FOCUSED ION BEAM TECHNIQUE

PRINCIPLE

A finely focused beam of ions is made to bombard with the sample which in turn causes the sputtering of ions & electrons.

1. Detecting the composition of material.

2. FIB Deposition

3. FIB Milling & Lithography

4. FIB Imaging

1. DETECTION OF COMPOSITION OF MATERIAL

The FIB technique is used in ION MICROSCOPY which is a type of SECONDARY ION MASS SPECTROMETER (SIMS) to analyze the elements and isotopes of a material.

The secondary ions (approximately 1% of sputtered material) are accelerated into a mass spectrometer, where they are sorted by mass/charge to mass ratios with a large sector magnet. As shown in diagram, In a mass spectrometer, ions travel different paths through the magnet to the detector due to their mass/charge ratios. A mass analyzer sorts the ions according to mass/charge ratios and the detector records the abundance of each ratio.

A series of detectors counts the ions in different mass categories. Analysts take these raw counts, apply corrections, normalize them to well-analyzed standards to arrive at the true abundance of elements & isotopes in the original sample.

For an analogy, think of how a prism refracts and scatter white light separating it into a spectrum of rainbow colors.

The different components of an ion microprobe are numbered and colorcoded in this diagram. Ion beam paths are shown in white. Starting from the left, the primary ion column (yellow) provides the highly-focused ion beam produced from one of two sources (1,2). The sample (5, red) is located where the primary ion column joins the secondary ion extraction system (blue) wherein lenses focus the sputtered secondary ions into the mass spectrometer entrance slit (9, orange). The secondary-ion mass spectrometer (orange) is a double focusing mass spectrometer with both electrostatic and magnetic sectors. The electrostatic analyser (10) bends lower energy ions more strongly than higher energy ions. The ions then pass through the electromagnet sector (13) where lower mass ions are bent more than higher mass ions. Finally, the secondary ions pass to the sensitive detection systems (green), which include an electron multiplier for counting individual ions (19), and Faraday cup for measuring ion current (20). Ion microprobes also have the capability to operate in "ion microscope" mode, providing elemental and isotopic imaging capability at ~1 micrometer spatial resolution. The images are captured by an imaging device consisting of a channel-plate (17) and a fluorescent screen (18) in the detection system

VIRTUES

SIMS allows the in-situ study of microscopic grain in their native habitant in the sample unlike other types of MASS SPECTROMETER where sample is first vaporized. For example: in Extraterrestrial samples the grains are so small that it is physically impossible to separate them for standard MASS SPETROMETRIC analysis. SIMS can measure the ISOTOPE RATIOS with a precision of a part per thousand or TRACE-ELEMENT abundance at the part per million to part per billion level, while retaining the mineralogical context on a microscopic scale. This allows isotope ratio measurement on very small samples, such as sub-micrometer PRESOLAR GRAINS or COMET SAMPLES returned by NASAs stardust mission.

Modern SIMS can analyze and image small grains in place in a rock with impressively high mass resolving power.

APPLICATIONS
1. Geochronology. 2. Meteoritic. 3. Environmental pollution. 4. Hydrological tracers.

5. Pale climate.
6. Metals in coal. 7. Sedimentary rocks, diagenesis, weathering, soil science. 8. Volcanic ash correlations. 9. Elemental diffusion, partitioning, movement. 10. Petrology & economic geology.

11. U-Pb determination.

FIB DEPOSITION
The FIB technique is used in ION BEAM-INDUSED DEPOSITION (IBID) which is very similar to ELECTRON BEAM-INDUSED DEPOSITION (EBID) with the major difference that ions are used instead of beam of electrons, usually 30 keV Ga+, is used instead of the electron beam. In both techniques, it is not the primary beam, but secondary electrons which cause the deposition.

Micro-electrochemical cell fabricated by ion-beam deposition of Pt. Notice the horizontal branch connecting the inner and outer electrodes

Metal deposition to connect the metal lines

Gas Injection Nozzle on a Carl Zeiss N-Vision

PROCESS
The gas is introduced by a nozzle which is positioned a few hundreds of microns above the area of interest. The gas is then adsorbed on the surface of the material. When the FIB hits the surface, secondary electrons with energy ranging from a few eV to a few hundreds of eV are generated. These secondary electrons will break chemical bounds. The adsorbed gas molecules will separate into different components: some of which remains volatile, others will form a depo on the surface. When the beam has moved to other location, some gas molecules will again deposit on the same site where beam and hence increases the thickness.

Ion beam will again visit the same site and break the chemical bounds. this operation will continue till a specified thickness of material is deposit on the surface.

VIRTUES:

IBID is used in CIRCUIT MODIFICATION in ICs (integrated circuits). For example: when a deposition of metal connection is required, care should be taken for avoiding the shorting the surrounding signal lines. Such deposition requires a minimal distance of 300 nm in both x & y direction from the site of deposition. In circuit modification using FIB, the ion beam uses a Gallium and other special gases for the deposition and removal of metal connection.
FIB induced deposition

Diamond like carbon deposition (DLC): DLC deposition features high break down voltage (example >1750V for a 120nm thick film), low leakage and high hardness. These properties make it a suitable passivation material for high voltage devices. Ion beam process technology is used for depositing thin DLC films on magnetic heads in the magnetic recording industry. This technique meet the demanding requirements of ultra-thin carbon overcoats for current and nextgeneration magnetic recording hard disks.
HR-TEM picture, 200kV, elastically filtered taken by TU Chemnitz, showing the interface of a 200 nm amorphous DLC film deposited on a Si wafer at the OPT application lab

FIB in MICROFABRICATION: SiO2 can be deposited directly to form a required pattern by FIB fabrication. For example, in case of MICRO-CYLENDRICAL LENS (2.8*7.5 micro-meter, NA=0.2). A Ga+ ion beam with energy between 5~50KeV, a probe current of 4 pA~19.7 nA, and a beam limiting aperture size between 25~350 micro-meter. For a smallest beam current, the beam can be focused down to 7nm diameter at full width at half maximum. The accelerating voltage and working distances was 50 KV and 27mm respectively, and the chamber base pressure was maintained at 9.1*10^-6 Torr during the whole operation. The micro-cylindrical lens is composed of many deposited SiO2 films with rectangular shapes and different sizes, which corresponds to slices with discrete thickness in terms of sag of lens, in which lens was formed by covering layer by layer. Finally, the micro-lens can be obtained by POST-PROCESSING after completing the deposition of all layers, which are overlapped from top to bottom. POST-PROCESSING is crucial to form the final required shape with smooth surface. Percentage of Si and O affects the transitivity of micro-lens directly.

Without post processing

With post processing

APPLICATIONS
Failure analysis of semiconductors in semiconductor industry. Hard disk industry to manufacture DLC coated magnetic heads. Optical fabrication industry for making micro-lenses.
The ADVANTAGES of IBID over EBID are: 1. Much higher deposition rate 2. Higher purities. IBID has the following DISADVANTAGES as compared to EBID: 1. Angular spread of secondary electrons is larger in IBID thus resulting in lower spatial resolution 2. Ga+ ions introduce additional contamination and radiation damage. 3. Deposition occurs in a FIB setup, which strongly limits characterization of the deposit during or right after the deposition. Only SEM-like imaging using secondary electrons is possible, and even that imaging is restricted to short observations due to sample damaging by the Ga+ beam. The use of a dual beam instrument, that combines a FIB and an SEM in one, circumvents this limitation.

SPUTTERING (ION MILLING) USING FIB

WHAT IS SPUTTERING
It usually involves an inert gas plasma, e.g. Ar, where the Ar+ ions are accelerated onto the substrate at high KEs. When the ions strike the surface atoms, momentum transfer takes places, and the atoms are knocked out of the surface and into the gas phase, where they are pumped away. This process is called 'sputtering'.

ENERGY LOST IN COLLISION CASCADE.

ENERGY FROM COLLISIONS NEAR THE SURFACE RESULTS IN LOW ENERGY SPUTTERED PARTICLES.

For the purpose of sputtering, energy band from 100 eV to 5000 eV is usually used. (for ion implantation, energies up to a few tens keV may be used)

The gallium (Ga+) primary ion beam hits the sample surface and sputters a small amount of material, which leaves the surface as either secondary ions (i+ or i-) or neutral atoms (n0). To measured the depth of the boxes an atomic force microscope (AFM) is used. The milling yield depends (mainly) upon 4 things, viz: 1. Angle of incidence: The milling yield of Si and SiO2, for example, increases by a factor of seven to eight in going from normal incidence at 0 to 7585. 2. Current: At low primary beam currents, very little material is sputtered. At higher primary currents, a great deal of material can be removed by sputtering. 3. Time of scan: For particular scan speeds at normal incidence, each pass of the beam removes a thickness of material, if the scan speed is lowered, the the thickness removed per pass is increases.

FIB SPUTTERING in SEMICONDUCTOR DEVCICES: FIB can be used to cut unwanted

electrical connections with applying a mask (called photoresist) to surrounding area to be protected from etching. For example: a prototype circuit for an acoustical transducer that require modification.
Fib cut through the SiO2 dielectric exposing the buried metal.

FIB TEM PREPARATION PRE-THIN METHOD

The FIB is commonly used to prepare samples for the transmission electron microscope. The TEM requires very thin samples, typically ~100 nano-meters. Some critical requirements and restrictions on tem preparation are: Locate the area of interest, FIB deposit a protective Tungsten layer, Mill initial trench & rough polish, Thin the central membrane, Perform frame cuts on central membrane, Polish mills to near nominal thickness, Polish for electron transparency of membrane, FIB mill to free membrane from trenches. The final size of the electron transparent cross-section varies, but can be as large as 150 square microns to as small as 45 microns squared.

FIB AFM cantilever tip apex modification FIB technique is also used to modify the tip apex of cantilever used in AFM. As shown in following 7 figures, 1. A hole is milled at the center of the tip from
backside, 2. A Pt pillar is deposited to fill the hole, 3. A Pt line is deposited connect the pillar & reach the cantilever level, 4. FIB clean the tip from Au coating, 5. A trench is milled at apex, 6. a Pt pillar, actually doughnut shaped, is deposited onto the trench, 7. FIB is aligned along each of the pyramid sides to shape the metal electrode into a tip.

Production of an AFM tip on virtually any surface. FIB deposition of TUNGSTEN or SILICON OXIDE 200 nm or thinner with aspect ratio than can exceed 50:1 (left). Subsequently these columns can be FIB machined to a point (right) with a radius of curvature less than 40 nm (inset at 0 degee tilt).

FIB IMAGING

Topographic contrast. Ion channeling contrast for grain size measurements. Secondary electron and ion images. Material contrast local composition differences (secondary electrons and ions). Voltage contrast electrical state differences. Passive and active voltage contrast(secondary electrons).

TOPOGRAPHIC CONTRASTS

ION CHANNELING CONTRASTS FOR GRAIN SIZE MEASUREMENTS USING FIB (ION CHANNELING): Ions penetrate
deeper in crystalline, material for certain grain orientations. Secondary electron yields are lower for areas that channel better than adjacent areas. Polycrystalline materials have grains with different orientations. Grain size can be determined by image at different angles.
Section of nickel, grain structure and porosity can be seen

SECONDARY ELECTRONS AND IONS IMAGES

REVEAL SURFACE STRUCTURE using FIB & SEM: dual plat instruments, a primary ion beam hits the sample surface and sputter a small amount of material which leaves the surface as either secondary ion or neutral atoms . The primary beam also produces secondary electrons. As the primary beam raster on the sample surface, the signal from the sputtered ions or secondary electrons is collected to form an image.

Expose cross-section with FIB. View cross-section with SEM.

MATERIAL CONTRASTS

SECONDARY ELECTRON

SECONDARY ION

VOLTAGE CONTRAST

Open contact in chain shown by charging.

Bridging open contact with metal deposition indicates remaining contacts are good.

ACTIVE VOLTAGE CONTRAST static biased VC: SRAM cell logic gates

LOGIC STATE 1

LOGIC STATE 0

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