Sample Repositioning Solutions for
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1 Sample Repositioning Solutions for in situ Preparation and Analysis Cheryl Hartfield*, Matt Hammer, Gonzalo Amador, and Tom Moore *Senior Applications Specialist, Omniprobe
2 OUTLINE TEM sample preparation challenges and solutions Atom probe challenges and solutions 3D analysis challenges and solutions 2/25/ DC Area FIB User's Group 2
3 1. Smooth surfaces TEM SAMPLE PREPARATION Challenges and Solutions Example: Flipchipbump and Auwire bonded Alpad Challenge: Milling rate Crystal orient. Material ldensity Curtain Effect Solution: Backside thinning 2/25/ DC Area FIB User's Group 3
4 TEM SAMPLE PREPARATION Challenges and Solutions 2. Constant lamellae thickness Example: Tall and narrow semiconductor structures Challenge: Curtain Effect Tilt Correction 1 um 4 um Ga+ ion Si Solution: Sideways thinning R. B. Irwin et al., JVST A 27, 1352 (2009) 4
5 3. Conservation of stress TEM SAMPLE PREPARATION Challenges and Solutions Example: PMOS transistorwithepitaxialsigeinthe in the source/drain regions Challenge: TEM sample reflects native strain condition i Compressive stress Top R. B. Irwin et al., JVST A 27, 1352 (2009) Solution: Sideways thinning 5
6 TEM SAMPLE PREPARATION Challenges and Solutions 4. FIB damage during cleaning Example: Atomic stacking analysisof wide band gap perovskite insulators Challenge: 5kV FIB cleaning Amorphization Curtain effect Available area for TEM LaAlO3/SrTiO3 (LAO/STO) multilayers Solution: Angled thinning E. Montoya et al., Microsc. Res. Tech. 70, 1060 (2007) 6
7 TEM SAMPLE PREPARATION Challenges and Solutions Results of FIB cleaning orientation on LAO/STO multilayer performance Cleaning Size of HRTEM HAADF Curtain effect Preferential LaO Oi Orientation tti HRTEM Area STEM destruction ti Top Extended Good Good Strong Observed Top angle Extended Good Good Weak Observed ed 90 o degree Small Good Good None Observed 180 o angle Small Good Good None but uneven milling Not observed Solution: Depends ondesiredoutcome outcome E. Montoya et al., Microsc. Res. Tech. 70, 1060 (2007) 7
8 TEM SAMPLE PREPARATION Challenges and Solutions 5. Cross section vs. Plan View Example: Vertical CavitySurface EmittingLasers (VCSELS) Cross section Plan View Solution: Solution: Depends Frontsideand ondesiredoutcome outcome planar thinning TEM photos courtesy Phil Russell 8
9 TEM SAMPLE PREPARATION Summary: Challenges and Solutions CHALLENGE SOLUTION 1. Smooth Surfaces 2. Thickness Consistency 3. Conservation of Stress Sample Repositioning 4. FIB Cleaning Damage CHALLENGE: 5. Different Views How to reorient efficiently? 9
10 REPOSITIONING SOLUTIONS INLO Sample Orientations Frontside (0 o ) Lift out Sample Backside (180 o ) Ga+ No Flip Flip Any Direction Ga+ Sideways (90 o ) Planar Prep (90 o ) Ga+ Ga+ Top Flip CCW Flip Forward 2/25/ DC Area FIB User's Group 10
11 Movie Rotation alone does not provide desired repositioning 2/25/ DC Area FIB User's Group 11
12 Double Lift Lift sample at 45 o tilt Attach to substrate (0 o tilt) Re lift sample at 45 o tilt Attach to grid/holder REPOSITIONING SOLUTIONS Planar Preparation Strategies Grid Rotation Attach cut face to flat grid Rotate grid 90 degrees Stage Shaft Rotation Lift sample at specific stage tiltand rotation Rotate probe shaft Attach to aligned (rotated) grid Final thinning ion beam Final thinning Uses mathematical ti transformations ti based on conversion from angle-axis to rotation-matrix representation patent pending 12
13 REPOSITIONING SOLUTIONS Planar Preparation Strategies Shaft Stage Rotation Method, Example FIB 1, 50 o port elevation over door Lift sample at 52 o tilt and o CW stage rotation Rotate probe shaft 66 o CCW Attach to grid rotated 47.2 o CCW, zero tilt Final thinning 2/25/ DC Area FIB User's Group 13
14 Movie Planar preparation using the stage shaft rotation method 2/25/ DC Area FIB User's Group 14
15 REPOSITIONING IONING SOLUTIONS 90 o (sideways) preparation The lift out process is identical to planar prep Orientationwhen welded to grid is different 90 o Preparation Planar Preparation Ga+ Ga+ VS OR Ga+ 2/25/ DC Area FIB User's Group 15
16 Movie Sideways (90 o ) preparation using the stageshaft rotation method 2/25/ DC Area FIB User's Group 16
17 90 o + 90 o Grid Rotation REPOSITIONING IONING SOLUTIONS 180 o (backside) preparation Short Cut Attach using 90 o solution of choice; Perform standard lift out. rotate tt grid 90 o Do NOT mount to support. 1. Sideways attach vertically GRD Planar attach to flat grid Short Cut product for ex situ grid mounting Top Bottom 17
18 Atom probe specimen geometry: ATOM PROBE SAMPLE PREPARATION Challenges and Solutions Requirements and needs: Sharp needle Multiple l samples for one Tip radius nm result* Modest taper <10deg Cross correlation with TEM semi angle Backside preparation p Minute samples: nanowires, particles Optimized sample prep* Cap adhesion Min. amorphization No oxidation Standard preparation methods: The needle IS the sample (metal electropolishing) Placement on post arrays and FIB shaping *Könnig et al., Ultramicroscopy 109 (2009) Photos courtesy Brian Gorman/David Diercks, University of North Texas 18
19 ATOM PROBE SAMPLE PREPARATION Correlative TEM & Atom Probe Analysis Short Cut Prep Approach 1 Approach 2 1. In situ lift out 1. Short Cut (blank tips) Approach 3 1. Needle IS the sample Frontside Thinning 2. Short Cut 2. Lift out + in situ attach 2. Short Cut Backside Thinning 3. FIB shaping 4. TEM AP 3. FIB shaping 4. TEM AP 3. TEM AP Tomography (LEAP, TEM) Site specific Backside Many at once Back or frontside No FIB 19
20 3D ANALYSIS Challenges and Solutions 1. Automated EDX tomography Example: Ferromagnetic specimencu/ag solderjoint Challenge: Bulk effects shadow background Redeposition Detection efficiency Solution: Block lift out provides substantial improvement M. Schaffer, J. Wagner, Microchimica Acta 161, 421 (2008) 20
21 CONCLUSIONS Sample repositioning solves analysis challenges in beam based microscopy, improving data and results quality. Efficient solutions for sample repositioning have been presented. 2/25/ DC Area FIB User's Group 21
22 Backup Slides 2/25/ DC Area FIB User's Group 22
23 THE SHORT-CUT : WHAT IS SPECIAL? Rapid sample reorientation for FIB processing and conversion of unique samples to TEM compatibility Frontside thinning A cylindrical sample is tilted and attached to a probe tip Sample is cut free from substrate Backside thinning Final FIB milling from preferred direction Tomography Sample Sample completes Short Cut process Tomography (LEAP, TEM) Gorman et al., Microscopy Today, Vol. 16, No. 4, July 2008, p DC Area FIB User's Group 23
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