Material innovation laboratory

three small square microchips placed on the pages of a book with visible text.

large, cylindrical metal chamber, likely part of scientific or industrial equipment. The chamber is open, revealing a complex mechanism inside.

complex assembly of industrial machinery, likely a component of a laboratory or manufacturing facility. The machinery is composed of shiny metal parts, including cylindrical and conical segments connected with various flanges and bolts.

Complex scientific instrument, likely an X-ray diffractometer, set up inside a laboratory environment. It features a cylindrical component at the centre, surrounded by various metallic parts and wiring.

More Information

About the Material innovation laboratory

Material research projects, thin film synthesis and thin film characterisation

The material innovation laboratory facility offers a range of capabilities ranging from synthesis and characterisation to full research projects focusing on high-throughput methodology.

The technology and setup available at the facility allow us to rapidly explore the compositional dependence, for a given family of materials, of chosen and specific fundamental characteristics.

High-throughput synthesis of thin film samples is combined with automated characterisation to efficiently acquire a unique and complete dataset of the material family. Using tailored software, the data is combined and analysed to produce an understanding of the relationship between composition, crystal structure and selected physical properties.

This approach has been implemented to study phase change memory materials, advanced alloys, functional ceramics, dielectrics, metals, electrocatalysts, battery materials (anodes, cathodes and electrolytes), hydrogen storage materials, gas sensors, thermoelectrics and photovoltaics as well as optical coatings and plasmonic materials.

The facility operates as an Engineering and Physical Sciences Research Council (EPSRC) small research facility and can be included on grant applications.

It also offers a contract service for external users upon discussion with the facility manager via the nC2 Engineering Consultancy.

Technical specification

High-Throughput evaporative Physical Vapour Deposition (HTePVD)

modified molecular beam epitaxy (MBE) system based on 100 mm wafer
- 3 x M600 chambers for up to 6 evaporation sources and one radio frequency (RF) atom source
- co-evaporation of up to 6 elements possible
- rotating heated manipulators up to 900 °C
- synthesis of material libraries on 35 x 35 mm substrates
6 x 3” targets radio frequency (RF) and direct current (DC) sputterer
- simultaneous deposition of up to 2 target materials
- argon or reactive sputtering
- rotating, heated manipulator
in vacuum x-ray photoelectron spectroscopy (XPS) system with automated X-Y stage
two high vacuum (HV) Load Locks, one with integrated glove box for sample preparation/protection
sample manipulation under ultra high vacuum (UHV) environment
sample storage and contact mask transfer capability in UHV
annealing chamber under vacuum up to 1100 °C

Complex mechanical apparatus with multiple cylindrical components attached symmetrically on either side.

Automated characterisation

Property	Technique	Array size	Acq. Time
Composition	EDS	14x14	4h
Structure	XRD	14x14	12h
Temperature induced changes	HTOMPT	14x14 (cont.)	6h
Optical constants	Ellipsometry	14x14	3h
Electrical resistance	4PP	14x14	2h-12h
Electrical impedance	LCR meter	14x14	6h
Electrochemical reactions	electrochemistry	10x10
Composition	XPS	5x5	4h

SEM-EDS

TESCAN VEGA scanning electron microscope equipped with Oxford Instrument energy dispersive spectroscopy detector (SEM-EDS)
secondary electron imaging (SEI) and backscattered electron imaging (BSE)
INCA and AZTEC software

A laboratory desk setup with an electron microscope and a computer monitor.

X-ray diffraction

Bruker D8 platform
Incoatec microsource, copper (Cu) radiation, 0.5 mm diameter
2D general area detector diffraction system (GADDS)
large, motorised X-Y-Z stage movement

$scientific instrument, likely an X-ray diffractometer, within a laboratory setting. At the center is a circular component with a black and white design, flanked by mechanical arms and electronic attachments.$

Ellipsometer

J.A. Woollam Ellipsometer, 250 nm to 1600 nm, automated X-Y stage
Refractive index (n) and Extinction coefficient (k) for PdxSn1-x alloys from 250 to 1600 nm
Refractive index (n) for AlAuPd system from 250 nm to 1200 nm
Extinction coefficient (k) for AlAuPd system from 250 nm to 1200 nm

laboratory setup featuring a sophisticated piece of equipment resting on a perforated metal table. Central to the setup is a black electronic device consisting of two vertical supports connected by a series of horizontal platforms and components, likely used for scientific measurement or research.

Atomic force microscope

Agilent 5600LS AFM

Probe station

signatone Probestation to enable automated electrical characterisation of materials
- HP4284A – Precision LCR meter – 20Hz to 1MHz, ± 20 Vdc bias
- network analyser
- semiconductor device analyser
- Keithleys DC SourceMeters and MultiMeters
- ferroelectric tester

Piece of laboratory equipment, specifically a microscope setup with dual eyepieces mounted on a metallic platform and placed in a lab environment. The equipment features several knobs and controls.

HTOMPT (High-throughput optical mapping of phase transitions)

purpose built apparatus which allows parallel screening of materials by recording optical changes in libraries as a function of temperature
controlled atmosphere
35 x 35 mm² samples max
Crystallisation Temperature of GeSbTe system
Oxidation of quinary system

A metallic cylindrical device with a transparent window on a perforated panel, surrounded by cameras and connectors.

RTA (Rapid thermal annealer)

Jipelec 150 RTA
150 mm wafers max
up to 1200 °C
controlled atmosphere

A laboratory machine with an open chamber, branded as "Jipelec" and "JETFIRST," showing its metallic interior and featuring an emergency stop button. The top section of the machine is open, revealing a circular metallic part with a glass section at the centre.

Tube furnace

100 mm diameter tube furnace
controlled atmosphere

A cylindrical laboratory furnace with a metal mesh cover on a blue control unit with labelled buttons.

Research

Since its development in early 2000’s, the High-Throughput evaporative Physical Vapour Deposition (HT-ePVD) methodology has been used to tackle various material innovations. The technology was key to the creation of Ilika Technologies Ltd, then a spinout company from the School of Chemistry specialising in material innovations using our high throughput approach with a focus on the metallurgy, electronics and energy sectors. During the last 20 years research projects led by both the Advanced Composite Materials Facility (now Material Innovation Laboratory) at the School of Chemistry, and Ilika have allowed further developments and specialisation in many aspects of material research as well as high-throughput technologies.

The High Throughput - evaporative Physical Vapour Deposition concept relies on simple geometry to allow intimate atomic mixing of elements. Each evaporated element has its own thermal evaporator (either an effusion cell or an electron beam source) and the concept uses the broad source nature of the evaporating material to create a shadowing of each source and achieve a variation in the deposition rate of each element as a function of position on the substrate. The high purity evaporants used in the ultra high vacuum environment produce high quality thin films which enabled the synthesis and optical characterisation of plasmonic materials. The co-deposition of all the constituents creates unique libraries and offers deep insight into the structure-composition-property relationship:

A benefit of the control of the composition spread of our technique is the fixed size of each library (35x35 mm_²). This enables the design and use of functional substrates such as Microelectromechanical Systems (MEMS). The simplest and probably most versatile is the Electrochemical Array which enables parallel electrochemical screening of 100 different compositions. It has been successfully employed to synthesise and screen alloys used for:

Another innovative and versatile MEMS device is an array of 49 micro-hotplates used for screening hydrogen storage materials where the characteristics of hydrogen absorption were probed as a function of composition. A modified version of the hot-plate array enabled the development of screening methodology for looking at heterogenous catalysis. The ability to capture single images of an entire library has, early on, showed the power of the high-throughput approach, this was further explored when focusing on the study of fluorescent materials for LED applications.

Each deposition chamber can hold up to 6 elemental sources, which can used simultaneously for the synthesis of multicomponent alloys. As well as binaries, ternaries, quaternaries, quinaries and senaries systems can be synthesised and characterised. This has facilitated projects in metallurgy and advanced alloys, such as:

The use of radio frequency (RF) atom sources to generate highly reactive fluxes of atomic gases (atomic oxygen, nitrogen or hydrogen) mixing directly with the condensed co-evaporants on the substrates have led to direct synthesis of complex materials, such as:

Combining many of these aspects, we can even probe functional thin film structure as in the case of solid state batteries and battery materials. Many other aspects of material research can be assessed using our high-throughput approach, including passive dielectrics, thermoelectrics, photovoltaics and gas sensors.