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Magnetic Science and Technology Microanalysis Laboratory. Summer 2003. Microscopy/Analysis of Metal Oxide Thin Films. Jennifer Haid Fairview Middle School 6 th Grade Science Jo Anne McBrearty Hawks Rise Elementary School 5 th Grade . What is a Metal Oxide Thin Film?.

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Magnetic science and technology microanalysis laboratory l.jpg

Magnetic Science and TechnologyMicroanalysis Laboratory

Summer 2003


Microscopy analysis of metal oxide thin films l.jpg

Microscopy/Analysis of Metal Oxide Thin Films

Jennifer Haid

Fairview Middle School

6th Grade Science

Jo Anne McBrearty

Hawks Rise Elementary School

5th Grade


What is a metal oxide thin film l.jpg
What is a Metal Oxide Thin Film?

  • It is a material grown on a substrate, which contains a transition metal, a group II and/or III element, and oxygen.

  • Type of ceramic


Purpose of metal oxide thin film research l.jpg
Purpose of Metal Oxide Thin Film Research:

  • Discover new and different properties of inorganic transition metal oxides

  • These properties may eventually be utilized in device applications:

    • High critical temperature superconductors

      • construct magnets, maglev trains, reduce energy costs, microscopic circuitry

    • Colossal magnetoresistance (huge magnetic field resistance) in the manganites.

      • Utilized in read-heads in computers


What metal oxides are being researched l.jpg
What Metal Oxides are Being Researched?

  • Ca2RuO4 (calcium ruthenate oxide) is the current focus

    • Properties: Paramagnetism, transitions between a conductor to insulator at very low temperatures

  • Lanthanum doped Ca2RuO4(lanthanum replaces small amount of calcium, Ca2-XLaXRuO4)

    • New properties: Weak ferromagnetism, conducting metal

Paramagnetism: disoriented electron spins;

must apply a magnetic force for it to have magnetic properties

Ferromagnetism: aligned electron spins


Ultimate goal l.jpg
Ultimate Goal:

  • Grow a film that is triple layered:

  • These layered metal oxides may have new properties:

    • Colossal magnetoresistence

    • Stronger ferromagnetism

Ca2-XLaXRuO4

Ca2RuO4

Ca2-XLaXRuO4


Research equipment l.jpg
Research Equipment:

  • Optical Microscope

  • ESEM (Environmental Scanning Electron Microscope)

  • Energy Dispersive X-ray Detector (detects element composition)

  • X-ray Diffraction Machine

  • TEM (Transmission Electron Microscope)

  • Hydraulic Pressure Machine

  • SQUID (Super Conducting Quantum Interference Device)

  • Pulsed Laser Deposition


Optical microscope l.jpg
Optical Microscope:

Microscope utilizing white light as its illumination source, allows up to 1,000X magnification

  • Uses:

  • Observe sample at lower magnifications

  • Prepare thin film samples under this microscope, because the microscopic nature of the thin film


Esem environmental scanning electron microscope l.jpg
ESEMEnvironmental Scanning Electron Microscope:

Microscope utilizing electrons as the illumination

source, allows up to 300,000X magnification

Use: Observe the surface features of samples in greater detail, better resolution


Tem transmission electron microscope l.jpg
TEMTransmission Electron Microscope:

Microscope utilizing electrons as the illumination

source, allows up to 1,500,000X magnification

  • Uses:

  • Observe the inside of a sample

  • (thin cross section)

  • 2) Observe atomic layer stacking

High Resolution of TEM

image of MgO crystal



X ray diffraction machine l.jpg
X-ray Diffraction Machine

  • Uses X-ray diffraction to confirm the structure of targets and thin films


Energy dispersive x ray detector detects element composition l.jpg
Energy Dispersive X-ray Detector (detects element composition)

  • - Attached to the ESEM and TEM

  • Use:

  • Creates a spectrum which gives the following information:

    • Element composition of

    • the sample

    • Quantities of each element detected


Hydraulic pressure machine l.jpg
Hydraulic Pressure Machine

Use: to compress the powder form of the chemicals in order to make the target

5 tons of pressure was being applied to this sample!


Squid super conducting quantum interference device l.jpg
SQUID (Super Conducting Quantum Interference Device)

  • Measure magnetic properties of a sample

- uses liquid Helium to test a wide range of temperatures

SQUID Cube

Liquid Helium Tank


Pulsed laser deposition l.jpg
Pulsed Laser Deposition

  • The laser beam is directed to the target, causing ions of the desired film to jump off in a plume. The ions in the plume hit the substrate, and a thin film grows upon this substrate.

KrF laser



Scientific method is applied in the thin film development l.jpg
Scientific Method is applied in the Thin Film Development!

  • Prepare sample

  • Gather data

  • Analyze data/Understand/Draw conclusions


Growth of thin film preparation of sample l.jpg
Growth of Thin Film(preparation of sample):

  • Make target by compressing the desired chemical compound for film and heat to 880°C

  • Use X-ray diffraction on target to be sure the structure is correct

  • Pulsed Laser hits target, ions jump off in a plume

  • Plume hits substrate and ions are deposited and grow to make a thin film


Characterization of thin film gathering data l.jpg
Characterization of Thin Film (gathering data):

  • Use ESEM, Energy Dispersive X-ray Detector (element composition) and X-ray Diffraction (structure) to confirm characteristics of film

  • Use TEM to investigate microstructures inside film, the stacking of atomic layers


Physical properties measurement of thin film gathering more data l.jpg
Physical Properties Measurement of Thin Film (gathering more data):

  • Measure magnetic property using SQUID (Super conducting quantum interference device)

  • Resistivity measurement


Analyze data understand draw conclusions l.jpg
Analyze Data/Understand/Draw Conclusions data):

  • A work in progress…


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New Questions/ Problems Arise While Conducting Research data):

  • CaO was used in making a target. The target was not confirmed to be the desired material…why? It was suspected that the CaO may have been exposed to water, making the target incorrect. We tested the CaO and did indeed find out, water had gotten into the chemical and may have changed it to Ca(OH)2


Special thanks l.jpg
Special Thanks: data):

  • Dr. Yan Xin

  • Mr. Xu Wang


Thanks l.jpg
Thanks: data):

  • National High Magnetic Field Laboratory

  • National Science Foundation

  • Center for Integrating Research and Learning

  • Dr. Pat Dixon, Director CIRL

  • Ms. Gina LaFrazza-Hickey,Education Specialist CIRL

  • Dr. Jack Crow


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