NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area...

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NEXT GENERATION SINTERING April 2021 Dr David Pearmain - Advanced Materials and Processes (AMP)

Transcript of NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area...

Page 1: NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area solid state electrolyte sintering on metals −Hardware designed with low temp furnace

NEXT GENERATION SINTERING

April 2021

Dr David Pearmain - Advanced Materials and Processes (AMP)

Page 2: NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area solid state electrolyte sintering on metals −Hardware designed with low temp furnace

Next Generation Sintering….

− Flash Sintering and Scalability/ Applications

− Contactless Flash Sintering

− Cold/Flash Hybrid Systems

− Pressure Application and Flash Bonding

Electric Fields

Page 3: NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area solid state electrolyte sintering on metals −Hardware designed with low temp furnace

What’s new in ceramics sintering? Latest trends and futureprospects

M. Biesuz, et al., Current Opinion in Solid State and Materials Science 24, 100868 (2020)

− Technologies developed after 2010 are highlighted in bold characters.

− A few possible technologies that might emerge in the next few years are

highlighted in purple italic characters.

− The “quaternary diagram of sintering”:

different sintering technologies with key

processing features: external heating

and pressure, presence of water and

electric fields/currents.

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Flash Sintering

10 mm

− The application of electric fields to a ceramic during its sintering process to

instigate a Flash Event.

− Can be via:

− Contact or…

− Contactless electrodes.

Tim

e fo

r S

inte

rin

g (

s)

se

co

nd

sm

inu

tes

ho

urs

1

10

100

1000

10000

100000

Furnace Temperature

Conventional

Hot Press

SPS

Flash Sintering

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Next Generation Sintering – Commercial Benefit

− Lucideon has developed world leading capability and experience in Flash

Sintering techniques for industrial application

− Activities involve increasing material performance & improving bond

between dissimilar materials

− Activities to increase productivity (significantly reduce sintering time >50%)

− Lucideon research for >9 years focusing on repeatability/ scalability and

commercialization

− Lucideon developed unique advanced real time control software

− Working with both academia and industry to develop scalable solutions

− People and facilities in both UK and USA

Page 6: NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area solid state electrolyte sintering on metals −Hardware designed with low temp furnace

Host PC

1kHz real-time PC

Programmable power supply

Furnace

Electrode system

Ceramic

Low-voltage

High-voltage

Transformers

Control – the key to scalability of all new technology

− Real-time feedback on millisecond timescale

− Highly flexible and customisable

− DC to High Frequency AC.

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Broad Range of Sintering Capabilities

Capability Suited for Case study

Control systemFast, repeatable densification

Property improvements

Technical ceramics / UHTC

Nuclear Fuels

High frequency Inhomogenous bodies Multi-phase materials

Adaptable electrical contact

Large thin bulk samples

Unusual geometries, e.g. tubes

Dynamic systems

Tileware

Beta-alumina

Ceramic/Metal joining

ContactlessCoatings

Large flat surfaces

Ceramic repair

Electrolyte/metal multilayers

Flash Bonding Joining dissimilar materials Armor and Aerospace

Cold/Flash Hybrid Refractory/Glass/Electroltye Work emerging

Page 8: NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area solid state electrolyte sintering on metals −Hardware designed with low temp furnace

− Proprietary controller− Prevents flash-over− Homogeneity− Repeatability− Microstructural control

− Product enabler

Case study - technical ceramics (CIM alumina and YSZ)

FS- 9 min in 1050oC

furnace

FS- 83 min in 1050oC

furnace

Conventional

5 hr in 1500oC furnaceFS- 80 sec in 1050oC

furnace

20 um

Localization Homogeneous heating

Page 9: NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area solid state electrolyte sintering on metals −Hardware designed with low temp furnace

Flash of CIM 3YSZ

3.0

3.5

4.0

4.5

5.0

5.5

6.0

6.5

800 1000 1200 1400 1600

Den

sit

y (

gr/

cm

3)

Furnace Temperature (oC)

− Comparable density

− Lower sintering temperature by 350°C and in

half the time.

Performance evaluation – enhanced properties

(conventional vs flash)

From Cho, J. et al. High temperature deformability of ductile flash-sintered ceramics via

in-situ compression. Nat Commun 9, 2063 (2018).

Page 10: NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area solid state electrolyte sintering on metals −Hardware designed with low temp furnace

Case study – Frequency & Encapsulation

Example ‘Whiteware inert body and waste container glass’

− Higher densities achieved

− Increased productivity through reducing firing cycle.

Homogeneity achieved by high frequencies

Sample:

50mm x 50mm x 8mm commercial floor tile

LF HF

Sample:

10mm OD – 11mm thick

Page 11: NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area solid state electrolyte sintering on metals −Hardware designed with low temp furnace

Flash for Nuclear Fuels: surrogate fuel (CeO2)

FS-1100ºC

CS-1600ºC30μm

30μm

− Microstructural control possible − Moving to Uranium Dioxide and MOx trials

A joint development with NNL and UoM for Advanced Fuels

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Contactless flash – dealing with geometries & surface repair

− Glaze defects are a common issue for may ceramic industries

− Laborious, energy and time consuming repairs (24-36hr cycle at 1150ºC)

− Time reduced to less than 30 minutes in localized area.

Substrate glaze

Defect created

Defect filled

Defect repaired

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Contactless flash sintering: continuing development

Single location, room

temperature operation -

spot defect repair

Mobile electrode,

variable temperature

ceramic on metal

Kiln

Multi-axis

Robot

Low temperature contactless sintering –

homogenous, large area sintering,

multiple electrode geometries

Further development and

scale up

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Third generation contactless system

− Evolved to large surface area solid state electrolyte sintering on metals

− Hardware designed with low temp furnace surround for delta T control

− Integrated HV-electromechanical control algorithm

− Currently Sintering Ceramic Electrolyte layers and Multilayer systems on metals

− Robot has 100 micron resolution, with max acceleration of 100 ms-2.

Page 15: NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area solid state electrolyte sintering on metals −Hardware designed with low temp furnace

Third generation contactless system

Fuel Source

3 axis robot

(Multi-axis optional)

Electrode head

assembly

Electrical panel

Real time PC

Function

generator

HV amplifier #1

HV amplifier #2

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Contactless flash sintering in action

Control over the degree of sintering

Green Sintered

Page 17: NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area solid state electrolyte sintering on metals −Hardware designed with low temp furnace

Joining dissimilar materials – product enabler

− First highlighted by our work on solid state electrolytes…

− Metal to Ceramic (inc. CMC) joining via FLASH BONDING

− Fundamental research is underway into EBC sintering technologies and the joining of dissimilar materials.

− For Armour, technology to address:− Light-weighting− Multi-hit capability (shunting)− Performance against medium and heavy platform threats

− Potential application for co-sintering of battery components for improved cell performance

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Cold / Flash Hybrid systems – emerging developments

− As a new hybrid process, a combination between FS and CSP is emerging.

− Here, the presence of a liquid such as water (to ensure electric conductivity) within a

CSP apparatus connected to a power source allows to heat the ceramic powder up.

− Flash Cold Sintering (FCS) could therefore combine in a unique technique the

presence of solvent, electricity, extreme heating rates and pressure.

− Dramatically reduced sintering times and energy input….

A joint development with UoS and Industry / Innovate UK

Page 19: NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area solid state electrolyte sintering on metals −Hardware designed with low temp furnace

“Hybrid Sintering for Decarbonisation and Productivity in Manufacturing”

−Lucideon, along with consortium partners

has received funding as part of the TFI

programme for the Hybrid Sintering project.

−The objective: To assess the possibility of

developing a process by employing both

Flash and Cold Sintering techniques

−To be used by the glass/ceramics sectors

offering benefits in resource and energy

efficiency.

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Use of Electric fields in Next Generation Processing and

Ceramic Products

Multi-layer Ceramics

(SOFCs)

Joining of Dissimilar

Materials

Thermal/Environmental

Barrier Coatings

Solid State

Electrolytes

Sintering of Ceramic

Matrix Composite (CMCs)

Toughening of

Ceramics

Ceramic Armor

https://www.lucideon.com/uploads/pdfs/Nuclear-Engineering-International-September-2020.pdf

Other resources

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Takeaway message

− Flash sintering is a powerful sintering technique and requires a robust and

sophisticated controller for scale-up and process management.

− Flash sintering can dramatically reduce sintering timescales from hours to minutes,

minutes to seconds

− Property enhancement due to flash sintering can be a product enabler

− Contactless glaze repair, joining dissimilar materials and microstructure control are

promising technologies for future development of flash sintering

− Cold/Flash Hybrid systems could be used to reduce energy consumption and speed to

incredibly low levels vs conventional techniques.

Page 22: NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area solid state electrolyte sintering on metals −Hardware designed with low temp furnace

Thank you

Contact details

David Pearmain

T +44 (0)7793 000858

E [email protected]

W www.lucideon.com

Page 23: NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area solid state electrolyte sintering on metals −Hardware designed with low temp furnace

Dynamic Electrodes – Prototype Design

Commercial tile

Externally driven electrodes

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How is FS different from SPS?

− FS is a pressureless technique, SPS under load in a graphite die

− Current flows through the sample in FS, in SPS through the highly

conductive die. Sintering mechanism different, and not entirely

known….

− Energy consumption lower by an order of magnitude in flash

− Flash has more scalable application given the absence of a die

and the utilisation of more continuous processing methods.

Page 25: NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area solid state electrolyte sintering on metals −Hardware designed with low temp furnace
Page 26: NEXT GENERATION SINTERING · Third generation contactless system −Evolved to large surface area solid state electrolyte sintering on metals −Hardware designed with low temp furnace

Thank you

Contact details

T +44 (0)1782 764403

E [email protected]

W www.lucideon.com