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SEMI F73-1102 © SEMI 2002 5 17 Related Documents 17.1 ASTM Stan dards ASTM F1372-93 — Standard Test Method for Scanning El ectron Microscope (SEM) Analysis of Metallic Surface Condition for Gas Distribution System Comp o…

SEMI F73-1102 © SEMI 2002 4

collection efficiency. Any adhesives used to mount

samples must not contaminate the surface to be

analyzed. To remove loosely adhered surface particles,

the sample may be blown off immediately before

introduction into the SEM with clean, dry, 0.1

micrometer filtered gas.

14.2 Place the sample in the SEM chamber for

pumpdown. Activate the electron beam when vacuum

conditions meet manufacturer’s recommendations. The

instrument accelerating voltage should be a consistently

selected value within the range 15 to 25 Kev; 20 KeV is

suggested. The working distance should be within the

range recommended by the instrument manufacturer.

Sample position (tilt angle and orientation) may be

adjusted to optimize EDS detector collection efficiency

for EDS analysis.

14.3 Increase the magnification to ≥ 400× for initial

focus; adjust instrument parameters for astigmatism and

other anomalies. Decrease magnification to 200× and

move the sample while viewing until an area judged as

representative of the whole is in view. The area to be

analyzed should be as free of particles and defect

features produced by sample preparation as possible.

14.4 Refocus and record images of this area at 200×,

1000×, and a pre-selected, consistently used

magnification within the range 3000 to 3600×. Move

to another representative area and record an image at

the same 3000–3600× magnification. Move to a third

representative area and record another image at the

3000–3600× magnification.

14.5 Each area selected for recording should include a

defect or metallurgical feature to demonstrate proper

focusing, contrast adjustment and resolution capability.

Contrast adjustment should be performed per the

technique described in Section 4.7.2.1 of Scanning

Electron Microscopy and X-Ray Microanalysis.

All

defects and/or features for which the change in signal

∆S due to the contrast exceeds the noise N by a factor

of 5 minimum must be clearly distinguishable in the

image recorded (see Section 4.5 of reference 5).

14.6 If any inclusions or contamination are noted in the

3000–3600× images, EDS analysis of representative

defect(s) may be performed if requested by the

company for which the test method is performed.

Collect X-ray signals for a sufficient length of time to

obtain an integrated count of ≥ 250,000 within the

range of 0 to 10 keV.

5 Scanning Electron Microscopy and X-Ray Microanalysis: A Text

for Boilogists, Materials Scientists, and Geologists; Joseph I.

Goldstein, Dale E. Newbury, Patrick Echlin, David C. Joy, A. D.

Romig, Jr., Charles E. Lyman, Charles Fiori, Eric Lifshin; Second

Edition, Plenum Press, New York (1992).

15 Calculations or Interpretation of Results

15.1 The 3000–3600× recorded images shall be placed

under the transparent overlay grid. The number of grid

squares that contain all or part of a surface defect shall

be counted and summed for each photomicrograph.

Each such grid square shall only be counted once; it is

not the intent of this Test Method to count individual

defects. If a defect appears in more than one adjacent

grid square, each grid square occupied shall be counted.

NOTE 2: Examples of scanning electron micrographs

overlaid with an alphanumeric indexed grid showing specific

types of defects with comments on their locations and

whether they should be counted may be viewed at

http://www.semi.org/web/wstandards.nsf/url/SurfaceAnalysis

Examples.

15.2 Surface film residues resulting from improper

cleaning are generally diffuse and difficult to quantify.

These residues, if present, are counted as one per

image. Particles that loosely adhere to the surface must

be presumed to be artifacts of sample preparation or

exposure, and therefore shall be ignored.

15.3 Peaks appearing in the EDS spectra shall be

identified and the spectra labeled to indicate whether it

is a representative area, or identified as a defect from a

photomicrograph.

16 Reporting Results

16.1 A tabular summary of defects counted per 3000–

3600× photomicrograph shall be presented.

Additionally, the table should indicate an average of

defect counts and the maximum from the three 3000–

3600× images. An example of a table reporting defect

counting results and the photomicrographs from which

the defect counts were taken are shown in Appendix 1.

16.2 All photomicrographs are to be permanently

labeled with sample identification, magnification, a

magnification scale bar, date, and analyst identification.

The photomicrographs should be available for

inspection upon request.

16.3 EDS spectra are to be labeled with the same

information, plus peak identifications. If any

instrument parameters (e.g., tilt angle) were changed for

EDS analysis, these must be noted. If peak height

differences are such that adequate representation of all

peaks cannot be made from the same plot, two plots

having different scaling shall be included.

Identification of each defect analyzed, either by arrow

on photomicrograph or by notation of grid position,

shall be made.

SEMI F73-1102 © SEMI 2002 5

17 Related Documents

17.1 ASTM Standards

ASTM F1372-93 — Standard Test Method for Scanning Electron Microscope (SEM) Analysis of Metallic Surface

Condition for Gas Distribution System Components

ASTM F1375-92 — Standard Test Method for Energy Dispersive X-Ray Spectrometer (EDX) Analysis of Metallic

Surface Condition for Gas Distribution System Components

APPENDIX 1

EXAMPLE OF AN ACCEPTABLE FORMAT FOR REPORTING DEFECT

COUNTING RESULTS

NOTE: The material in this appendix is an official part of SEMI F73 and was approved by full letter ballot procedures.

Table A1-1 Example of an Acceptable Format for Reporting Defect Counting Results

Analyst Name: John Doe

Analytical Service Provider: ABC Services Lab

Date: May 10, 1999

(Customer; Order Number; Source): Pure Products, Inc.

Sample

Micro

No.

Defect

Count

Comments

(Location indexing optional)

Average

Count

Maximum

Count

1 (from

Figure

A1-1)

13 Inclusion J7, K7, I8, J8, K8; Pits A8, C7 and C8,

E9, F8, J9, I12, I15

2 (from

Figure

A1-2)

30 Stringer G14 to P3; Pit C13 and C14

A22-6/5/97

3 (from

Figure

A1-3)

4 Pits D10 and E10, G13. Grain, twin boundaries,

white sample prep debris not counted.

1 12 Pits; stringer

2 23 Scratch

(Sample #2

Identification)

3 16 Inclusion

1 9 Stringer

2 4

(Sample #3

Identification)

3 6 Pits