GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors:...

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GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: Jim Speck Lab Group Funding: DARPA & ONR Special Thanks to:Ben Haskell & Patrick Waltereit

Transcript of GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors:...

Page 1: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

GaN Crystal Growth & TEM Sample Preparation

Mentors:Feng Wu & Jan Lofvander

Faculty Advisor: Jim Speck

Lab Group Funding:DARPA & ONR

Special Thanks to:Ben Haskell & Patrick Waltereit

Page 2: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

Project Focus

• First 3 weeks: – TEM Manual Sample Preparation

• Last 3 weeks: – Automated Sample Preparation (FIB) & – GaN Crystal Growth

Page 3: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

Gallium Nitride

• Blue Light Emitting Diodes (LEDs) & Lasers– Wide Band Gap (3.4 ev)

• Transistors– Electrical Properties– Stability

Page 4: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

3 Methods to Grow GaN

• HVPE– Hydride Vapor Phase Epitaxy

• MOCVD– Metal Organic Chemical Vapor Deposition

• MBE– Molecular Beam Epitaxy

Page 5: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

Comparison of GaN Crystal Growth Methods

highestlowestFilm Quality

lowestmediumhighestGrowth Rate

lowest700 °C

medium1000 °C

highest1050 °C

TempMBEMOCVDHVPE

Page 6: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

Crystal Defect Structures

• Caused by slight incompatibility between GaN & Substrate– Lattice Structure– Thermal Properties– Other

• Examples:– Point Defect 0-D– Dislocation 1-D– Stacking Fault 2-D

http://www.tf.uni-kiel.de/matwis/amat/def_en/kap_5/backbone/r5_2_2.html

Page 7: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

Structural Characterization Tools• X-Ray Diffraction• Atomic Force

Microscope (AFM)• Optical Microscope• Scanning Electron

Microscope (SEM)• Transmission

Electron Microscope (TEM)

Page 8: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

TEM Image Stacking Fault

Plan View

Page 9: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

TEM imageDislocation

Plan View

Page 10: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

TEM Sample Preparation

• Manual Polishing– 1 day – 2 weeks

• Automated Polishing– 2-4 hours– Focused Ion Beam (FIB)

Page 11: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

TEM Sample• Thin film (GaN)• Substrate (Sapphire or Silicon Carbide)

GaN film

Plan ViewGaN film

Substrate

Side View

Page 12: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

Manual Polishing1. Cut & Glue the Sample

GaN film

Substrate

Silicon Silicon

Side View

Page 13: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

Manual Polishing2. Attach sample to Pyrex holder3. Insert Pyrex holder into Tripod

Sample

SampleTripodPyrex Holder

Page 14: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

Manual Polishing

4. Polish 1st side of Sample on Diamond Lapping Film until smooth

5. Glue Sample onto Copper Grid

6. Polish 2nd side of Sample until 10 µm thick

7. Ion Milling until 100 nm thick

Page 15: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

TEM imageDislocation

Plan View

Page 16: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

TEM imageDefects?

Cross Section

Page 17: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

FIB Focused Ion Beam

• No Sample Preparation

• 2 Beams– Electron– Ion

Page 18: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

FIB Procedures

1. Locate Site of Interest2. Mill a trench on either side3. Thin the wall4. Cut it out

Page 19: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

TEM imageDislocation

Cross Section

Page 20: GaN Crystal Growth & TEM Sample Preparation · GaN Crystal Growth & TEM Sample Preparation Mentors: Feng Wu & Jan Lofvander Faculty Advisor: ... Comparison of GaN Crystal Growth Methods

Reflections…• Research Lessons:

– TEM Sample Preparation • Time-Consuming• Delicate• Easy to Make Mistakes

– TEM images give most detailed info– Other forms of Microscopy used as a gage

• Classroom Applications:– Interviewing experts key– Learning about other components made it more

interesting/meaningful