ISO 23420 pdf free download

ISO 23420-2021 pdf free download.Microbeam analysis – Analytical electron microscopy – Method for the determination of energy resolution for electron energy loss spectrum analysis.
7.2 Predetermination of binding energy
7.2.1 Obtain graphite and the other reference sample
Obtain a graphite and a second reference sample. The graphite reference sample has a Carbon K-edge and an EEL peak Eaip in an EEL spectrum. The second reference sample should have an EEL peak ECZLP appearing close to the zero-loss peak, hut the peak spread should not overlap with the zero-loss peak. For example, the boron nitride plasmon-loss (it – i’i9 peak is suitable for the Ep as good as the graphite plasmon-loss (it + a) peak.
7.2.2 Measure Cis of graphite by using the XPS
Measure the carbon K-shell binding energy of the graphite using XPS. The Cis is used as carbon K edge energy ECK of graphite of the EELS. The XPS shall be calibrated by ISO 15472:2010.
7.3 Setup of the S/TEM and the EELS and sample setting
Samples are recommended to be drop-cast onto a TEM grid. e.g. a holey carbon film support grid, to
ease the measurement. The electron microscope should be adjusted for S/TEM observation in advance.
EELS should also be adjusted in advance so that EEL spectra can be easily obtained. Parameters of the
S/TEM and the EELS are recorded as described in 7.
The quality of an EEL spectrum is easily affected by electron beam induced carbon contamination. The use of an anti-contamination device Is strongly recommended for suppression of the contamination. Additionally, a clean environment in the column is also needed to minimise the contamination.
7.4 First energy step, SE1, calibration
7.4.1 EELS acquisition set-up
Set the EEL spectrometer acquisition time and integration numbers so as to secure a sufficient signal-to-noise ratio without any peak saturation for all measurements, including measurements in subsequent sections. Since the measurement conditions such as irradiation current, entrance aperture diameter and capturing device characterization like CCD / CMOS camera are different, acquisition time and integration number cannot be uniformized. Therefore, users of this procedure should optimise acquisition time and integration number for their own systems and should record these values.
7.4.2 Determining the EELS first energy step, SE1
Set the energy step SE1 to cover all range from the zero-loss peak to the carbon K edge EC.K of graphite.
In the parallel detection system, energy step SE1 is selected from the preset value under the condition as Formula (2).
SEIECK/m (2)
where
EC.K is carbon K edge energy in the EELS m is total number of available channels in the parallel detection system of the EELS In the serial detection system, set a full measurement range as the zero-loss peak to the carbon K edge EC.K of graphite. Energy step SE1 is obtained as Formula (3).
SE1 =SE5/B
where
SE is energy width of the energy-selecting window in the serial detection system of the EELS B is spatial width of energy selecting window in the serial detection system of the EELS
7.4.3 Acquisition of carbon K-edge EEL spectrum
Irradiate a thin region of graphite with the electron beam and acquire an EEL spectrum including the ZLP and the carbon K-shell edge. A d/A (sample thickness / mean free path) ratio check should be performed to ensure the thickness of the area irradiated is suitable for the procedure.
Since the intensities of the zero-loss peak, the plasmon-loss (it + a) peak and carbon K edge EC.K are considerably different, spectra including all these peaks may need to be acquired separately.
If it is necessary to acquire separate EEL spectra, an EEL spectrum should be acquired to include the zero- loss peak and the plasmon-loss (it + a) peak, this region will give the value for Ch1(G, P), (Figure 2). Acquire a 2’ spectra which includes the plasmon-loss (it + a) peak and carbon K edge ECK, this region will give the value for Ch1(G, C-K), (Figure 3).
Furthermore, the sum of Ch1(G, P) and the Ch1(G, C-K) gives the value for Cl-I1 (see Z4A).
Certain EELS systems are able to acquire Ch1(G, P) and Ch1(G, C-K) simultaneously if the EELS system has a function capable of obtaining two regions of the EEL spectrum.
7.4.4 Calculate calibrated energy step SE1
Obtain calibrated energy step SE1 as Formula (4). 6E1 is the calibrated value of energy step SE1. 6E1 = EC.K / Cl-I1 = EC.K / (Ch1(G. P) + Ch1(G, C-K))
where
Ch1(G, P) is the number of channels of the range from the zero-loss peak [Figure 2. key 1J to the graphite plasmon-loss (it + a) peak Ep [Figure 2. key 2] on the energy step SE1 in the parallel detection system. In the serial detection system, Ch1(G, P) is distance between the zero-loss peak [Figure 2. key 11 and the graphite plasmon-loss (it + a) peak ECZLp [EigurL key 2] on the energy step SE1.
Ch1(G, C-K) is the number of channels of the range from the graphite plasmon-loss (it + a) peak [Eig. ur.3, key 1] to carbon K edge ECK IFigure 3. key 2] on the energy step SE1 in the parallel detection system. In the serial detection system, Ch1(G, C-K) is distance between the graphite plasmon-loss (it + a) peak [Figure 3. key 1] and carbon K edge EC.K [Figure 3. key 2] on the energy step SE1.
In this document, the EELS carbon K edge position corresponding to the XPS Cls peak is set to half height [Figure 4, key 2] between peak [Figure 4. key 1] and dip [Figure 4. key 3J of a background- subtracted spectrum for EELS carbon K edge as example of Figure 4.ISO 23420 pdf download.