SCANNING ELECTRON MICROSCOPY/1976 (Paxt III) Proceedings of the Workshop on Techniques for Particulate Matter Studies in SEM IIT Research Institute Chicago, Tllinois 60616, U.S.A. i april 1976 ee MULTICOMPOSITIONAL PARTICLE CHARACTERIZATION USING THE SEM-MICROPROBE 6. Grantl, 5.8. Hail”, A.F, Reid! and M, Zutderwyk? Division of Mineral Chemistryl CSIRO, Box 124 Port Melbourne, Vic. 3207, Australia Julius Kruttschnitt Mineral Research Centre’ University of Queensland \ustra: ABSTRACT An essential requirement for an understanding of industrial proc- esses such as mineral beneficiation is the classification of multicom- ponent particles by size and composition. To measure these parameters for samples consisting of whole particles or for polished cross-sections of multicomponent materials, a digital scan system has been constructed which, under mini-computer control, steps the electron beam over the specimen to generate the necessary data. Algorithms in the computer program treat these data to provide the geometrical properties of each particle component. Particle size and compositional distributions, aodal analyses and the statistics of “coupositeness” of the populations are then ed. Self-generated raster patterns from 20 x 20 to 4000 x 4000 points or computer controlled specific patterns are available from the digi scanning unit. Dwell time per point can be ted from 10-7 to T sec- ond. Digital values of the X and Y beam co continuously imen until eight-bit composition code and the beam coordinates memory. Each inage ie recorded as a compressed digital map of Line segment and points To reduce the total area to be scanned in detail rectangles bounding each particle are determined by an initial fast scan. This strategy also minimizes the size of data arrays. Once all particles within a frame have been examined, the specimen stage is moved under program control to centre the next search area under the beam. The software strategy ensures that all particles on the search boundaries are located, and thereby en- ables the examination of specinen areas large conpared to the SEM frame size. The algorithms determine the particle parameters by linking over- lapping run lengths on adjacent raster lin meters, moments and bounds for each partic: are compiled in FORTRAN IV and are linked to the be: tion driver, programs incorporated in the assenbly language operatin system of the mini-computer. The programs occupy in all approximately Lek of 16-bit word: Digital Scanning, Image Analysis, Scanning Electron Microscopy, Particle Dimensions, Particle Composition, Mineral Particle Classification, Stereology KEYWORDS 401MILTICOMPOSITIONAL PARTICLE CHARACTERIZATION USING THE SEN-ICROPROBE G. Grant , 5.5. Hall , A.P. Reid and M. Zuiderwyk Introduction ‘he determination of the sizes and composite iona of complex particles, aa well as their peri- meters and shapes, is a primary requirement for an understanding of the physical and chenioal behav- sour of particles in industrial and mineral treat~ ment processes. This topic is the subjectlof ex- tensive Literature, but automatic methods of part icle classification yielding compositions and data in even two dinensions are not yet common, nor of General application and reliability. The use of igital images obtained, preferably on-line, from ‘the SEM has been considered for sone years (1,2). Jones and Shaw (3) have used signals from a micro- probe to determine intercept lengths over sect- joned particles, and this data has been inter~ preted (4) to obtain estinates of particle prop- erties Wnite et al. (2,5,6/7) have developed the use of the automated SEN for the measurement of sizes and chemical composition of vhole particles. However, their systen requires considerable off- Line computer capacity, and the image must first be stored on magnetic tape. For our purposes, ‘the prograns described do not cope with the rath er complex problen of composite particles, nane- ly determination of the exposed areas of differ~ fent composition in multicomponent grains. ‘The statistics of such distributions are of particular inportance in mineral flotation and in the determination of the degree of Liberation of minerals during grinding or similar operations. ‘The determination of areas in grain mounts and “whole-rock" samples is also needed for ore and mineral assessment. To treat these various problens a systen vas required which would alloy digital imaging of sample areas many tines larger than SEM frane size, and with the option of treating the data on-line in a mini-conputer. Measured rather than inferred areas and perimeters were sought, ‘$0 that shape functions, as for example des- cribed by Davies (8), could be derived, Tt was also required that the beam coordinates be add- ressable by software, and that manual setting and checking of control paraneters be available. ‘The system developed, satistying these requirements, 4s the subject of this paper. Bean Scanning system ‘The electron beam position is controlled by two addressable 12-bit D/A converters, which provide a step raster of 4000 x 4000 points. 402 ‘The converters are driven by a 10 MHZ digital pulse generator, vhich linits the dvell tine Per point to a minimin of 10-7 seconds. ‘The dwell tine can be extended to a maxinun of 1 second, and dwell points can be spaced fron 1 to 200 steps apart. Reduced scan limits tnt Faax’ Yain’ Yang) 29 A180 be set, These various paranetars can be software or front panel controlled, Figure 1. The X and ¥ positions of the beam are continuously displayed. Aa well. as being driven in free-running raster node, the bean may be explicitly positioned by software for beam patterning, which enables generation of sampling patterns about given.or detected features of the specizen. ‘The scan control operating paraneters,in hexadecimal form,are contained in four 16-bit words loaded on to a 64-bit buffer at the bes- Anning of each frame scan. Once this control buffer ie loaded, the scanner is free-running until halted by “Line-end", "Frame-end" or a change in status of the signal channels. The bean stops and the scanner Interrupts the com, puter. The X-nd ¥ hexadecimal bean coordin- Bees and an a-bie digical pateern, cepreseatiog ‘the status of the signal channels, are read into the computer in a total of 32 bits. This S-bit status patter ds the result of 2 analogue and 5 X-ray discriminators having found a particular grey level or particle composition. In the us~ ual mode of operation, the ¥ coordinate is not stored. A digital acceptance filter can be set so that a change to « new signal channel status must be verified for 1, 2, 4 or 8 successive ‘steps before causing the scanner to halt. This facility rejects noise signals, and ensures that composition boundaries have been correctly re- cognized. Hexadecimal data transfers are used throug out to increase operating speed, reduce soft~ ware overheads and to provide the correct format for assenbly Language logic and arithmetic. Image storag ‘The image is stored as a Linear array of x and if required, ¥ coordinates, with associated ‘composition codes. Usually the Y coordinates fare inferred from the end of line stops (7), and the number of steps per line is Limited to 256, 0 that the inage can be stored as a simple se~ quence of 16-bit words, with one S-bit byte re- Presenting the X coordinate and the other the composition code. The location of the words in the array give their index value.Figure 1. Digital scan control for SEM bem. A. Frame. Scan paraneters: step size, novread interval," C. signal channalat fnateator swieche ‘of K and ¥ beam coordinates and frame limita, " S. . ee ‘Thusbwheel mvitches for manual setting of reduced jell tine, frame, line, sing Rows 1-5, x-rays ‘colums 2 and 3, selection indicators and switches. D. Signal is accepted only after 1, 2, 4 of 8 positive indications. E. repetitive, read length, rows’ 6-7, analogue. Column 1, interrupt Digital acceptance filter ‘Visual atsplay ‘This data format is used directly, without unpacking or reconstruction of the image, in the perineter and area algorithas. This imediate Utilization contributes considerably to mint- mizing computational tine and storage require Signal Processing ‘he three available analogue channels aco- ‘opt the outputs from any of the secondary elect- ron, backscattered electron, or absorbed current Getectors. Non-linear amplifiers and upper and lower level discriminators are used to select. the voltage "window" corresponding to signale from a given chemical phase. If required, the sane detector signal can be fed to all three channels simultaneously to give a total of four levels of discrimination (0 1, 2, 3). Diacrim Snator tine constants are sat at 10-4 second. the X-ray detector channels consist of eight presettable overflow counters, which can be used Separately, oF in pairs to provide upper and low oF level discrimination. Dwell ties for sufficient X-ray counta vary from 10? to 107} seconds. are urually derived from an enersy dispersive Getector, but are also available from the crys: tal spectrometers fitted to cur microprobe = SEM. Any shadoved areas vithin particle boundar sen, reglatering as background, are assigned to the major compositional fraction by the sub- sequent softwar For a given element, count rates and dvell ‘tines are chosen by the operator, and minimn count values required during the dwell tine are set manually on thumbwheel svitches, prior to 403 Particle imaging. The beam scanner has provis- fon for repetitive scanning of a single line, alloving the operator to adjust threshold volt- ‘age levels of count rates to suitable values by Inspection of known standarde or features in the samples. Once thresholde are set, ond scanning is begun, a change of signal status 1s registered if one of the values obtained differs ‘from the value observed at the previous beam position. Such an occurrence halts the Deas Scanner, which then sends an interrupt to the couputer for transfer of X, ¥ and composition values. Signal processing is thus kept inde- Pandent of the control functiona of the computer. pectnen stage X-¥ control ‘The X and ¥ stage positions are controlled by stepper motors with gearing ratios which give an X of Y displacenant of 1 aicronetre per motor Pulse. ‘The stage displacements are digitized by the number of motor pulses with respect to a zero position. Pulses are counted by up-down presettable counters, and the "present™ position fa continually compared with the value Loaded conto buffers on the motor control interfaces Vien the requested position Is reached the motor stops. Ag with the beam gcanner, the motor novenents are independent of the computer. This control system is described in more detail in reference 9. Softvare supervisory Systen In our control programs we have used the IWTERDATA 70 operating system with all redundant routines renoved, but with additional software Grivers which are specific to the various dev- terthe softvare contra} progras, shich gen- exaten the necessary parameter words for the Sean tcanner and notor controllers, and which ends" fon the scanner the coordinate and’ com Position inforastion, adresses the sofeare” Eriver routines by neane of the inetraction, oe avaliable an the anverdata Aasenbly tang * Sige.” than the inage analysis precediree for "Sivan Glemtion ara independent of the soar tefvand stage control driven sovtineai'and any enaily be Felonded with a variety of prgrane. Frovielons for Linking FOREMAN roveines, Sapited CEE"line ace included in cur eperstiog syetan. Qperationsl Procedurs once signal discrininator levels have been set, and the firet frame of the specinen aren has been located, the beam is stepped at the highest useful speed over the vnole frane area, using a relatively coarse raster. An electron Signal channel locates the edges of particles without specific reference to composition. The Fesulting X-coordinates are then treated by the perineter algorithn to determine the location of ‘the rectangles bounding each separate particle in the frane, Figure 2. The position of these rectangles 1s related to the zero point of stage ovenent with a precision of #1 micrometres, ‘the reproducibitity of our automated stage. Bach rectangle, enlarged by one or two stops widths, is then scamed as slowly and in as much detail as is necessary, using discrim- inated secondary electron or X-ray signals. For many purposes, a raster of 50 x 50 steps per rectangle gives nore than adequate inform ation. The particle is closely bounded by the Fectangle, and sone 1200 “on-particle™ points would be expected. In the systen described by Troutnan et al (7), the beam is driven along a frane Line at. high speed until a particle edge is located, ‘and then svitched £0 slow speeds during the traverse of a particle. Our system enables 8 comparable saving of tine but additionally reduces very considerably the anount of data Storage required. Pull information for each particle is retained and the data arrays are Small compared with whole frame arrays. Adopt- fon within each rectangle of short and long dvell times "off" and "on" the particle, would hovever enable a further saving of time, and is being investigated. once the set of Local rectangles within the whole frane has been fully treated, the stage is moved to bring the next sample area under the dean. This movenent ie less than the scan frane by the maximum expected dimension of the largest particle. This procedure effectively re-exan- ines a band around the trailing X and ¥ edges of ‘2 search area delineated by stage movenent, Figure 2, and ensures the inclusion of every particle hen all of the sample area is exanined. 404 If a particle near a frane edge is relocated dur- ing the high-speed scan of an adjacent frane it ds soft-ware rejected and not re-exanined in detail. When search areas are spaced out so as to obtain only a statistical sampling of the vhole area, particles vholly within the overlap band are rejected, while particles on the boundary between "search" and overlap area are accepted. ‘This procedure ensures that the statistical size distribution is not skewed . ‘This approach differs fron those in which particles cutting frames are simply given areas Gouble those cbserved, or a snali frane enlarge ‘nent is added in one direction only. Jmage Analysis Prograns and Algori thas Particle area and perineter determination are treated as discrete operations based on al~ gorithms which manipulate the digital inage data for the scanned frane or the rectangles which contain individual particles. These computat~ onal operations can either be part of the data- gathering program, or can be performed off-line, ‘They are writeen in ANSIT-standard FORTRAN but versions of the routines are now being written in assembly language to increase the speed of Processing in the mint-computer. Details of the algorithms and programs will be given in ‘8 separate publication, and only the main points fare discussed her ‘The approach finally found most useful is to determine and label firet the connected bound- ary points of the particle, and then to determin the area. ‘The perineter algorithm takes advantage of the Linear nature of the information array, and from the run lengths defined by the X-coordin~ ates for ON and OFF the particle for a given raster Line, overlaps between isage Lines are Getermined, Consideration of the relationships for a particle boundary cutting or not cutting across. two adjacent raster lines gives three potsible topological cases vhich are: simple concave change of direction; oF convex change of direction. Taking these sit ‘ations into account, consecutive boundary coordinates are connected vectorially until the Doundary is closed. Area is then obtained by ‘summing up the run Lengths between adjacent. labelled locations on the sane raster Line, with ue account of individual compositions, and the contributions of the total run lengths to the Hirst moment about the X and ¥ bounds of the particle are also sumed. These latter values Lead to a simple determination of the X and Y coordinate values for the centroid of the part- ele in ite two-dimensional projection. If required, the perimeter contributions of each of the different conposition types forming the boun- dary can be separately sumed.Visual Display of Particles: As the boundary coordinates of particles or sub-areas are located, the successive (x,¥) pairs around the boundary of their indexed manory loce ations, are stored in an array separate from that containing the raster information. For @isplay, pairs of coordinates are loaded se- 7 quentially onto D/A converters, and the result-.. ing X and ¥ analogue voltage values can be directly applied to an ordinary oscilloscope ‘Alsplay. A perimeter defined by 200 points loaded into the D/A nodules at one transfer per millisecond produces a flicker-free display vith ‘2 phosphor having a .25 second persistence. Such a rate of data transfer poses no problems for a miniconputer interfa ferineters of sub-areas can also be displayed in a similar anner, and we intend to install a 3-color Gieplay monitor so that particle and sub-area outlines can be shovn in different colors. ‘mis aystem of data display obviates the need for the very fast data streams necessary for TV raster refresh rates, and simplifies the @isplay equipment required. We believe that our perimeter determination and storage 1s of particular value for this reason. he aigoriehme which we have developed can be applied to the digital inages of any discrete objects, elther mlcro- or nacro-sized, provided that their boundaries are defined and’ continuous, With the aid of an SEM, particles, particle cross-sections, cross-sections of ‘continuous agglomerates such as fine-grained ores, or the pore holes in sections of ceranics, can equally Well be characterized. ‘The algorithms are also applicable to mth spectral optical images, such as those of blood cells (10) oF those obtained using 3-color 7V ‘scanning of inage sources in general. Sample Mounting Techni In determinations of particle characteris tics, sampling and sample mounting is of import~ ance if unbiased information is to be obtained. By using the present measuring procedure, which either examines all particles on a mount or ‘hich examines spaced areas without overall bias, the problem of obtaining a uniform dist- ribution on the mount is largely removed. For flotation concentrates ve have found that a sample of particles spread onto a filter paper can be mounted on a flat surface such as a carbon or aluminium block, aluminized glass of beryllium sheet by smearing a very thin layer Of epoxy over the surface of the mount vith the edge of a razor blade, and then pressing the 40s inverted mount onto the samples For sectioned grain mounts, our major pre- ‘cation in sample preparation is the use of the nifieragraphic technique of placing the sample “mould in an evacuated chanber imediately after mixing or pouring in epoxy, so that air entrain- ment and subsequent formation of holes and the Plucking of particles during polishing, are sinimized. Mounts containing whole grains on a flat yurface are carbon coated vhilat rotating to ‘endure coating of all exposures of the particlé ‘The nounting of particles for SEM eranin- ation is a subject treated in detail by sever- ‘al authors (11) and in our vork we have essent- Aally folloved such published techniques. Stereology of Particles ‘The backscattered electron detectors in our SEX give a view of the particles normal to the pounting surface. This introduces obvious ste: Logical bias if the particles are mounted on thelr Largest faces, and a second set of detect~ ora to give biaxial vievs will be fitted around the collimator of the energy-dispersive X-ray detector. As vell as giving the sane View for X-rays an for backscattered electrons, this will allow better estimates of particle sizes in three dimensions (12). Im order to obtain estinates of the probab- Alities of cbserving the different compositional ‘areas on random particles, we have mounted a number of particles on a small goniometer, and have obtained digitized images of ope normal axis view and five oblique views at a 60° angle fron ‘the normal, spaced 72° apart around the normal axis. The results of this analysis will be pub- Lished in the future, Many stereological problens renain to be solved, but it is expected that with the iner- ed ease of obtaining sufficient 2-dinens: ional statistical data, and with the particular parameters vhich we are able to obtain, namely intercept lengths, areas, true perimeters, or- dered perimeter arrays, centroid positions and the dimensions of the rectangles bounding the particles or positeness distributions can be developed. Retults ‘The automated scan control and data acqui ition “hardvare” and the necessary software control prograns are fully operational. Timing tests shoved that the operations involved be tween halting the beam, interrupting the com puter, transferring the beam position and con position code values to menory, and restartingthe bean scan take a total of 2.9 milliseconds. ‘mis Includes a deliberate hardvare delay to allow discriminators to settle, and a software olay to alloy reliable loading and reading of the buffers, Tt also inclodes the tine taken by the operating systen to perform all necessary vapidtey ‘checks. "in fallablliey tests, up to sequential interrupt and data transfer cycles vere performed without ezror. ‘The algorithms and prograns to determine perimeters, areas and centroids perform reliably and rapidly Off-Line in FORTRAN, and in the COC 7600 system to which we have access, computation tines are fractions of a second per particle. hen the programs are used on-line in our INTER- DATA 70 system for a particle as shown in Pig~ lure 3a, occupying a 50x 50 raster image, the perimeter and area computation taki Ly 8 seconds. It is expacted that this tine will be considerably reduced once the programs are vritten in assenbly language. Signal processing provides most of the re maining problems in the data acquisition system, especially vhen vhole particles with rough sur~ faces are being examined. The backscattered electron signal particularly ie affected by auch roughness, and discrininator levels are sonetines aitticult’to set. This aspect of our system 1 being further developed. In general, digital inayes of moderate - stzed whole grains, and especially of sectioned exposures, are readily obeained, and a typical ‘example of an inage from a whole grain is shown in Figure 3. The raster spacing ie that used for data acquisition. Much more finely detatl~ fe4 inages can be formed by the 4000 x 4000 raster wmode, which in fact provides higher spatial dis: crimination than it is possible to reproduce on the 1000 line Ckr fitted to our SEM. ‘the paraneters derived for the particle ‘shown in Figure 3 are given in Table 1. Apart from this dizect numerical information a nunber of further paraneters can be derived, such as fitted equivalent ellipses; perimeter to area ratios and ratio functions and Feret's diameters land average chord lengths, Information such Second moments of line intercepts, touch points of the particle on the bounding rectangle, max~ imum chord in the X-direction and the number of upward or downward convexities or concavities ‘can also be obtained within the program. Th particular, the intercept lengths and moments Fequired for the stereological Interpretations used by Jones and Barbery (3, 4) would be a sub- ‘et of our information. Such easentially one~ Ginensional data requires severely limiting ass- unptions for its interpretation, and directly Getermined areas and perineters carry far high fer inforaation content. In the present paper we have described our autonated SEM control system, and the treatment 405 of the digitized SEM inage to obtain particle pare wnatars. ‘The application of these measurement techniques to suites of samples, and the further development of the perineter - centroid relation- ships to give shape information such as is dis cussed by Davies (8) will be the subject of fature publications. Acknowleagenen te ‘The authors express their gratitude to 1, G. Dorfler and J.C. Ruse, "A system for Stereonetric Analysis with the Scanning Electron Microscope", Scanning Electron Microscopy/1970, TET Research Institute, Chicago, Illinois, 67=72 (4970). 2. BLM. White, 6.6. Johnson, Jr. and KA. Mexinstxy, "Computer Processing of SEM Inages", Scanning Electron Microscopy/1968, IIT Research Institute, chicago, flinois, 95-103 (1968). 3. MP. Jones and J.L. Shaw, "Automatic Measure- inant and stereological Assessmant of Mineral Data for Use in Mineral Technology", 10th Int. Mineral Processing Congress, MJ. Jones (E4.), The Institution of Mining and Metallurgy, London, 1974, pp. 737-75 4. G. Barbery "Determination of Particle size Distribution from Measurements on Sections” Powder ‘Technology, 9, 231-240 (1974). 5. BM. White, HM. GSEz, G.G. Johnson Je.» and Rig, MoMillan, “Particle Size Distributions of jarticulate Aluninas from Conputer-processed SEM Images”, Scanning Electron Micros Research Institute, Chicago, 49°64 (1970). 6, E.W, white, K. Mayberry and G.G. Johnson 1 “Computer Analysis of Multichannel SEM and x-ray Inages from Fine Particles.” Pattern Recognition, 4, 173-193 (1972). 7.8: Troutman, G.G. Johnson Jr., £.W. white and J, Lebledzik, “Automated Quantitative SEM Characterization of Complex Particulate Samples", International Laboratory, March/April, 1974, 11-26. 8. _R, Davies, "A Simple Feature-space Rapre- sentation of Particle shapes” Powder Technolozy, 42, 1ni-iz4 (1975). 9. Avr. Rold and M. Zulderwyk, "An Interface System for Minicomputer Control of Instruments and Devices” CSIRO Mineral Research Laboratories, Division of Mineral Chemistry, Investigation Report 115, August, 1975. (available through CSIRO, Box'124, Port Melbourne, Vic. 3207, Australta)407 Figure 2. Schematic of search and scan proced- re for particle location and examination. Search areas are defined by stage movenents Ox, OY, and the scanned area by OX,, O¥;. The overlap dimensions X,-X, and ¥,-¥, are set at. the daximm chord of the largest particle. All particles within the frane are located by an initial fast scan and the rectangles defining their minina and maxina are determined. Those cutting the frane, e.g. 1 and 6, are not exan- {ned further. Those on the bousdary of the overlap area are always included, but when spaced out rather than adjacent areas are examined, particles wholly within the overlap band, such as 2, are omitted ‘TABLE 1 (COMPUTED PARTICLE PARWMETERS” SAMPLE BOUGATNVILLE 7-73-106 PRAME 1 PARTICLE e RECTANGLE Location x 210 Locarrow 320 DIMENSION x 50 DIMENSION ¥ “ wo. oF cHoRDS 39 MAX x CHORD as xKIW 3 XMAK 2 YIN 3 YHAK a cENTROID x 26.6 CENTROID ¥ 2215 PERIMETER 142.5 AREA 1267 SUBAREA TYPE 2 67 Figure 3. (a) Rastar image of a quartz-chalco- pyrite composite particle obtained with back- Scattered electrons. PW = 50 um. () Digital sap of image (a). 1= quarts, 2= chalcopyrite. 1 character space = 1 ym.” In the computer array, only the coordinates of each change of position are stored.10, 1. Young, “Localization of cellular Structures", IEEE Transactions on Bicnedical Engineering, EME~22, 35-40 (1978). AL. 0. Jahari and P.B. DeNee, "Handling, Mounting and Examination of Particles for Scanning Electron Microscopy" Sc ‘Scanning Electron Microscopy/1972 TIT Research Tastitute, Chicago Hilinois, 249-256 (1972). 12, ELE. Underwood, “quantitative stereology” Addison-Wesley, New York, 1970, P. 264-246," 13. S.B, Gray, “Local Properties of Binary Images in Two Dinensions™, IEEE Transactions on Computers, 6-20, 851-561, 1971. "computer Processing of 60), 14. H. Freeman, Line-Drawing Taages", Computing Surveys 57-97 (1974). DISCUSSION WITH REVIEWERS Reviewer ysis How ong does a full picture ana- Authors: This tine is a simple mitiple of the tine per particle. defining fairly complex particl dvell tine per point for back-scattered electrons (BSE), the recording tine is 0,25 seconds. For x-ray, with a dell tine 2x10" seconds, record~ ng tine is 50 seconds. Computing tines have so far boen tested only for single, although com- plex, particles. With 50x30 raster envelope, Gnilne computing time in compiled FORTRAN was B seconds (off-Line on a CDC-7600, the tine was Jess than 0.2 seconds). We are still testing the overall procedure for multiple fields of particles. Computing tine per particle is ‘essentially proportional to the number of raster Lines. For simpler composite particles on a 20x20 ‘raster, 20 msec dwell time, and about 2 seconds computing time, we expect that 100 par- ticles will take approximately 1000 seconds for x-rays and 280 seconds for BSE. Reviewer IIT: Can you specify, beam current, ‘spatial resolution, number of fields, number of particles and the type of output that will be Obiained tor a specific problem. Bean currents are typjeal bac ed electron imaging values, 10°® to 10~ Spatial resolution is dependent on edge ness, and on the nature of the electron response. The digital scan system can resolve secondary electron images dovm to the ultinate resolution of the SEM, at least 100%. For fields of 10 to 1000 microns diameter, the spatial reproducibility as judged by beam tracks impressed in electron resist materials, is essentially within the 3 bit resolution of our high-stability 12 bit D/A convertors, i.e, 21 in 8000. The nunber of fields can be made as great as desired. Fields are obtained by automat stage movenents which bring successive sample 408 areas under the beam centre. The contents of each field are examined, and their paraneters ‘computed and printed (or stored) before the next field is examined. The nunber of particles which can be outlined for subsequent exanination is as Nigh as the computer storage will allow at four coordinates per particles. The output is as given in Table 1 Reviever II: What statistical results can be ‘outinely obtained? Authors: For each particle, parameters are ob- tained as given in Table 1.” Statistical distri- butions for suites of particles are obtained from the populations of single particle paraneters. Reviewer II: Can all the additional parameters you mention be derived from the data? Authors: Yes. Reviewer III: What criteria are used for proper Setting OF discriminator levels? Authors: Of the three methods described by Morton ‘{GSTH Publication STPS04, 1972, pp.£1-94) wo use manual threshold setting at the $04 maximun-nini- mun value as displayed on a vaveform nonitor dur- ing a line scan. The entire inage is then check- ed'for spatial fidelity in teras of an undiscri- ‘inated inage. The inage, rather than the dis- crininators themselves, is used as the final Selection criterion for threshold settings. hadowed areas" determined? Reviewer I: How are " Authors: A shadowed area is recorded as back- round by the detectors, but is recognized by Software as lying within a particle boundary. Its area is either added to that of the major compo- nent, or is determined if holes are actual f ‘tures of interest. Reviewer III: What particle configurations are now al ‘Authors: Any configuration is allowed, provided that ft has a recognizable boundary. Touching particles of the sane phase can be discriminated only if there is a region of contrast at the con- tract, as usually occurs in secondary electron images. Touching particles of different phases are discriminated as a matter of course, lioles t affect ina particle are recognizable and do ‘the outcone. They can be treated as subareas, or equated to the major particle composition. Discussion continued on p. 450.Additional discussion of paper on '‘Multicompositional Particle Characterization Using the SEN-Microsprobe"" by G, Grant et. al., continued from p. 408. Reviewer I: what are statistical limits and fests deteraining whether an element is present or absent at a given raster location? Authors: The 90% confidence level is taken as veak)% - 2(Background)” > (Background), where Peak and Background values are initially’ deter- ined from counting tines mich longer than dwell, times. The acceptance level is then set in terms of a dwell tine and overflow counter value, and the inage is tested with these values. If Correct spatial definition is not obtained, dvell times and overflow values are increased. Reviewer IT: Is it not the case that two BSE jetectors cannot give stereo pairs? Authors: This is so, and the two sets of BSE detectors will be used to obtain two distince views of the sae particl Wat acguracy of beam positioning 10-7 sec. dvell time and 20x20 point density? To ay knowledge no comercial SEM can handle that speed, or even close. If the time constant of apalog discriminators is set to fixed value 10°45, why vould one change the dwell tine toa value different than 1045 or so,since this gives the optional filtering of the analog signal? For exazple, 10-7 dwell tine will be totally useless since at best at 4009 points per line, the line tine will be 4x10" (or 10-7x4000) thus any change in contrast will be filtered out. Authors:” 10-7 seconds is the inverse of the digital tine base, 10 12. This perigd is not used in practice as a dweil tine, 10° seconds being the usual minimun. However, the slow speed to the next dwell pgint, say 200 raster points avay, is 200 x 10°? seconds, and the Rinimim tine for a complete 4000x4000 raster for visual or photographic viewing is 1.6 seconds. What is the cost of the systent Reviewer Authors: Approximately, US $75,000 for the Scanning microscope with energy dispersive X-ray detector and moter driven stage, US $15,000 for computer system, and US $10,000’ for the digital ‘beam scanner and computer interfaces. Reviewer I: How many bits are the D/A conver~ ters! Authors: The 0/A converters are 12-bit high ‘Stability Burr-Brown bipolar DAC-40 series. Reviewer I: How is your device different from one by Yew & Pease (IITRI/SEM/1974 p, 191-197). Authors: In our system, signals from X-ray or STectron detectors are digitized as received and ‘these digital values are stored in the computer 450 in a condensed digital array. In the Yow & Pease System, the inage is physically stored on an array of 206’ solid state capacitors, and 1s thus able to be retained for signal processing or enhance. tent before re-disply as visual oF photographic image. Reviewer III: To what real problems has the sys- ‘tem actually been applied? Authors: Primarily to measuring the perimeters, ‘reas and subareas of a large number of individual particles such as shown in Figure 3, These data fre being used to establish statistical and geo- metrical paraneters for the occurrence probabi- Lities of particle inclusions. The digital scan control and data collection programs have been thoroughly tested in this way. Only a linited number of test runs have been made with specinens containing a nunber of particles mounted on sli oF metal foil, and systenatic and routine seasur- iments are just beginning. Stage movenent and control to bring successive fields into view has been extensively tested and is fully established, ‘The perimeter and area programs have been run off Line, for narticles of extreme complexity without Jogical failure, and have been run on-line (in compiled FORTRAN forn) for particles such as shown in Figure 3, with output parameters as in Table 1, The prograns are “on-line” in the sense of being resident. in the control computer and operating on the digital inage array once it has been obtained.