SAMPLE PREPARATION FOR TRANSMISSION ELECTRON MICROSCOPE

By Engr.Nafis-ul-Haque(MM-10) Course code: MM-535

Department of Materials Engineering NED University of Engineering and Technology, Karachi

Refrences

ASM Metal Handbook Vol 10 http:/bama.ua.edu/~hsmithso/index.shtml G. Thomas and M.J. Goringe, Transmission Electron

Microscopy of Materials, John Wiley & Sons, 1979 Goodhew, P.J., Humphreys F.J, Electron Microscopy and Analysis, 2nd ed., Taylor & Francis, 1988. Loretto, M.H., Electron Beam Analysis of Materials, 2nd ed.,
Chapman and Hall, 1984. Williams, D.B. and Carter, C. B., Transmission Electron Microscopy, Plenum, 1996 Brandon, D. and Kaplan, W.D., Microstructural Characterisation of Materials, Wiley, 1999 or latest edition. Wachtman, J.B., Characterization of Materials, Butterworths-Heinemann, 2000 or latest edition

AIM OF THE SAMPLE

Form: Solids (metals, ceramics, minerals, polymers,

biological, and so on)

Size: An approximately 5-m-thick, 3-mm-diam disk Preparation: Bulk specimens must be sectioned and

electrothinned or ion milled to produce regions that

permit transmission of the electron beam. Powdered samples are often dispersed on a thin carbon substrate.

THE IDEAL TEM SAMPLE

Representative Thin Stable

Clean
Flat

The Ideal TEM Sample is

Parallel-sided Easily handled Conductive Free from segregation Self-supporting/or alternatively be able to support on various types of grids

Common Techniques for Initial Preparation

TEM SAMPLE PREPARATION METHODS

1. 2.

General Sample Preparation Mechanical TEM Sample Preparation

3.

Replica TEM Sample Preparation

1. GENERAL TEM SAMPLE PREPARATION METHODS

Dimpling
Dimpling is based on the mechanical action of abrasion. The friction of grains of a material harder than the object to be polished generates a dimple. Abrasion takes place in the presence of a fluid, which acts both as a lubricant and as a cooling agent.

Electropolishing / Chemical polishing

This technique is only suitable for conducting materials such as metals and semi conductors. Whether fragile or ductile, specimen must be of bulk type, compact and generally single phased. For some multiphased materials and in the presence of precipitates or segregations the appropriate polishing conditions can remain hard to define.

Ultramicrotomy
Sectioning a sample with the cutting edge of a diamond knife. The fracture is initiated by the knife and propagates parallel to the surface without disruption of the sectioned slice.

Cleaving
This technique is used for the limited materials and is relatively non-specific

FIB/ Ion Milling

It is common to thin specimens to electron transparency by bombarding them with energetic ions

SATGES FOR GENERAL TEM SAMPLE PREPARATION Initial Thining

Disk Cutting Desk punch

Pre-thining

Mechanical pre-thining Tripod polishing Sandwich Technique

Final Thining

Electropolishing Ion milling ultramicrotomy

Sample mounting

INITIAL THINNING DISK CUTTING

Starting materials is ground or sliced (cleaved) to slabs about 200 um in thickness Then the disc can be cut using ultrasonic disc cutter or the disc punch

Ultrasonic Disc Cutter

The Ultrasonic Disc Cutter is ideal for cutting TEM disks from brittle materials such as ceramics and semiconductors.

Sheet placed in punch

Ultrasonic Disc Cutter

Use an abrasive slurry of either boron nitride or silicon carbide

Disc Punch (mechanical)

The Disc Punch is ideal for cutting TEM disks from Metals

MECHANICAL PRE-THINING

The Dimpler provides with the easiest and most reliable means to produce many different types of samples for TEM and can be used on ceramics, many semiconductors, carbons, carbon composites, oxides, borides, silicides, glasses and many others. When prethinning, the Dimpler produces an ultra-high area for successful, artifact-free ion thinning, while maintaining a greater edge thickness to help prevent breakage while handling. The thickness achieved will depend on the material being thinned; however, hard specimens typically can be dimpled to less than 5 mm with a 100 mm thick.

DIMPLING

Model 656 Dimple Grinder

Concave dimple

MECHANICAL PRE-THINING
DIMPLER GRINDER

CONT..

Grinding wheel provides thin center and durable rim Pressure, speed, and depth of grinding can be selected by controls

Model 980 Precision Dimple Grinder

Stop at several m thickness

Dimple grinding of 3 mm discs is usually preparative to another more precise method of thinning, such as ion milling, chemical or electropolishing.

MECHANICAL PRE-THINING
TRIPOD POLISHING

CONT..

It consists in two main tools: a polishing machine and a specimen holder maintained by the operator. The low speed rotary polisher is fitted with a glass plate as a support for the abrasive disc. The glass or Pyrex specimen holder is adjusted by means of three micrometer screws (tripod). Polishing is generally carried out using a lubricant (water or other solvent).

Top view of the tripod polisher

Front view of the tripod polisher

Bottom view of the tripod polisher

SANDWICH TECHNIQUE
To protect the material surface while achieving a cross section. It also allows doubling or multiplying the observable material quantity in the same object. The specimen is cut to the desired dimensions. (1.7 mm wide, 5-10 mm long and 0.2-1 mm thick). A thin glue film is spread over each surface to be protected. A specimen-glue-specimen sandwich is formed when the two coated surfaces are put together face to face

Multilayer prepared as a sandwich prior to tripod polishing (1.5-1.7 mm wide).

Sandwich inserted into the metal ring.

Sandwich maintained by the transversal bars. Embedding resin appears in red.

SANDWICH TECHNIQUE

Schematic of a sample sandwich. The films sides of two pieces of the original semiconductor wafer are glued together. They are supported by two dummy pieces. The dummy pieces are usually scraps remaining from other wafers and are the same material as the substrate.

FINAL THINNING
ELECTROPOLISHING

Polish 1st side of Sample on Diamond Lapping Film until smooth Glue Sample onto Copper Grid Polish 2nd side of Sample until 10 m thick Ion Milling until 100 nm thick

FINAL THINNING

CONT

ELECTROPOLISHING

The most common technique for thinning electrically conductive materials such as metal alloys is electropolishing The principle behind the method is that the specimen is made the anode in an electrolytic cell so that when current is passed through the cell, the solution dissolves the alloy and deposits it on the cathode

major limitation of electropolishing is that it cannot be used on nonconducting materials such as ceramics and semiconductors

FINAL THINNING

CONT

ION MILLING It is common to thin specimens to electron transparency by bombarding them with energetic ions The ions knock atoms off the surface in a process called sputtering, gradually thinning the material. The ions used are accelerated toward the sample with an applied potential ranging from 4 to 6 keV at angles ranging from 58 to 208 from the sample surface, i.e., at a glancing angle Usually two ion guns are used so that the sample can be thinned from both sides simultaneously, and the sample is often cooled with liquid nitrogen to avoid excessive heating by the ion beams

ION MILLING
A focused ion beam (FIB) microscope is becoming popular for preparing thin membranes for TEM A FIB microscope is similar to a scanning electrom microscope (SCANNING ELECTRON MICROSCOPY) except that it uses electrostatic lenses to focus an ion beam on the specimen instead of electromagnetic lenses and electrons The ions are typically accelerated toward the specimen at 30 keV so that rapid sputtering of the sample occurs

Focused Ion Beam Milling

Schematic of sample after ion milling. The area bordering the hole is electron transparent. The hole crosses the film/substrate interface twice on each piece (four times total for the sample).

MOUNTING THE SAMPLE

Select stubs that are flat on the surface and do not have rounded edges. A step milled around the rim of the stub can protect the samples that project radially outward. Keep the epoxy that holds down the sample to the stub to a minimum. This makes it easier to remove the samples. A spot of epoxy is used as an index and to check when epoxy is cured. Use a Cut-down and a sharp pair of tweezers to break the sample from the stub. Use a normally prepared grid to mount the sample.

CRUSHING

It is applicable to materials in bulk or fine particles forms. It is essentially used to study ceramics, minerals and mixed composite materials. Materials must be fragile or rendered fragile, very to medium hard.

2.MECHANICAL TEM SAMPLE PREPARATION

CRYO-ULTRAMICROTOMY To make a thin slice of constant thickness (30-150

nm) with very soft materials that cannot be cut at room temperature. This technique has been improved by biologists and suits polymer preparation.

TRIPOD POLISHING

Polishing by gentle abrasive rubbing of a specimen with a slight tilt (0.3-0.7) to obtain an electron transparent wedge with smooth and highly polished surfaces.

ULTRAMICROTOMY Sectioning a sample with the cutting edge of a diamond knife.

The fracture is initiated by the knife and propagates parallel to the surface without disruption of the sectioned slice.

WEDGE CLEAVAGE

Fracture by cleavage along an atomic plane of the material. Cleavage uses the fact that crystals can split along weakly bonded planes. It depends on plane atom density and type of inter atom bonds. Cleavage is also made easier by the generation of dislocations at initial stage.

3. REPLIA TEM PREPARATION

When it is not practical or possible to put certain specimens into the TEM, the replica technique may be employed to examine surface features. Replicas may be negative (single stage) or positive (double stage) and a number of materials may be used to make these replicas. The materials and methods employed in this exercise are most suitable for non-biological materials or for hard, dry biological materials.

TEM Replica Types

Figure: Three replication techniques: (a) Direct carbon replica (b) Shadowed Carbon-platimun Replica (c) Two-stage plastic-carbon replica

Making Replica
A metallurgical specimen is generally first polished flat, in order to make the later lifting of the replica as easy as possible, and then etched. The specimens must now be washed and dried and the replication stage should be started as soon as possible to avoid the deposition of airborne dust which would contaminate the replica. A thin layer of carbon must now be coated onto the etched surface. This is generally achieved by using a carbon arc source in a vacuum coating unit.

Materials
Any of the solid material can be analysed in the TEM microscope, the sample preparation technique remain the same but the tools and apparatus may some time change Because some materials need special care for preparation like abrasive cutoff should not be used for low melting temperature material, it may alter the internal strucuture