Beruflich Dokumente
Kultur Dokumente
Elektronenmikroskopie-Zentrum der ETH Zrich (EMEZ) u c/o Institut fr Angewandte Physik u ETH-Hnggerberg o CH-8093Zrich u
Contents
1 Cutting slices 2 Forming a stack 3 Embedding the stack in a tube 4 Cutting the tube into disks 5 Polishing the disks 6 Dimple-grinding 7 Ion milling 8 Final TEM sample 1 3 5 7 9 11 14 17
Preface
! Note that the following instructions are not suitable for the cross-section preparation of every kind of sample material; if your sample is soluble in water or acetone, you should rather consider a sample preparation by e.g. focused ion beam (FIB) cutting! ! Also, this manual is written for cross-section sample preparation of samples that consist of a substrate with a stack of thin-lm layers on top of it. It can be easily adapted to the preparation of e.g. metal samples as well.
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1. Cutting slices
Step-by-step:
- for mixing the glue, cut a piece of Al foil with scissors, fold piece four times - put appropriate number of droplets of both hardener and resin on the Al foil - stir with toothpick 3
2. Forming a stack
- put slice of Si wafer on another piece of Al foil - apply epoxy glue sparingly on the slice of Si wafer - put slice of sample on top of slice of Si wafer - anneal at 120 C; the best way to nd out when the epoxy glue has hardened is to put a small drop of epoxy glue next to the stack on the Al foil - in order to have as little epoxy glue as possible between the slices (for better stability of the sample, less preferential etching of the epoxy glue during ion etching and applicability of the auto-stop in the ion etcher) the slices are pressed during annealing of the epoxy glue. If the pressure, however, is only a little bit too strong, this will again lead to cracks in the sample material. Therefore, it is recommended to put some pressure onto the stack with the tweezers before annealing and only x the stack during the annealing
Figure 2.1: Left: Mixing hardener and resin in a ratio of 1:10. Right: Forming a stack by slice of solar cell on the top and Si wafer on the bottom
Step-by-step:
- check whether the stack ts into the respective tube; if it does not, grind the stack with abrasive paper - clean the tube in an acetone bath - place the tube standing on a piece of Al foil - ll a droplet of the epoxy glue into the tube (use toothpick) - drop the stack into the tube on top of the epoxy glue - place the tube standing on the Al-foil on a heating plate (120 C); the epoxy glue becomes more uid after a few seconds, the stack will sink into the epoxy glue - only if the stack does not sink totally into the epoxy glue, a small pressure by the tweezers may be applied - after the initial droplet of epoxy glue has hardened, the tube is lled with some more epoxy glue: always add droplets where the distance between the 5
stack and the wall of the tube is smallest. This way, you will avoid gas bubbles within the adhesive, which would destabilize the samples during further preparation - some epoxy glue should always run out of the tube - this tells you the tube is completely lled with glue; the colour of the epoxy glue will change from transparent-yellow to brown when it is fully hardened; you may also check with the tweezers
Figure 3.1: Left:Filling a droplet of the epoxy glue into an Fe tube. Middle: Dropping the stack into the tube. Right: The stack is sealed within the hardened epoxy glue.
Step-by-step:
- the tube is glued with thermo-wax on an Al holder. With a diamond wire saw disks of about 300-400 m thickness are cut - when mounting the tube on the Al holder, put thermo-wax all around the tube, thus, best adhesion to the Al holder is guaranteed, and also the cut disks will not drop o the holder - keep in mind that the wire of the saw has typically a thickness of about 300 m; therefore, a distance of 600 - 700 m from one cut to the next is reasonable - the counterweight applied on the wire depends on the stability of the sample material. The more brittle it is, the less counterweight should be applied - the speed of the diamond wire saw should be kept rather low - one Al holder may be used to cut about 20-30 disks, i.e. several tubes! - just cut once at each position of the Al holder! - if the sample contains a layered structure which easily delaminates, the tube has to be placed with the interfaces parallel to the wire. Best x the tube in such a way onto the Al holder that the Si-wafer on top of the layered structure faces the diamond wire (see gure 4.1) 7
Figure 4.1: Fe tube mounted on the Al holder: the Si wafer faces the diamond wire
Step-by-step:
- select a glass cylinder to be used as a support of the disk and measure its height using a micrometer gauge - glue one disk with thermo-wax on top of the glass cylinder (see gure 5.1) - polish one side plan-parallelly to the other side - ip the disk on the other side - measure the total thickness (cylinder+disk); calculate the disk thickness - polish the other side; the disk is to be ground down to a thickness of about 95 - 110 m; thus, one achieves high stability as well as short time for dimplegrinding - at the lapping machine, use rst 400-, 1000- or 1200-grade grinding paper (depending on the brittleness of the sample material, then 4000-grade grinding paper - if the polishing procedure is done by hand, move the glass cylinder with the mounted disk in circles on the grinding paper; the thickness of the sample may be estimated by the number of turns on the milling paper, if the diameter of the circles are always approximately the same. When polishing the second 9
side of the disk, twist the glass cylinder several times to prevent the disk from becoming wedge-shaped - the thickness of the disk may also be controlled by checking the colour of the epoxy glue - if the sample contains a layered structure which easily delaminates, always grind in a direction parallel to the layers! - remove the disk from the glass cylinder on the heating plate and check the nal thickness of the polished disk using a micrometer gauge
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Chapter 6 Dimple-grinding
Using a GATAN 656 dimple-grinder, a sphere-shaped deepening is ground into the polished disk. The dimple-grinder consists of a specimen mount, on which the glass cylinder with the polished disk is mounted, and a dimpling wheel. For the polishing procedure, a suspension of diamond particles in oil or in water is used (oil is preferable, since it does not evaporate at room temperature). Depending on the brittleness of the sample material, the disk may be dimple-ground just from one side or from both sides. Dimple grinding the sample from both sides reduces the deformation of the surface; for very brittle sample materials, dimple-grind just from one side. The depth of the deepening should not exceed ca. 80 m for one-side dimplegrinding, and 40-45 m for two-side dimple-grinding. The remaining sample thickness in the middle of the deepening should have 15-20 m for silicon. For III/V semiconductors, 25-30 m is preferable, as these materials are rather brittle. The deeper the deepening is, the shorter will be the ion milling process afterwards. As for the counterweight, in the case of silicon 30-40 g, for III/V semiconductors 20 g may be applied; in metals 10 g could already be too much, because in metals dislocations are introduced very easily. See gure 6.1 for details.
Step-by-step:
- rst, center the glass cylinder with the polished disk using the binocular in such a way that the desired position of the later hole remains in the middle of the turning specimen mount - adjust the counterweight of the dimple-grinder; for brittle samples begin with a small counterweight (e.g. 15-20 g), then increase it slowly.
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6. Dimple-grinding
- stop turning of dimpling wheel and specimen mount - lower the cam control carefully (very left wheel on the side) - turn micrometer drive (left knob next to the specimen mount) counterclockwise, until dial indicator remains at zero (the zero point need not be identical to the zero on the dial indicator) - press twice zero - turn table wheel clockwise to set desired thickness of deepening; the digital dimple depth display is more accurate than the analog dial indicator - raise the cam control - put two 2 drops of grinding suspension (enough!) on the sample - turn on the dimpling wheel (arm) and the specimen mount (table); best clean the dimpling wheel with acetone - carefully lower the cam control, lowering the turning dimpling wheel on the sample - from time to time, raise the cam control, clean carefully both dimpling wheel and disk, add drops of grinding suspension, and lower the cam control again - if too much suspension is added, it may run in the inner part of the magnetic turntable or the dimpling wheel, thus, hindering the dimple-grinding; in this case, stop grinding, and clean everything carefully with a wiping cloth - if the sample contains a layered structure which easily delaminates, the disk may be positioned in such a way that the interfaces are parallel to the dimpling wheel, without any rotation of the specimen mount in order to prevent delamination
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6. Dimple-grinding
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7. Ion milling
Step-by-step:
- mount the dimple-ground sample on the PIPS Al sample holder (see gure 7.1) in such a way that the desired position of the future hole is centered (use the binocular) - for sample dimple-ground on both sides, the deepening at the lower side has to be smaller than ca. 40 m - for samples dimple-ground on one side, make sure that the dimpled side is oriented face up - make sure that the PIPS machine is turned on approximately 30 minutes before ion milling to reach stable, high-vacuum conditions - mount the Al sample holder into the PIPS - for layered structures, beam modulation should be used; make sure the layers are parallel to the marks on top of the PIPS - turn beam modulation on - close the cover, evacuate chamber - when the green light lights up, lower the sample holder into the ion milling chamber - set turning velocity, ion milling angle, ion milling voltage and duration of ion milling - start the ion milling process - the nal hole should be as small as possible
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7. Ion milling
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