“Lift-out” FIB-TEM Specimen Preparation Technique
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The procedure of “lift-out” FIB-TEM specimen preparation technique is:

          i) Mechanically cut a piece of materials from a sample to fit inside FIB chamber.

          ii) Coat a conductive layer, such as carbon (C), chromium (Cr), or platinum (Pt), to prevent charging if the surface of the sample is insulator.

          iii) Mount the sample on a stub.

          iv) Load the stub together with the sample into FIB.

          v) Deposit a metal line on the area of interest (AOI) to prevent damage on the top portion of the specimen from sputtering. Typical dimensions of the metal line are 1~2 µm wide × 5~30 µm long × 2~3 µm high.

          vi) Cut a large stair-step trench on one side of the AOI with high Ga+ beam current.

          vii) Cut a rectangular trench on the other side of the AOI.

          viii) Tilt the sample to an angle greater than 45°.

          ix) Cut the bottom, left side, and a portion of the right side of the specimen.

          x) Tilt the sample back to its starting position (at 0° of angle).

          xi) Reduce the beam current to perform milling on each side of the specimen to reduce redeposition of sputtered material onto the surface of the specimen.

          xii) Clean the specimen by further reducing the beam current until the membrane is thinned to < 100 nm. The final thickness of the specimen will depend on the information you need and the density of the material(s).

          xiii) Remove the bulk sample from the FIB vacuum chamber.

          xiv) Put the bulk sample under a light optical microscope that has an objective lens with a large working distance.

          xv) Insert a sharp tip (~20–30 µm in size) into the arm of a hydraulic micromanipulator.

          xvi) Lift out the electron transparent membrane from the bulk sample by using the micromanipulator.

          xvii) Place the membrane onto a carbon- or formvar-coated Cu TEM mesh grid. In this step, the membrane is lifted out by electrostatic forces.

One clear disadvantage of this "lift-out" technique is that this technique does not permit further thinning if the prepared TEM specimen is too thick.

Table 2542. Example uses of FIB lift-out technique for TEM sample preparation.

Materials References
Biological materials [1, 2]
Composite materials [3, 4]
Geological materials [5]
Glasses [6]
Fibers [7]
Fracture surfaces [8, 9]
High temperature coatings [10]
Metals, alloys [11]
Monolithic ceramics [12]
Powder particles [5, 13]
Polymeric materials [14]
Plan view specimens [15]
Semiconductor materials [15]
Thin film cross sections [16]

 

 

 

 

 

 

 

 

 

 

 

 

 

[1] Giannuzzi LA, Prenitzer BI, Drown-MacDonald JL, Shofner TL, Brown SR, Irwin RB, Stevie FA, “Electron Microscopy Sample Preparation For the Biological and Physical Sciences Using Focused Ion Beams,” J. Process Analytical Chemistry, vol. IV, No. 3,4p. 162-167 (1999).
[2] Clayton FB, Kempshall BW, Schwarz SM, and Giannuzzi LA, “Automated Crystallography and Grain Mapping in the TEM,” Microsc. and Microanal. 8 (Suppl. 2), 656-657CD (2002).
[3] Giannuzzi LA and Lewinsohn CA, “Interphase Oxidation In SIC/SIC Composites At Varying Partial Pressures Of Oxygen,” Annual Conference on Composites, Advanced Ceramics, Materials, and Structures: B, Ceramic Engineering and Science Proceedings, eds. Ersan Ustundag and Gary Fischman, Vol. 20, Issue 4, p. 115-122 (1999).
[4] Giannuzzi LA and Lewinsohn CA, “Interphase Oxidation in SiC/SiC Composites,” Annual Conference on Composites, Advanced Ceramics, Materials, and Structures: A, Ceramic Engineering and Science Proceedings, eds. Todd Jansen, Ersan Ustundag, Vol. 21, Issue 3, p 469-477 (2000). 
[5] Drown-MacDonald JL, Prenitzer BI, Shofner TL, and Giannuzzi LA, “TEM FIB Lift-Out of Mount Saint Helens Volcanic Ash,” Microscopy and Microanalysis, vol.5, supplement 2, Proceedings: Microscopy & Microanalysis 99, 908-909 (1999). 
[6] Stevie FA, Vartuli CB, Giannuzzi LA, Shofner TL, Brown SR, Rossie B, Hillion F, Mills R H, Antonell M, Irwin RB, and Purcell BM, “Application of Focused Ion Beam Lift-Out Specimen Preparation To TEM, SEM, STEM, AES, and SIMS Analysis,” Surface Interface Analysis, 31, 345-351 (2001). 
[7] Giannuzzi LA, Drown JL, Brown SR, Irwin RB, and Stevie F, “Applications of the FIB Lift-Out Technique for TEM Specimen Preparation”. Micr. Res.Tech. 41 285-290 (1998). 
[8] Giannuzzi LA and Lewinsohn CA, “Interphase Oxidation In SIC/SIC Composites At Varying Partial Pressures Of Oxygen,” Annual Conference on Composites, Advanced Ceramics, Materials, and Structures: B, Ceramic Engineering and Science Proceedings, eds. Ersan Ustundag and Gary Fischman, Vol. 20, Issue 4, p. 115-122 (1999d).
[9] Giannuzzi LA and Lewinsohn CA, “Interphase Oxidation in SiC/SiC Composites,” Annual Conference on Composites, Advanced Ceramics, Materials, and Structures: A, Ceramic Engineering and Science Proceedings, eds. Todd Jansen, Ersan Ustundag, Vol. 21, Issue 3, p 469-477 (2000). 
[10] Carim AH, Dobbins TA, Mayo MJ, and Giannuzzi LA, “Interfacial Microstructure For As-Deposited And Cycled-To-Failure Thermal Barrier Coatings,” in Elevated Temperature Coatings: Science and Technology IV, N. B. Dahotre, J. M. Hampikian, and J. E. Morral, eds., TMS, Warrendale, PA, pp. 45-59 (2001). 
[11] Hampton MD, Lomness JK, and Giannuzzi LA, “Surface Study of Liquid Water Treated and Water Vapor Treated Alloy,” accepted and in press, International Journal of Hydrogen Energy, (2002). 
[12]Lomness JK, Kempshall BW, Giannuzzi LA, Watson MB, “TEM of Sub-Micrometer Particles Using the FIB Lift-Out Technique,” Microsc. Microanal., 7 (Suppl 2: Proceedings), Microscopy Society of America, 950-951 (2001b).  
[13] Prenitzer BI, Giannuzzi LA, Newman K, Brown SR, Irwin RB, Shofner TL, and Stevie FA, “Transmission Electron Microscope Specimen Preparation of Zn Powders Using the Focused Ion Beam Lift-Out Technique,” Met. Trans. A, Vol. 29A, pp. 2399-2405. (1998).
[14] White H, Pu Y, Rafailovich M, Sokolov J, King AH, Giannuzzi LA, Urbanik-Shannon C,
Kempshall BW, Eisenberg A, Schwarz SA, and Strzhemechny YM, “Focused ion beam/lift-out transmission electron microscopy cross sections of block copolymer films ordered on silicon substrates”, Polymer 42, 1613-1619 (2000).
[15] Stevie FA, Irwin RB, Shofner TL, Brown SR, Drown JL, and Giannuzzi LA, “Plan View Sample Preparation Using the Focused Ion Beam Lift Out Technique,” Proceedings of the 1998 International Conference on Characterization and Metrology of ULSI Technology, vol. 449, Gaithersburg, MD, March 23-27, 1998, eds. DG Seiler, AC Diebold, WM Bullis, TG Shaffner, R. McDonald, EJ Walters, p 868-871 (1998).
[16] Stevie FA, Shane TC, Kahora PM, Hull R, Bahnck D, Kannan VC, and David E, “Applications of Focused Ion Beams in Microelectronics Production, Design and Development,” Surface and Interface Analysis, 23, 61-68 (1995).
 
 
 
 
 

 

 

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