expansion Comparison:– Average Kroll Plant Capital Cost US$ 19k/tpa– TiRO™ ‘Worst Case’ Capital Cost US$ 12k/tpa

TiRO™ capital cost is significantly below Kroll plants


Operating Cost ‐ comparisonAssuming common cost for TiCl4 and Mg

$0.00$1.00$2.00$3.00$4.00$5.00$6.00$7.00$8.00$9.00

US$/kg TI*

Sundry

Maintenance

Labour

Electricity &utilitiesCompany A B C D E F G

Potential for TiRO™ product to be used as a sponge replacement while the CP grade powder market is grown

Source: Ti‐Metal, TZMI*Costs adjusted for inflation from 2006


TiRO™ ‐ the next year• Scale‐up CVDU from 0.2 to 2.5 kg/h Ti• Design an integrated 2.5 kg/h TiRO™ process• Construct and operate an integrated 2.5 kg/h

TiRO™ process at commercial partner’s site in Laverton, Victoria (Coogee Chemicals)

– 1000 m2 facility• Produce powder for internal & third party

evaluation

Example of Ti sheet made with TiRO™ powder


Thank‐youTeam TiRO™• Christian Doblin• David Freeman• Matt Richards• Andrew Brent• David McCallum• Daniella Caruso

Techno‐economic evaluation

• Alex Kingsbury

Dr Christian DoblinCSIRO Future Manufacturing FlagshipProject Leader – Titanium metal productiont +61 3 9545 8658E [email protected] http://www.csiro.au/TitaniumTechnologies

ongoing development the · 2018. 4. 14. · tiro™ intermediate product (poppy seed) • small...

Documents