Low-Voltage Microscopy When electron beams impinge on nonconducting samples a charge can build up which can make SEM imaging difficult or impossible By operating at low beam energies this problem can often be minimized or eliminated Charge balance Electrons cannot be created or destroyed so currents at a point must sum to zero. The current flow to earth Isc is the difference between the in and out currents Ib Ib Ib If the sample is a conductor Isc can take any value (+ve or -ve) to achieve charge balance sc Non-conductors For a non-conductor Isc is zero so charge accumulates Sample can accumulate negative charges or positive charges There can be a dynamic charge balance + - Complex materials In the case of complex materials (e.g. layered) then the charge balance must be considered separately for each component If a beam penetrates a layer then it will charge positively, a net electron emitter. SE BS substrate Imaging non-conductors On a new SEM this will be the lowest available energy On older machines you must decide how low to go before the performance becomes too poor to be useful for the purpose intended Set the SEM to the lowest operating energy Negative charging -ve charging E 0> E2 If the scan square is brighter than the background then the sample is charging negative Positive Charging +ve charging E 0< E2 If the scan square is dark compared to the background then the sample is charging positive Is that all there is to it? No - charging is a complex phenomena and simply running the SEM at a low energy does not guarantee an image that is free from charge artifacts To understand why we must look in more detail at what happens when a poorly conducting specimen is hit with an electron beam Mechanisms for Charging STATIC CHARGE Static charging depends on the net charge balance in the sample DYNAMIC CHARGING Dynamic charging comes from charge generated in the sample itself from electron-hole pairs There is no global condition where this term is zero Combining these two contributions we can synthesize a detailed model of the charging process Charge Distribution The net amount of negative charge injected = 1-. This is deep in the sample The net charge that is emitted = and gives a positive region at the surface Induced charge occurs throughout the interaction volume and could be of either sign Incident beam Ib +ve -ve Even at charge balance there is still stored charge and fields in the sample Conductivity and Charging The +/- charge separation produces a field which moves the induced carriers producing conductivity (EBIC) Traps reduce the number of electrons. If the escape time from the traps is >> than the time between electron arrivals so the charge buildsup. A charged region is therefore like a leaky capacitor EBIC is the key to dynamic charging effects dQ L Charge e Vbias Area A Ramo' s Theorem V V so work done e dx VdQ L L dQ V Thus I e . velocity dt L V V If velocity k . field k then by Ohm' s law R and L I L. A resistivity e. k force e. Surface Potential and Electric Fields The fields produced by even small amounts of charging are very high. This is seen as a drifting image -1.0 -0.8 2E5 -0.6 0 -1E5 3E5 4E5 -0.4 Thickness (m) It is these fields which deflect the incident beam, push the secondary electrons around, move the electron-hole pairs and may even change the yield of electrons X-electric field distribution with EBIC -3E5 6E5 -0.2 0.0 8.4E5 9E5 9.6E5 1E6 -1E6 -1.5E6 1.5E6 -2.5E6 1.6E6 -1.6E6 -1.1E6 9.2E5 1.2E6 -4E6 2.4E6 1.8E6 -2.2E6 -8E5 1E6 -3.2E6 -1.2E6 1.3E6 1.5E6 -9E5 1.3E68.8E5 -1.3E6 1.1E6 0.2 PMMA 0.4 0.6 -5E5 8E5 1.4E6 1.7E6 -3.9E6 1.4E6 -2.1E6 1.4E6 8E5 7E5 Cr -7E5 -6E5 5E5 -4E5 0.8 -2E5 9.7E4 -1.0 -0.8 -0.6 -0.4 -0.2 0.0 0.2 0.4 0.6 0.8 1.0 Position (m) Monte Carlo calculation of fields in and above a resist sample Minimizing dynamic charging Reduce the beam current as the charging varies directly with IB Change to Ultra-High resolution operating mode and lower the emission current Reduces S/N Dynamic Charging Reduce the magnification Dynamic charging depends on dose and on the magnification Limits resolution by limiting magnification Time dependent charging Dynamic charging is time dependent because of the leaky capacitor effect (EBIC) Scanning at a high speed extracts a signal before charging occurs The whole scanned area now floats to a uniform potential allowing stable focussing and stigmation Coating specimens Coating should be as thin as possible, a good conductor, and a good emitter of SE Au/Pd, Cr are good Carbon is bad (the filler contaminates ) and the evaporator heats the sample Coating is effective but may hide real surface detail May be only route if high beam energy is required e.g for EDS How coatings work Coatings do not make the specimen conductive They form a ground plane - eliminate fields due to charge Increase SE yield reduce charging Field deflects electrons Field deflects incident and exit electrons ----- ---------- 'image charge' NO EXTERNAL FIELDS ++++ +++++ ++++ coating ----- ---------- ground plane Charge in Charge in sample sample metal is equipotentia ground plane Result of coating Both Au-Pd and Cr effectively eliminate charging up to about 8keV Even at higher beam energies charge-up is minimal Thin coats do not affect EDS analysis Other options Heating the sample effective for ceramics, oxides etc Use a low pressure of a gas (VP-SEM mode or from a gas jet) Low energy electron or ion flood beam to neutralize the charging Use BSE detector for imaging- much less sensitive to charging Try different SE detector, mixed or upper Try high energy if sample is thin or on a substratedepends on what you want to examine Choice of detector The choice of the detector that is used can be very significant in determining how seriously charging will appear to be Try biasing the sample stage Try mixing the detector signals, or switching to the lower detector if possible S4700 TTL detector This detector is very efficient and gives a symmetric view These electrons are very sensitive to chemistry and to charging effects High energy SE, BSE, and SE3 are excluded from the signal - this improves contrast S4700 detectors Lower (ET) and upper (TTL) detectors on S4700 have different characteristics Lower (ET) detector accepts SE1,II and III as well as some BSE Upper (TTL) detector accepts only low energy SE1 and 2 SE spectra The upper detector accepts SE with energies around the peak of the SE spectrum. Peak position depends on amount of charge, chemistry, electronic structure, so these effects cause image contrast on TTL detector Lower (ET) detector accepts everything below 50eV. Much less sensitive to charging SE spectrum from Aluminum Nonconducting samples Latex paint at 1keV in Hitachi S4500 Uncoated, slow scan image at E2 energy 30kx original magnification Lower (ET) detector for topography, reduces visibility of charging Lower detector Individual polymer macro- molecules on a silicon substrate imaged at 1.5keV The lower detector shows little or no contrast Upper detector The upper detector easily reveals the macro- molecules This is because they are charging negative and the TTL detector is highly sensitive to charging effects Charging can be a useful form of contrast Doping contrast Chemical contrast in the SE mode Sensitive to both Pand N-type dopants Only visible on upper (TTL) detector Boron doping in Si 1.5keV Upper detector Birds-beak dopant contrast in a device S4500 at 1keV This is a unique imaging capability - 2 dimensional dopant profiling at high resolution and sensitivity (1ppm) Damage at low energies It is often stated that operation at low beam energies minimizes or eliminates beam induced damage From casual observation this may appear to be true, but measurements show that the truth is just the opposite Damage and beam energy At high energies the damage rate is low Damage rate rises as the energy is reduced, reaching a peak at about 100eV At still lower energies the stopping power falls again Experimental Stopping Power Data for Copper Damage while scanning If the beam is scanning then the rise in damage rate is less drastic but still considerable however damage is confined to the near surface and not spread through a volume