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hardness_porosity.org
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metallurgy.org (Stored with Git LFS)
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#+TITLE: Piezo
Use the below to create your own sonotrode
https://www.thorlabs.com/newgrouppage9.cfm?objectgroup_id=14002
No, like seriously, if you combine this with a frequency generator and a waveform aplifier capacable to handling high frequency loads, you'd have a academic weapon.
Music acoustics
https://www.phys.unsw.edu.au/jw/basics.html
https://www.animations.physics.unsw.edu.au/jw/dB.htm
https://sengpielaudio.com/calculator-leveladding.htm
The ‘piezoelectric effect’ describes a phenomenon exhibited by a few crystalline materials in which they produce an electrical charge when subjected to mechanical stress, i.e. squeezed. The sign of the resulting voltage changes if compression crosses over to tension. For historical reasons this is referred to as ‘the direct piezoelectric effect’. The phenomenon is reversible. For these same materials, forcing a charge onto their surface via applied voltage will cause them to mechanically expand or contract. This is referred to as ‘the converse piezoelectric effect’. As with the direct effect, the direction of crystal distortion (i.e. expansion or contraction) will follow the plus or minus sign of the applied voltage.
The converse piezoelectric effect is what makes power ultrasonic devices possible. While natural crystals exhibit piezoelectricy, quartz being the prime example, artificial crystals can exhibit much higher electromechanical conversion effectiveness and are exclusively used for the power ultrasonics we will discuss. Lead zirconate titanate compounds in ceramic form are by far the most commonly use for devices currently in use.
An AC voltage applied to a piezoelectric crystal will cause it to expand and contract in response. The expansion and contraction can create sound pressure waves or otherwise act on adjacent media. For practical use, piezoelectric crystals are bolted, bonded, soldered, or otherwise incorporated into composite ultrasonic transducers with the right geometry to convert the applied AC voltage into useful vibrational energy.
Piezo-driven ultrasonics have low power and high-power applications. Examples of low power applications include medical devices for imaging internal organs or structures such as heart valves and fetuses and clock signal generators in electronic instrumentation. We will focus on the high-power application including sonar, flow metering, underwater communications, ultrasonic drills, ultrasonic cleaners, friction welding, cutting blades, dental scalers, and fluid atomization.
* Langevin transducer
An ultrasonic transducer where one or more piezoelectric elements are mechanically compressed (prestressed) between end masses (i.e., a front driver and a back driver).
The term “ Langevin transducer” now describes any piezoelectric-driven longitudinal resonator based on sandwiching piezoelectric materials between two plates secured by a center bolt. Figure 3 shows a modern Langevin ultrasonic transducer. The components of the transducer perform the following functions:
The transducer has two layers of piezoelectric discs. Use of two piezoelectric discs allows the outer metal cylinders to be at ground potential which protects personnel from shock hazards and minimizes the risk of a short circuit. The discs are placed such that their polarities are opposite to each other; and that allows applying high voltage only to a single location, a center conductor that is sandwiched between the two piezoelectric discs.
The bolt provides precompression on the piezoelectric discs. Piezoelectric materials can fracture easily from tensile stresses of around 2,000 psi, but their compression strength can withstand a five times greater pressure of 10,000 psi. The bolt bias the discs into their compression region. Thus, when the discs vibrate, their motion is from full compression to a small amount of compression and they never see destructive tension. The Animation in Figure 4 illustrates the motion of the transducer.
The end plates distribute the point force of the bolt over the entire piezo surface so that the both the static and dynamic compressions in the piezo material are uniform through its volume.
#+CAPTION: Example of simple Langevin transducer (Berlincourt (3), p. 249)
[[attachment:_20240323_194235screenshot.png]]
* Horn design
Horn Designs
Because the only real rule for horn design is conservation of momentum, there are a huge variety of horn shapes and horn tips. Examples of the myriad styles of horn shapes with different tips are shown in Figure 6. The far-right horn, for example, is an assembly of multiple horns attached to one transducer. Each shape has a unique purpose. Each design converts the vibration at the face of the Langevin engine to a vibration on the face of the tip of the horn. The geometrical design of the horn tip provides a cross sectional shape and motion designed to accomplish a specific task.
* Tornplitz
By itself, the Langevin transducer creates mechanical motion. The transducer has plenty of power, but by itself does not lend itself to producing useful work. In Part 2, I introduced a transmission mechanism, the horn, which attaches to the Langevin piezoelectric transducer, the acoustic engine. The horn directs and amplifies the mechanical motion generated by the Langevin transducer allowing its energy to be delivered to the tip of the horn in a high velocity regime suitable for friction welding, cutting, and scaling among other applications. You could think of the horn as an acoustic lever.
In this final part, I will present a second transmission method, Tonpilz transmission technology. In contrast to the horn that leverages the Langevin’s energy into a high vibrational velocity tip for mechanical work, the Tonpilz transmission scheme is aimed at getting 100% of the Langevin’s output into broadcasting acoustic waves from one end and 0% off the other. This makes the Tonpilz type transducer ideal for energy efficient high intensity ultrasound sources.
Applications Using the Tonpilz Transmission
One application in which the Tonpilz transducer-transmission assembly excels is its use in an ultrasonic cleaner. Some ultrasonic cleaners have piezoelectric discs glued permanently to the bottom of the tank. That construct works fine until a piezoelectric disc breaks. Replacement involves a time-consuming effort to chip off the broken disc, cleaning down to the metal, and bonding a new disc into place. Installing a new disc involves faith that another disc may not break soon so the whole process would have to be repeated. Fortunately, there is a better solution. The solution is the construction of ultrasonic cleaners with modular, replaceable piezoelectric elements which can be bolted and unbolted from the assembly. Figure 5 shows an ultrasonic cleaner module and a cross-sectional view of an assembly having two piezoelectric discs, the bolt, the heavy metal back end and the lighter metal, most likely aluminum, head. This is bolted to the bottom of the cleaner tank.
* Practical stuff
https://blog.piezo.com/how-to-safely-solder-joints-onto-piezo-transducers
* Thorlabs
Introduction
In this tutorial we will look at some of the basics of piezoelectronic device structure and operation. These devices utilize piezoelectricity, a phenomenon in which electricity is created from pressure on the device. Piezoelectrics either produce a voltage in response to mechanical stress (known as direct mode) or a physical displacement as a result of an applied electrical field (known as indirect mode). Due to these modes, piezoelectric materials have found considerable use in both sensors and actuators and are often called “smart” or “intelligent” materials. One material in particular, lead-zirconate-titanate (PZT), has found prolific use for piezoelectric devices. Consequently, PZT is the ceramic material that makes up the bulk of piezoelectric actuator devices available on the market. It is not only piezoelectric but also pyroelectric and ferroelectric. PZT devices are capable of driving precision articulation of mechanical devices (such as a mirror mount or translating stage) due to the piezoelectric effect, which can be described through a set of coupled equations known as strain-charge (essentially coupling the electric field equations with the strain tensor of Hooke’s law):
$$ D_i = e^{\sigma}_{ij} d^{d}_{im}\sigma_m $$
$$ \epsilon_k = d^{c}_{jk} + s^{E}_{km} \sigma_m $$
Here D is the electric displacement vector, ε is the strain vector, E is the applied electric field vector, σm is the stress vector, eσij is the dielectric permittivity, ddim & dcjk are the piezoelectric coefficients, and sEkm is the elastic compliance (the inverse of stiffness). The specific matrix elements are used to calculate the useful measures of PZT functionality, though the full derivation of these equations is beyond the scope of this tutorial.
* Piezo Symbol Definitions
|--------+-------------+-------+-----------------+-------------------------------------------------------------|
| Symbol | Object Type | Size | Units | Meaning |
|--------+-------------+-------+-----------------+-------------------------------------------------------------|
| T | vector | 6 x 1 | $\frac{N}{m^2}$ | stress components (e.g. s1) |
| S | vector | 6 x 1 | $\frac{m}{m}$ | strain components (e.g. e3) |
| E | vector | 3 x 1 | $\frac{N}{C}$ | electric field components |
| D | vector | 3 x 1 | $\frac{C}{m^2}$ | electric charge density displacement components |
| s | matrix | 6 x 6 | $\frac{m^2}{N}$ | compliance coefficients |
| c | matrix | 6 x 6 | $\frac{N}{m^2}$ | stiffness coefficients |
| \epsilon | matrix | 3 x 3 | $\frac{F}{m}$ | electric permittivity |
| d | matrix | 3 x 6 | $\frac{C}{N}$ | piezoelectric coupling coefficients for Strain-Charge form |
| e | matrix | 3 x 6 | $\frac{C}{m^2}$ | piezoelectric coupling coefficients for Stress-Charge form |
| g | matrix | 3 x 6 | $\frac{m^2}{C}$ | piezoelectric coupling coefficients for Strain-Voltage form |
| q | matrix | 3 x 6 | $\frac{N}{C}$ | piezoelectric coupling coefficients for Stress-Voltage form |
|--------+-------------+-------+-----------------+-------------------------------------------------------------|
* Hooke's Law and Dielectrics
What is a constitutive equation? For mechanical problems, a constitutive equation describes how a material strains when it is stressed, or vice-versa. Constitutive equations exist also for electrical problems; they describe how charge moves in a (dielectric) material when it is subjected to a voltage, or vice-versa.
Engineers are already familiar with the most common mechanical constitutive equation that applies for everyday metals and plastics. This equation is known as Hooke's Law and is written as:
$$ S = s . T $$
In words, this equation states: Strain = Compliance × Stress.
However, since piezoelectric materials are concerned with electrical properties too, we must also consider the constitutive equation for common dielectrics:
$$ D = \epsilon . E $$
In words, this equation states: ChargeDensity = Permittivity × ElectricField.
* Coupled Equation
Piezoelectric materials combine these two seemingly dissimilar constitutive equations into one coupled equation, written as:
$$ S = s_E . T + d^t . E $$
$$ D = d . T + \epsilon_T . E $$
The piezoelectric coupling terms are in the matrix d.
In order to describe or model piezoelectric materials, one must have knowledge about the material's mechanical properties (compliance or stiffness), its electrical properties (permittivity), and its piezoelectric coupling properties.
The subscripts in piezoelectric constitutive equations have very important meanings. They describe the conditions under which the material property data was measured. For example, the subscript E on the compliance matrix sE means that the compliance data was measured under at least a constant, and preferably a zero, electric field. Likewise, the subscript T on the permittivity matrix eT means that the permittivity data was measured under at least a constant, and preferably a zero, stress field.
* Material Selection
Select from the following list of piezoelectric materials to view their constitutive property data. The data is presented in constitutive matrix form.
Insulators
Ammonium Dihydrogen Phosphate
Potassium Dihydrogen Phosphate
Barium Sodium Niobate
Barium Titanate
Barium Titanate (poled)
Lithium Niobate
Lithium Tantalate Lead Zirconate Titanate:
PZT-2, PZT-4, PZT-4D, PZT-5A, PZT-5H, PZT-5J, PZT-7A, PZT-8
Quartz
Rochelle Salt
Bismuth Germanate
Semiconductors
Cadmium Sulfide
Gallium Arsenide
Tellurium Dioxide Zinc Oxide
Zinc Sulfide
#+TITLE: Piezo
Use the below to create your own sonotrode
https://www.thorlabs.com/newgrouppage9.cfm?objectgroup_id=14002
No, like seriously, if you combine this with a frequency generator and a waveform aplifier capacable to handling high frequency loads, you'd have a academic weapon.
Music acoustics
https://www.phys.unsw.edu.au/jw/basics.html
https://www.animations.physics.unsw.edu.au/jw/dB.htm
https://sengpielaudio.com/calculator-leveladding.htm
The ‘piezoelectric effect’ describes a phenomenon exhibited by a few crystalline materials in which they produce an electrical charge when subjected to mechanical stress, i.e. squeezed. The sign of the resulting voltage changes if compression crosses over to tension. For historical reasons this is referred to as ‘the direct piezoelectric effect’. The phenomenon is reversible. For these same materials, forcing a charge onto their surface via applied voltage will cause them to mechanically expand or contract. This is referred to as ‘the converse piezoelectric effect’. As with the direct effect, the direction of crystal distortion (i.e. expansion or contraction) will follow the plus or minus sign of the applied voltage.
The converse piezoelectric effect is what makes power ultrasonic devices possible. While natural crystals exhibit piezoelectricy, quartz being the prime example, artificial crystals can exhibit much higher electromechanical conversion effectiveness and are exclusively used for the power ultrasonics we will discuss. Lead zirconate titanate compounds in ceramic form are by far the most commonly use for devices currently in use.
An AC voltage applied to a piezoelectric crystal will cause it to expand and contract in response. The expansion and contraction can create sound pressure waves or otherwise act on adjacent media. For practical use, piezoelectric crystals are bolted, bonded, soldered, or otherwise incorporated into composite ultrasonic transducers with the right geometry to convert the applied AC voltage into useful vibrational energy.
Piezo-driven ultrasonics have low power and high-power applications. Examples of low power applications include medical devices for imaging internal organs or structures such as heart valves and fetuses and clock signal generators in electronic instrumentation. We will focus on the high-power application including sonar, flow metering, underwater communications, ultrasonic drills, ultrasonic cleaners, friction welding, cutting blades, dental scalers, and fluid atomization.
* Langevin transducer
An ultrasonic transducer where one or more piezoelectric elements are mechanically compressed (prestressed) between end masses (i.e., a front driver and a back driver).
The term “ Langevin transducer” now describes any piezoelectric-driven longitudinal resonator based on sandwiching piezoelectric materials between two plates secured by a center bolt. Figure 3 shows a modern Langevin ultrasonic transducer. The components of the transducer perform the following functions:
The transducer has two layers of piezoelectric discs. Use of two piezoelectric discs allows the outer metal cylinders to be at ground potential which protects personnel from shock hazards and minimizes the risk of a short circuit. The discs are placed such that their polarities are opposite to each other; and that allows applying high voltage only to a single location, a center conductor that is sandwiched between the two piezoelectric discs.
The bolt provides precompression on the piezoelectric discs. Piezoelectric materials can fracture easily from tensile stresses of around 2,000 psi, but their compression strength can withstand a five times greater pressure of 10,000 psi. The bolt bias the discs into their compression region. Thus, when the discs vibrate, their motion is from full compression to a small amount of compression and they never see destructive tension. The Animation in Figure 4 illustrates the motion of the transducer.
The end plates distribute the point force of the bolt over the entire piezo surface so that the both the static and dynamic compressions in the piezo material are uniform through its volume.
#+CAPTION: Example of simple Langevin transducer (Berlincourt (3), p. 249)
[[attachment:_20240323_194235screenshot.png]]
* Horn design
Horn Designs
Because the only real rule for horn design is conservation of momentum, there are a huge variety of horn shapes and horn tips. Examples of the myriad styles of horn shapes with different tips are shown in Figure 6. The far-right horn, for example, is an assembly of multiple horns attached to one transducer. Each shape has a unique purpose. Each design converts the vibration at the face of the Langevin engine to a vibration on the face of the tip of the horn. The geometrical design of the horn tip provides a cross sectional shape and motion designed to accomplish a specific task.
* Tornplitz
By itself, the Langevin transducer creates mechanical motion. The transducer has plenty of power, but by itself does not lend itself to producing useful work. In Part 2, I introduced a transmission mechanism, the horn, which attaches to the Langevin piezoelectric transducer, the acoustic engine. The horn directs and amplifies the mechanical motion generated by the Langevin transducer allowing its energy to be delivered to the tip of the horn in a high velocity regime suitable for friction welding, cutting, and scaling among other applications. You could think of the horn as an acoustic lever.
In this final part, I will present a second transmission method, Tonpilz transmission technology. In contrast to the horn that leverages the Langevin’s energy into a high vibrational velocity tip for mechanical work, the Tonpilz transmission scheme is aimed at getting 100% of the Langevin’s output into broadcasting acoustic waves from one end and 0% off the other. This makes the Tonpilz type transducer ideal for energy efficient high intensity ultrasound sources.
Applications Using the Tonpilz Transmission
One application in which the Tonpilz transducer-transmission assembly excels is its use in an ultrasonic cleaner. Some ultrasonic cleaners have piezoelectric discs glued permanently to the bottom of the tank. That construct works fine until a piezoelectric disc breaks. Replacement involves a time-consuming effort to chip off the broken disc, cleaning down to the metal, and bonding a new disc into place. Installing a new disc involves faith that another disc may not break soon so the whole process would have to be repeated. Fortunately, there is a better solution. The solution is the construction of ultrasonic cleaners with modular, replaceable piezoelectric elements which can be bolted and unbolted from the assembly. Figure 5 shows an ultrasonic cleaner module and a cross-sectional view of an assembly having two piezoelectric discs, the bolt, the heavy metal back end and the lighter metal, most likely aluminum, head. This is bolted to the bottom of the cleaner tank.
* Practical stuff
https://blog.piezo.com/how-to-safely-solder-joints-onto-piezo-transducers
* Thorlabs
Introduction
In this tutorial we will look at some of the basics of piezoelectronic device structure and operation. These devices utilize piezoelectricity, a phenomenon in which electricity is created from pressure on the device. Piezoelectrics either produce a voltage in response to mechanical stress (known as direct mode) or a physical displacement as a result of an applied electrical field (known as indirect mode). Due to these modes, piezoelectric materials have found considerable use in both sensors and actuators and are often called “smart” or “intelligent” materials. One material in particular, lead-zirconate-titanate (PZT), has found prolific use for piezoelectric devices. Consequently, PZT is the ceramic material that makes up the bulk of piezoelectric actuator devices available on the market. It is not only piezoelectric but also pyroelectric and ferroelectric. PZT devices are capable of driving precision articulation of mechanical devices (such as a mirror mount or translating stage) due to the piezoelectric effect, which can be described through a set of coupled equations known as strain-charge (essentially coupling the electric field equations with the strain tensor of Hooke’s law):
$$ D_i = e^{\sigma}_{ij} d^{d}_{im}\sigma_m $$
$$ \epsilon_k = d^{c}_{jk} + s^{E}_{km} \sigma_m $$
Here D is the electric displacement vector, ε is the strain vector, E is the applied electric field vector, σm is the stress vector, eσij is the dielectric permittivity, ddim & dcjk are the piezoelectric coefficients, and sEkm is the elastic compliance (the inverse of stiffness). The specific matrix elements are used to calculate the useful measures of PZT functionality, though the full derivation of these equations is beyond the scope of this tutorial.
* Piezo Symbol Definitions
|--------+-------------+-------+-----------------+-------------------------------------------------------------|
| Symbol | Object Type | Size | Units | Meaning |
|--------+-------------+-------+-----------------+-------------------------------------------------------------|
| T | vector | 6 x 1 | $\frac{N}{m^2}$ | stress components (e.g. s1) |
| S | vector | 6 x 1 | $\frac{m}{m}$ | strain components (e.g. e3) |
| E | vector | 3 x 1 | $\frac{N}{C}$ | electric field components |
| D | vector | 3 x 1 | $\frac{C}{m^2}$ | electric charge density displacement components |
| s | matrix | 6 x 6 | $\frac{m^2}{N}$ | compliance coefficients |
| c | matrix | 6 x 6 | $\frac{N}{m^2}$ | stiffness coefficients |
| \epsilon | matrix | 3 x 3 | $\frac{F}{m}$ | electric permittivity |
| d | matrix | 3 x 6 | $\frac{C}{N}$ | piezoelectric coupling coefficients for Strain-Charge form |
| e | matrix | 3 x 6 | $\frac{C}{m^2}$ | piezoelectric coupling coefficients for Stress-Charge form |
| g | matrix | 3 x 6 | $\frac{m^2}{C}$ | piezoelectric coupling coefficients for Strain-Voltage form |
| q | matrix | 3 x 6 | $\frac{N}{C}$ | piezoelectric coupling coefficients for Stress-Voltage form |
|--------+-------------+-------+-----------------+-------------------------------------------------------------|
* Hooke's Law and Dielectrics
What is a constitutive equation? For mechanical problems, a constitutive equation describes how a material strains when it is stressed, or vice-versa. Constitutive equations exist also for electrical problems; they describe how charge moves in a (dielectric) material when it is subjected to a voltage, or vice-versa.
Engineers are already familiar with the most common mechanical constitutive equation that applies for everyday metals and plastics. This equation is known as Hooke's Law and is written as:
$$ S = s . T $$
In words, this equation states: Strain = Compliance × Stress.
However, since piezoelectric materials are concerned with electrical properties too, we must also consider the constitutive equation for common dielectrics:
$$ D = \epsilon . E $$
In words, this equation states: ChargeDensity = Permittivity × ElectricField.
* Coupled Equation
Piezoelectric materials combine these two seemingly dissimilar constitutive equations into one coupled equation, written as:
$$ S = s_E . T + d^t . E $$
$$ D = d . T + \epsilon_T . E $$
The piezoelectric coupling terms are in the matrix d.
In order to describe or model piezoelectric materials, one must have knowledge about the material's mechanical properties (compliance or stiffness), its electrical properties (permittivity), and its piezoelectric coupling properties.
The subscripts in piezoelectric constitutive equations have very important meanings. They describe the conditions under which the material property data was measured. For example, the subscript E on the compliance matrix sE means that the compliance data was measured under at least a constant, and preferably a zero, electric field. Likewise, the subscript T on the permittivity matrix eT means that the permittivity data was measured under at least a constant, and preferably a zero, stress field.
* Material Selection
Select from the following list of piezoelectric materials to view their constitutive property data. The data is presented in constitutive matrix form.
Insulators
Ammonium Dihydrogen Phosphate
Potassium Dihydrogen Phosphate
Barium Sodium Niobate
Barium Titanate
Barium Titanate (poled)
Lithium Niobate
Lithium Tantalate Lead Zirconate Titanate:
PZT-2, PZT-4, PZT-4D, PZT-5A, PZT-5H, PZT-5J, PZT-7A, PZT-8
Quartz
Rochelle Salt
Bismuth Germanate
Semiconductors
Cadmium Sulfide
Gallium Arsenide
Tellurium Dioxide Zinc Oxide
Zinc Sulfide

48
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@ -1,24 +1,24 @@
* Porosity in Thermal Spray Coatings
Thermal spray coatings are susceptible to the formation of porosity due to a lack of fusion between sprayed particles or the expansion of gases generated during the spray process. The determination of area percent porosity is important to monitor the effect of variable spray parameters and the suitability of a coating for its intended purpose.
ASTM E 2109 Test Methods for Determining Area Percentage Porosity in
Thermal Sprayed Coatings
These test methods cover the determination of the area percentage porosity of thermal sprayed coatings. Method A is a manual, direct comparison method using seven standard images shown on figures in the standard. These figures depict typical distributions of porosity in thermal spray coatings. Method B is an automated technique requiring the use of a computerized image analyzer. The methods quantify area percentage porosity only on the basis of light reflectivity from a metallo-
* Coating Thickness
ASTM B 487 - Test Method for Measurement of Metal and Oxide Coating Thickness by Microscopical Examination of a Cross Section
This test method covers measurement of the local thickness of metal and oxide coatings by the microscopical examination of cross sections using an optical microscope.
Under good conditions, when using an optical microscope, the method is capable of giving an absolute measuring accuracy of 0.8 um.
The measuring device may be a screw (Filar) micrometre ocular or a micrometre eyepiece. An image splitting eyepiece is advantageous for thin coatings on rough substrate layers. The measuring device shall be calibrated at least once before and once after the measurement using a stage micrometre. The magnification should be chosen
so that the field of view is between 1.5 and 3 the coating thickness.
For the use of automatic image analysis see Section 18.5.5.
* Porosity in Thermal Spray Coatings
Thermal spray coatings are susceptible to the formation of porosity due to a lack of fusion between sprayed particles or the expansion of gases generated during the spray process. The determination of area percent porosity is important to monitor the effect of variable spray parameters and the suitability of a coating for its intended purpose.
ASTM E 2109 Test Methods for Determining Area Percentage Porosity in
Thermal Sprayed Coatings
These test methods cover the determination of the area percentage porosity of thermal sprayed coatings. Method A is a manual, direct comparison method using seven standard images shown on figures in the standard. These figures depict typical distributions of porosity in thermal spray coatings. Method B is an automated technique requiring the use of a computerized image analyzer. The methods quantify area percentage porosity only on the basis of light reflectivity from a metallo-
* Coating Thickness
ASTM B 487 - Test Method for Measurement of Metal and Oxide Coating Thickness by Microscopical Examination of a Cross Section
This test method covers measurement of the local thickness of metal and oxide coatings by the microscopical examination of cross sections using an optical microscope.
Under good conditions, when using an optical microscope, the method is capable of giving an absolute measuring accuracy of 0.8 um.
The measuring device may be a screw (Filar) micrometre ocular or a micrometre eyepiece. An image splitting eyepiece is advantageous for thin coatings on rough substrate layers. The measuring device shall be calibrated at least once before and once after the measurement using a stage micrometre. The magnification should be chosen
so that the field of view is between 1.5 and 3 the coating thickness.
For the use of automatic image analysis see Section 18.5.5.

403
proposal_archive/thesis_original.org
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@ -1,403 +0,0 @@
#+TITLE: Thesis
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%% This Source Code Form is subject to the terms of the MIT License.
%% If a copy of the MIT was not distributed with this file, You can obtain one at https://opensource.org/licenses/mit
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%% Last update: 2021/10/11
%%
%% author: Dorian Gouzou <jackred@tuta.io>
%% repository hosted on github at https://github.com/jackred/Heriot_Watt_Thesis_Template
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%% Subsection, 12-point, italic
\titleformat{\subsection}[hang]
{\normalfont\bfseries\itshape\fontsize{\subsectionFontSize}{\subsectionBaseline}\selectfont}{\thesubsection}{5pt}{}
% \titleformat{\subsection}[hang]
% {\normalfont\bfseries\itshape\fontsize{\subsectionFontSize}{\subsectionBaseline}\selectfont\MakeLowercase}{\thesubsection}{5pt}{\makefirstuc}
%% left|above|below
\titlespacing{\subsection}{0pt}{20pt}{10pt}
%% table of content
\renewcommand{\contentsname}{Table of Contents}
\setcounter{tocdepth}{2}
\setcounter{secnumdepth}{2}
%% list of figure
\renewcommand*\listfigurename{Figure table}
%% init gloassaries
%% noidx cause otherwise we have to do a normal glossary, compile, then remove it so it is cached
%% because we only use acronym
\makenoidxglossaries
%% bibliography config
%% https://tex.stackexchange.com/a/6977
\DeclareBibliographyCategory{cited}
\AtEveryCitekey{\addtocategory{cited}{\thefield{entrykey}}}
\addbibresource{Bibliography.bib}
\addbibresource{BibMine.bib}
%% hyperref setup
\hypersetup{
colorlinks = true,
linkcolor = blue, % normal internal links, like ref, can be black tbh
citecolor = blue, % bibliographical links
urlcolor = blue, % linked urls
filecolor = black % url which open local files
}
%% modified reference function
%% https://tex.stackexchange.com/a/438998
\newcommand\eref[1]{equation~(\ref{#1})}
\newcommand\tref[1]{table~\ref{#1}}
\newcommand\fref[1]{figure~\ref{#1}}
%% 1.5 line spacing
\setstretch{1.5}
#+END_SRC
** Info
#+CAPTION: Information pertaining to me and the university
#+BEGIN_SRC latex :tangle I-info.tex
%% The title of Thesis
\newcommand{\thesisTitle}{Cavitation Erosion of Blended Stellite Alloys}
%% Number of Volume, if more than one
%% not sure how it works out with latex tbh
%\newcommand{\numberVolume}{2}
%% The number of this volume
%\newcommand{\actualVolume}{1}
%% The author's name (you)
\newcommand{\authorName}{Vishakh Pradeep Kumar}
%% Distinctions/Qualifications if desired
%\newcommand{\distinction}{}
%% The qualification
\newcommand{\degreeQualification}{MSc. Mechanical Engineering}
%% The institution
%\newcommand{\institution}{Some weird institute no one ever heard about}
%% The school
\newcommand{\school}{School of Engineering and Physical Sciences}
\newcommand{\university}{Heriot-Watt University}
%% Month of submission
\newcommand{\monthDate}{April}
%% Year of submission
\newcommand{\yearDate}{2024}
#+END_SRC
** Glossary
#+CAPTION: Glossary
#+BEGIN_SRC latex
\newacronym{gcd}{GCD}{Greatest Common Divisor}
\newacronym{lcm}{LCM}{Least Common Multiple}
#+END_SRC
* Document
#+CAPTION: Document begin
#+BEGIN_SRC latex
\begin{document}
\dominitoc
#+END_SRC
** Preliminaries
#+BEGIN_SRC latex
\input{Preliminaries/1-titlepages}
#+END_SRC
*** Titlepage
#+BEGIN_SRC latex :tangle no
\pagestyle{empty}
\begin{center}
\vspace*{15pt}\par
\setstretch{1}
% \hrule
% \vspace{10pt}\par
\begin{spacing}{1.8}
%% you can replace by \MakeUppercase if you want uppercase
{\Large\bfseries\MakeLowercase{\capitalisewords{\thesisTitle}}}\\
\end{spacing}
% \hrule
% This thesis is composed of \numberVolume volumes. This one is the number \actualVolume.
\vspace{40pt}\par
\includegraphics[width=140pt]{Figures/logo.png}\\
\vspace{40pt}\par
{\itshape\fontsize{15.5pt}{19pt}\selectfont by\\}\vspace{15pt}\par
{
\Large \authorName
% , \distinction
}\vspace{55pt}\par
{
\large Submitted for the degree of \\ \vspace{8pt} \Large\slshape\degreeQualification\\
}
\vspace{35pt}\par
{\scshape\setstretch{1.5} \institution\\ \school\\ \university\\
}
\vspace{50pt}\par
{\large \monthDate\ \yearDate}
%\vfill
%\begin{flushleft}
%\setstretch{1.4}\small
%The copyright in this thesis is owned by the author. Any quotation from the thesis or use of any of the information contained in it must acknowledge this thesis as the source of the quotation or information.
%\end{flushleft}
\end{center}
\clearpage
#+END_SRC
*** Abstract
#+BEGIN_SRC latex
\pagestyle{preliminary}
%\input{Preliminaries/2-abstract}
\begin{center}
\LARGE\textbf {Abstract}
\end{center}
\vspace{5pt}
\noindent
In accordance with the Academic Regulations the thesis must contain an abstract preferably not exceeding 200 words, bound in to precede the thesis. The abstract should appear on its own, on a single page. The format should be the same as that of the main text. The abstract should provide a synopsis of the thesis and shall state clearly the nature and scope of the research undertaken and of the contribution made to the knowledge of the subject treated. There should be a brief statement of the method of investigation where appropriate, an outline of the major divisions or principal arguments of the work and a summary of any conclusions reached. The abstract must follow the Title Page.
\clearpage
#+END_SRC
*** Dedication
#+BEGIN_SRC latex
\begin{center}
\LARGE\textbf {Dedication}
\end{center}
\vspace{5pt}
If a dedication is included then it should be immediately after the Abstract page.\par
I don't what it is actually.
\clearpage
#+END_SRC
*** Acknowledgments
#+BEGIN_SRC latex
\begin{center}
\LARGE\textbf {Acknowledgements}
\end{center}
\vspace{5pt}
\noindent I wanna thanks all coffee and tea manufacturers and sellers that made the completion of this work possible.
\clearpage
#+END_SRC
*** Declaration
#+BEGIN_SRC latex
% % read about declaration in file
% % \input{Preliminaries/5-declaration}
\includepdf[pages=-]{Preliminaries/5-declaration.pdf}
{
\setstretch{1}
\hypersetup{linkcolor=black}
\tableofcontents
\listoftables % optional
\listoffigures % optional
\glsaddall % this is to include all acronym. You can do a sort of citation for acronym and include only the one you use, Look at the glossary package for details.
\printnoidxglossary[type=\acronymtype, title=Glossary] % optional
%% put your publications in BibMine.bib
%% They will be displayed here
\begin{refsection}[BibMine.bib]
\DeclareFieldFormat{labelnumberwidth}{#1}
\nocite{*}
\printbibliography[omitnumbers=true,title={List of Publications}]
\end{refsection}
}
%% if you don't want pagination you need to use this commented part instead of the one above for the table of content/list of figure/etc
%% this is because the toc is defined in an annoying way, especially multi page one
%% solution found here: https://tex.stackexchange.com/a/173423
% {
% \hypersetup{linkcolor=black}
% \pagestyle{empty} % Removes numbers from middle pages.
% \fancypagestyle{plain} % Re-definition removes numbers from first page.
% {
% \fancyhf{}% % Clear all header and footer fields.
% \renewcommand{\headrulewidth}{0pt}% Clear rules (remove these two lines if not desired).
% \renewcommand{\footrulewidth}{0pt}%
% }
% \tableofcontents
% \thispagestyle{empty}
% \listoftables %optional
% \thispagestyle{empty}
% \listoffigures %optional
% \thispagestyle{empty}
% \glsaddall % this is to include all acronym. You can do a sort of citation for acronym and include only the one you use, Look at the glossary package for details.
% \printnoidxglossary[type=\acronymtype, title=Glossary] % optional
% \thispagestyle{empty}
% %% put your publications in BibMine.bib
% %% They will be displayed here
% \begin{refsection}[BibMine.bib]
% \DeclareFieldFormat{labelnumberwidth}{#1}
% \nocite{*}
% \printbibliography[omitnumbers=true,title={List of Publications}]
% \end{refsection}
% \thispagestyle{empty}
% }
\clearpage
#+END_SRC

32
rig.org
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@ -1,16 +1,16 @@
#+TITLE: Rig
- [[https://gitlab.com/openflexure/openflexure-block-stage/][A 3D Printable high-precision 3 axis translation stage]]
Use for scanning samples?
https://arxiv.org/abs/1911.09986
Has 2 x 2 x 2 mm3 travel range, with sub 100 nm resolution.
- [[https://www.printables.com/model/874575-14-od-tube-organizer-with-zip-ties][1/4" OD Tube Organizer with Zip-ties]]
Use for organizing the water/vacuum/air pressure tubes?
#
#+TITLE: Rig
- [[https://gitlab.com/openflexure/openflexure-block-stage/][A 3D Printable high-precision 3 axis translation stage]]
Use for scanning samples?
https://arxiv.org/abs/1911.09986
Has 2 x 2 x 2 mm3 travel range, with sub 100 nm resolution.
- [[https://www.printables.com/model/874575-14-od-tube-organizer-with-zip-ties][1/4" OD Tube Organizer with Zip-ties]]
Use for organizing the water/vacuum/air pressure tubes?
#

960
sem_eds/eds.org
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@ -1,480 +1,480 @@
#+TITLE: SEM & EDS
Things to do
https://github.com/BAMresearch/automatic-sem-image-segmentation/tree/master
https://link.springer.com/article/10.1007/s13632-023-01020-7
https://github.com/IDEAsLab-Computational-Microstructure/EDS-PhaSe
* SEM
Honestly, a really good introduction to SEM
- Concepts
- [[https://youtu.be/d7ch1XSmOgI?si=v2Eb6ujTmoDv--o9][Scanning Electron Microscopy (SEM) Foundation Lecture (30 min)]]
yt:d7ch1XSmOgI
- [[https://www.youtube.com/watch?v=eOyfoMRHfgE][Connecting SEM Concepts to practice (16 min)]]
[[yt:eOyfoMRHfgE]]
- Basic Operations
- [[https://www.youtube.com/watch?v=luC-5TgNPsQ&t=0s][Basic SEM Alignment (Source Tilt, Focus, Astigmatism, Lens Alignment) (7 min)]]
[[yt:luC-5TgNPsQ]]
- [[https://www.youtube.com/watch?v=YeukVt1Fyi0&t=317s][Details of Astigmatism Correction (8 min)]]
[[yt:YeukVt1Fyi0]]
- [[https://www.youtube.com/watch?v=1syySgnTEqU][Fixing the Stigmator Alignment (5 min)]]
[[yt:1syySgnTEqU]]
- Specific to Tescan Vega
- [[https://www.youtube.com/watch?v=ypD_fqO4ptI][Tescan Vega SEM Operation (13 min)]]
[[yt:ypD_fqO4ptI]]
** Detectors
The detection system may contain a set of detectors designed for detecting various signals resulting from electron beam interaction with the sample surface. The microscope is always delivered with the SE detector
*** SE detector
The detector works in high vacuum only.
Secondary electrons enhance topographic contrast contrary to material contrast of back-scattered electrons. The secondary electron (SE) detector is a basic standard detector always present in the microscope.
The SE detector is of an Everhart-Thornley type. The grid on the front part of the detector has positive potential. This attracts and accelerates the low-energy secondary electrons arising on the specimen surface and focuses them onto the scintillator. The light flashes, which result from the impingement of the electrons on the scintillator, are transferred through the light guide to the photo-multiplier outside the chamber of the microscope.
*** BSE detector
The detector works in high and low vacuum.
Back-scattered electrons (BSE) enhance material contrast of the sample. The BSE detector is of the scintillation type. An annular (YAG) mono-crystal scintillator with a conductive surface is placed in the optical axis directly under the lower pole extension of the objective. The high energy back-scattered electrons impinge the scintillator without any additional acceleration and excite the scintillator atoms that emit visible radiation photons successively. The photons are carried, by means of the light guide, through the side outlet of the scintillator to the cathode of the photo-multiplier. They are then processed in the same way as the signal coming from the secondary electrons.
The BSE detector is manufactured in an R-BSE (Retractable BSE) version. This modification allows the retraction of the detector from under the pole piece position if the detector is not used. This enables the specimens to be moved as close as possible to the objective when viewed by other detectors.
** Considerations for Optimal SEM Imaging Results
- Beam Settings
- Voltage
Is specimen conductive (high) or non-conductive (low)?
Beam-sensitive (low) or not?
From what depth do you want signal to emerge, and which signal?
- Current
Is specimen conductive (high) or non-conductive (low)? Beam-sensitive (low) or not?
Optimize signal (high) vs. resolution (low), choose small aperture (imaging) or large (x-ray).
- Working Distance
If not constrained by geometry of application, optimize resolution (low) vs. depth of field (high);
signal may decrease at too long or too short W; when in doubt, operate at eucentric height.
EDX should be done with a working distance of 15 mm
- Detector Settings
Detector Type:
- SE (topographic contrast, some Z)
- BSE (atomic #, aka Z)
- EDS/WDS (elemental composition).
Using detector Bias, you can switch between different modes, please do not do so. Take one picture SE and one picture BSE. One might argue that the acquisition process for both are the same, but do it anyway, it makes life so much easier when you're trying to plot it on a report.
- Alignments
- Basic Technique:
After gun tilt, iteratively adjust focus, astigmatism, lens alignment based on visual cues.
- 1st Approximation (Focus/Stig):
Use reduced area window w/longest dwell time that gives near-live refresh rate.
- Perfected:
Make comparisons using “alignment rectangle” in full frame or reduced window (integrate 1 frame).
- Scan Settings
- Brightness & Contrast:
Optimize using Videoscope at dwell/pixel capture settings.
(try in full frame or line scan).
- Live (single frame) vs. frame & line averaging/integration
Frame averaging spreads out dose to mitigate charging artifacts, by averaging out the effects of a sudden flash. However, it does not overcome the general effects of charging and should be seen as a last ditch effort.
Note: This is unusual for thermal spray coatings and anything conductive.
- Scan Orientation:
Change scan rotation to scan perpendicular vs. parallel to features;
evaluate scan artifacts (is there image compression/stretching due to beam drift?) and mitigate charging artifacts.
* EDX
Energy-dispersive X-ray spectroscopy (EDS, EDX, or XEDS), sometimes called energy dispersive X-ray analysis (EDXA) or energy dispersive X-ray microanalysis (EDXMA), is an analytical technique used for the elemental analysis or chemical characterization of a sample. The EDS analysis can be used to determine the elemental composition of individual points or to map out the lateral distribution of elements from the imaged area.
The energy dispersive spectroscopy (EDS) technique is mostly used for qualitative analysis of materials but is capable of providing semi-quantitative results as well. Typically, SEM instrumentation is equipped with an EDS system to allow for the chemical analysis of features being observed in SEM monitor. Simultaneous SEM and EDS analysis is advantageous in failure analysis cases where spot analysis becomes extremely crucial in arriving at a valid conclusion. Signals produced in an SEM/EDS system includes secondary and backscattered electrons that are used in image forming for morphological analysis as well as X-rays that are used for identification and quantification of chemicals present at detectable concentrations. The detection limit in EDS depends on sample surface conditions, smoother the surface the lower the detection limit. EDS can detect major and minor elements with concentrations higher than 10 wt% (major) and minor concentrations (concentrations between 1 and 10 wt%). The detection limit for bulk materials is 0.1 wt% therefore EDS cannot detect trace elements (concentrations below 0.01 wt%) [1].
[[https://youtu.be/y75CAupTmUo?si=5D96lFYpyjykaQ4A][Tutorial on using the AZtecLive software]]
[[https://www.youtube.com/watch?v=XxrGunKAL0o&t=1s][Introduction to Energy Dispersive Spectroscopy (EDS)]]
EDS Mapping displays the X-ray data as individual elemental images for different energy ranges. Mapping gives a quick understanding of the scanned area. Unlike Point Analysis, it shows the elements distribution across the scanned area.
Construct Maps
- Map
- TruMap
Performs deconvolution to separate the images
- QuantMap
Image Scan Size - 1024
Dwell Time 10 um
Input Signal [ ] SE [ ] BSE
AutoLock On
Fixed Duration
Energy Range 20 kEV
Number of channels 2048
Process Time 2
Pixel Dwell Time us 50
Frame Live Time 10
Would suggest Line Spectra to show the change in composition from the top surface to the
Change the colors by selecting AutoLayer to really bring out the image
[[https://www.unamur.be/services/microscopie/sme-documents/Energy-20table-20for-20EDS-20analysis-1.pdf][Great PDF with EDS specific Periodic Table]]. Need to eventually make our own using https://tikz.net/periodic-table/
** Displaying Outset
Use outset graphs in EDX in order to show the change in composition
https://mmore500.com/outset/index.html
* Stellite Composition
#+CAPTION: The chemical compositions of the HIPed Stellite alloys and blends A, B and C in wt.%
|---------+----------+------------------------+-------+-------+-------+------+------+------+------+------+------|
| | Stellite | Description | Co | Cr | W | Mo | C | Fe | Ni | Si | Mn |
|---------+----------+------------------------+-------+-------+-------+------+------+------+------+------+------|
| Blend A | A1 | (Stellite 6 (HS6)) | 58.46 | 29.50 | 4.60 | 0.22 | 1.09 | 2.09 | 2.45 | 1.32 | 0.27 |
| | A3 | (50% HS6 + 50% HS20) | 50.80 | 30.68 | 10.45 | 0.25 | 1.72 | 2.30 | 2.37 | 1.16 | 0.27 |
| | A5 | (Stellite 20 (HS20)) | 43.19 | 31.85 | 16.30 | 0.27 | 2.35 | 2.50 | 2.28 | 1.00 | 0.26 |
|---------+----------+------------------------+-------+-------+-------+------+------+------+------+------+------|
| Blend B | B1 | (Stellite 1 (HS1)) | 46.84 | 31.70 | 12.70 | 0.29 | 2.47 | 2.30 | 2.38 | 1.06 | 0.26 |
| | B2 | (75% HS1 + 25% HS12) | 48.93 | 31.19 | 11.56 | 0.27 | 2.23 | 2.24 | 2.30 | 1.02 | 0.26 |
| | B3 | (50% HS1 + 50% HS12) | 51.00 | 30.68 | 10.43 | 0.25 | 1.98 | 2.19 | 2.21 | 0.99 | 0.27 |
| | B4 | (25% HS1 + 75% HS12) | 53.11 | 30.16 | 9.29 | 0.22 | 1.74 | 2.13 | 2.13 | 0.95 | 0.27 |
| | B5 | (Stellite 12 (HS12)) | 55.22 | 29.65 | 8.15 | 0.2 | 1.49 | 2.07 | 2.04 | 0.91 | 0.27 |
|---------+----------+------------------------+-------+-------+-------+------+------+------+------+------+------|
| Blend C | C1 | (Stellite 4 (HS4)) | 48.53 | 31.00 | 14.40 | 0.12 | 0.67 | 2.16 | 1.82 | 1.04 | 0.26 |
| | C2 | (75% HS4 + 25% HS190) | 48.57 | 30.06 | 14.40 | 0.14 | 1.31 | 2.15 | 2.07 | 1.03 | 0.27 |
| | C3 | (50% HS4 + 50% HS190) | 48.61 | 29.13 | 14.40 | 0.16 | 1.94 | 2.13 | 2.32 | 1.02 | 0.29 |
| | C4 | (25% HS4 + 75% HS190) | 48.66 | 28.19 | 14.40 | 0.18 | 2.58 | 2.12 | 2.56 | 1.01 | 0.3 |
| | C5 | (Stellite 190 (HS190)) | 48.72 | 27.25 | 14.40 | 0.20 | 3.21 | 2.1 | 2.81 | 1.00 | 0.31 |
|---------+----------+------------------------+-------+-------+-------+------+------+------+------+------+------|
|--------------+-------+------+-------+-------+------+------+------+------+------+------|
| | | Co | Cr | W | Mo | C | Fe | Ni | Si | Mn |
|--------------+-------+------+-------+-------+------+------+------+------+------+------|
| Stellite 6 | HS6 | Bal. | 29.50 | 4.60 | 0.22 | 1.09 | 2.09 | 2.45 | 1.32 | 0.27 |
| Stellite 20 | HS20 | Bal. | 31.85 | 16.30 | 0.27 | 2.35 | 2.50 | 2.28 | 1.00 | 0.26 |
| Stellite 1 | HS1 | Bal. | 31.70 | 12.70 | 0.29 | 2.47 | 2.30 | 2.38 | 1.06 | 0.26 |
| Stellite 12 | HS12 | Bal. | 29.65 | 8.15 | 0.20 | 1.49 | 2.07 | 2.04 | 0.91 | 0.27 |
| Stellite 4 | HS4 | Bal. | 31.00 | 14.40 | 0.12 | 0.67 | 2.16 | 1.82 | 1.04 | 0.26 |
| Stellite 190 | HS190 | Bal. | 27.25 | 14.40 | 0.20 | 3.21 | 2.10 | 2.81 | 1.00 | 0.31 |
|--------------+-------+------+-------+-------+------+------+------+------+------+------|
* EDS
#+BEGIN_SRC jupyter-python :var tbl=EDS_Energy_Table :results output :session py
print(tbl)
#+end_src
** EDS Energy Table
#+NAME: EDS_Energy_Table
#+CAPTION: Energy table for EDS analysis
| atomicNumber | name | Kalpha1 | Kalpha2 | Kbeta1 | Lalpha1 | Lalpha2 | Lbeta1 | Lbeta2 | Lgamma1 | Malpha1 |
|--------------+------+-----------+----------+----------+----------+-----------+----------+----------+----------+---------|
| 3 | Li | 54.3 | | | | | | | | |
| 4 | Be | 108.5 | | | | | | | | |
| 5 | B | 183.3 | | | | | | | | |
| 6 | C | 277 | | | | | | | | |
| 7 | N | 392.4 | | | | | | | | |
| 8 | O | 524.9 | | | | | | | | |
| 9 | F | 676.8 | | | | | | | | |
| 10 | Ne | 848.6 | 848.6 | | | | | | | |
| 11 | Na | 1040.98 | 1040.98 | 1071.1 | | | | | | |
| 12 | Mg | 1253.60 | 1253.60 | 1302.2 | | | | | | |
| 13 | Al | 1486.70 | 1486.27 | 1557.45 | | | | | | |
| 14 | Si | 1739.98 | 1739.38 | 1835.94 | | | | | | |
| 15 | P | 2013.7 | 2012.7 | 2139.1 | | | | | | |
| 16 | S | 2307.84 | 2306.64 | 2464.04 | | | | | | |
| 17 | Cl | 2622.39 | 2620.78 | 2815.6 | | | | | | |
| 18 | Ar | 2957.70 | 2955.63 | 3190.5 | | | | | | |
| 19 | K | 3313.8 | 3311.1 | 3589.6 | | | | | | |
| 20 | Ca | 3691.68 | 3688.09 | 4012.7 | 341.3 | 341.3 | 344.9 | | | |
| 21 | Sc | 4090.6 | 4086.1 | 4460.5 | 395.4 | 395.4 | 399.6 | | | |
| 22 | Ti | 4510.84 | 4504.86 | 4931.81 | 452.2 | 452.2 | 458.4 | | | |
| 23 | V | 4952.20 | 4944.64 | 5427.29 | 511.3 | 511.3 | 519.2 | | | |
| 24 | Cr | 5414.72 | 5405.509 | 5946.71 | 572.8 | 572.8 | 582.8 | | | |
| 25 | Mn | 5898.75 | 5887.65 | 6490.45 | 637.4 | 637.4 | 648.8 | | | |
| 26 | Fe | 6403.84 | 6390.84 | 7057.98 | 705.0 | 705.0 | 718.5 | | | |
| 27 | Co | 6930.32 | 6915.30 | 7649.43 | 776.2 | 776.2 | 791.4 | | | |
| 28 | Ni | 7478.15 | 7460.89 | 8264.66 | 851.5 | 851.5 | 868.8 | | | |
| 29 | Cu | 8047.78 | 8027.83 | 8905.29 | 929.7 | 929.7 | 949.8 | | | |
| 30 | Zn | 8638.86 | 8615.78 | 9572.0 | 1011.7 | 1011.7 | 1034.7 | | | |
| 31 | Ga | 9251.74 | 9224.82 | 10264.2 | 1097.92 | 1097.92 | 1124.8 | | | |
| 32 | Ge | 9886.42 | 9855.32 | 10982.1 | 1188.00 | 1188.00 | 1218.5 | | | |
| 33 | As | 10543.72 | 10507.99 | 11726.2 | 1282.0 | 1282.0 | 1317.0 | | | |
| 34 | Se | 11222.4 | 11181.4 | 12495.9 | 1379.10 | 1379.10 | 1419.23 | | | |
| 35 | Br | 11924.2 | 11877.6 | 13291.4 | 1480.43 | 1480.43 | 1525.90 | | | |
| 36 | Kr | 12649 | 12598 | 14112 | 1586.0 | 1586.0 | 1636.6 | | | |
| 37 | Rb | 13395.3 | 13335.8 | 14961.3 | 1694.13 | 1692.56 | 1752.17 | | | |
| 38 | Sr | 14165 | 14097.9 | 15835.7 | 1806.56 | 1804.74 | 1871.72 | | | |
| 39 | Y | 14958.4 | 14882.9 | 16737.8 | 1922.56 | 1920.47 | 1995.84 | | | |
| 40 | Zr | 15775.1 | 15690.9 | 17667.8 | 2042.36 | 2039.9 | 2124.4 | 2219.4 | 2302.7 | |
| 41 | Nb | 16,615.1 | 16,521.0 | 18,622.5 | 2,165.89 | 2,163.0 | 2,257.4 | 2,367.0 | 2,461.8 | |
| 42 | Mo | 17,479.34 | 17,374.3 | 19,608.3 | 2,293.16 | 2,289.85 | 2,394.81 | 2,518.3 | 2,623.5 | |
| 43 | Tc | 18,367.1 | 18,250.8 | 20,619 | 2,424 | 2,420 | 2,538 | 2,674 | 2,792 | |
| 44 | Ru | 19,279.2 | 19,150.4 | 21,656.8 | 2,558.55 | 2,554.31 | 2,683.23 | 2,836.0 | 2,964.5 | |
| 45 | Rh | 20,216.1 | 20,073.7 | 22,723.6 | 2,696.74 | 2,692.05 | 2,834.41 | 3,001.3 | 3,143.8 | |
| 46 | Pd | 21,177.1 | 21,020.1 | 23,818.7 | 2,838.61 | 2,833.29 | 2,990.22 | 3,171.79 | 3,328.7 | |
| 47 | Ag | 22,162.92 | 21,990.3 | 24,942.4 | 2,984.31 | 2,978.21 | 3,150.94 | 3,347.81 | 3,519.59 | |
| 48 | Cd | 23,173.6 | 22,984.1 | 26,095.5 | 3,133.73 | 3,126.91 | 3,316.57 | 3,528.12 | 3,716.86 | |
| 49 | In | 24,209.7 | 24,002.0 | 27,275.9 | 3,286.94 | 3,279.29 | 3,487.21 | 3,713.81 | 3,920.81 | |
| 50 | Sn | 25,271.3 | 25,044.0 | 28,486.0 | 3,443.98 | 3,435.42 | 3,662.80 | 3,904.86 | 4,131.12 | |
| 51 | Sb | 26,359.1 | 26,110.8 | 29,725.6 | 3,604.72 | 3,595.32 | 3,843.57 | 4,100.78 | 4,347.79 | |
| 52 | Te | 27,472.3 | 27,201.7 | 30,995.7 | 3,769.33 | 3,758.8 | 4,029.58 | 4,301.7 | 4,570.9 | |
| 53 | I | 28,612.0 | 28,317.2 | 32,294.7 | 3,937.65 | 3,926.04 | 4,220.72 | 4,507.5 | 4,800.9 | |
| 54 | Xe | 29,779 | 29,458 | 33,624 | 4,109.9 | | | | | |
| 55 | Cs | 30,972.8 | 30,625.1 | 34,986.9 | 4,286.5 | 4,272.2 | 4,619.8 | 4,935.9 | 5,280.4 | |
| 56 | Ba | 32,193.6 | 31,817.1 | 36,378.2 | 4,466.26 | 4,450.90 | 4,827.53 | 5,156.5 | 5,531.1 | |
| 57 | La | 33,441.8 | 33,034.1 | 37,801.0 | 4,650.97 | 4,634.23 | 5,042.1 | 5,383.5 | 5,788.5 | 833 |
| 58 | Ce | 34,719.7 | 34,278.9 | 39,257.3 | 4,840.2 | 4,823.0 | 5,262.2 | 5,613.4 | 6,052 | 883 |
| 59 | Pr | 36,026.3 | 35,550.2 | 40,748.2 | 5,033.7 | 5,013.5 | 5,488.9 | 5,850 | 6,322.1 | 929 |
| 60 | Nd | 37,361.0 | 36,847.4 | 42,271.3 | 5,230.4 | 5,207.7 | 5,721.6 | 6,089.4 | 6,602.1 | 978 |
| 61 | Pm | 38,724.7 | 38,171.2 | 43,826 | 5,432.5 | 5,407.8 | 5,961 | 6,339 | 6,892 | |
| 62 | Sm | 40,118.1 | 39,522.4 | 45,413 | 5,636.1 | 5,609.0 | 6,205.1 | 6,586 | 7,178 | 1,081 |
| 63 | Eu | 41,542.2 | 40,901.9 | 47,037.9 | 5,845.7 | 5,816.6 | 6,456.4 | 6,843.2 | 7,480.3 | 1,131 |
| 64 | Gd | 42,996.2 | 42,308.9 | 48,697 | 6,057.2 | 6,025.0 | 6,713.2 | 7,102.8 | 7,785.8 | 1,185 |
| 65 | Tb | 44,481.6 | 43,744.1 | 50,382 | 6,272.8 | 6,238.0 | 6,978 | 7,366.7 | 8,102 | 1,240 |
| 66 | Dy | 45,998.4 | 45,207.8 | 52,119 | 6,495.2 | 6,457.7 | 7,247.7 | 7,635.7 | 8,418.8 | 1,293 |
| 67 | Ho | 47,546.7 | 46,699.7 | 53,877 | 6,719.8 | 6,679.5 | 7,525.3 | 7,911 | 8,747 | 1,348 |
| 68 | Er | 49,127.7 | 48,221.1 | 55,681 | 6,948.7 | 6,905.0 | 7,810.9 | 8,189.0 | 9,089 | 1,406 |
| 69 | Tm | 50,741.6 | 49,772.6 | 57,517 | 7,179.9 | 7,133.1 | 8,101 | 8,468 | 9,426 | 1,462 |
| 70 | Yb | 52,388.9 | 51,354.0 | 59,370 | 7,415.6 | 7,367.3 | 8,401.8 | 8,758.8 | 9,780.1 | 1,521.4 |
| 71 | Lu | 54,069.8 | 52,965.0 | 61,283 | 7,655.5 | 7,604.9 | 8,709.0 | 9,048.9 | 10,143.4 | 1,581.3 |
| 72 | Hf | 55,790.2 | 54,611.4 | 63,234 | 7,899.0 | 7,844.6 | 9,022.7 | 9,347.3 | 10,515.8 | 1,644.6 |
| 73 | Ta | 57,532 | 56,277 | 65,223 | 8,146.1 | 8,087.9 | 9,343.1 | 9,651.8 | 10,895.2 | 1,710 |
| 74 | W | 59,318.24 | 57,981.7 | 67,244.3 | 8,397.6 | 8,335.2 | 9,672.35 | 9,961.5 | 11,285.9 | 1,775.4 |
| 75 | Re | 61,140.3 | 59,717.9 | 69,310 | 8,652.5 | 8,586.2 | 10,010.0 | 10,275.2 | 11,685.4 | 1,842.5 |
| 76 | Os | 63,000.5 | 61,486.7 | 71,413 | 8,911.7 | 8,841.0 | 10,355.3 | 10,598.5 | 12,095.3 | 1,910.2 |
| 77 | Ir | 64,895.6 | 63,286.7 | 73,560.8 | 9,175.1 | 9,099.5 | 10,708.3 | 10,920.3 | 12,512.6 | 1,979.9 |
| 78 | Pt | 66,832 | 65,112 | 75,748 | 9,442.3 | 9,361.8 | 11,070.7 | 11,250.5 | 12,942.0 | 2,050.5 |
| 79 | Au | 68,803.7 | 66,989.5 | 77,984 | 9,713.3 | 9,628.0 | 11,442.3 | 11,584.7 | 13,381.7 | 2,122.9 |
| 80 | Hg | 70,819 | 68,895 | 80,253 | 9,988.8 | 9,897.6 | 11,822.6 | 11,924.1 | 13,830.1 | 2,195.3 |
| 81 | Tl | 72,871.5 | 70,831.9 | 82,576 | 10,268.5 | 10,172.8 | 12,213.3 | 12,271.5 | 14,291.5 | 2,270.6 |
| 82 | Pb | 74,969.4 | 72,804.2 | 84,936 | 10,551.5 | 10,449.5 | 12,613.7 | 12,622.6 | 14,764.4 | 2,345.5 |
| 83 | Bi | 77,107.9 | 74,814.8 | 87,343 | 10,838.8 | 10,730.91 | 13,023.5 | 12,979.9 | 15,247.7 | 2,422.6 |
| 84 | Po | 79,290 | 76,862 | 89,800 | 11,130.8 | 11,015.8 | 13,447 | 13,340.4 | 15,744 | |
| 85 | At | 81,520 | 78,950 | 92,300 | 11,426.8 | 11,304.8 | 13,876 | | 16,251 | |
| 86 | Rn | 83,780 | 81,070 | 94,870 | 11,727.0 | 11,597.9 | 14,316 | | 16,770 | |
| 87 | Fr | 86,100 | 83,230 | 97,470 | 12,031.3 | 11,895.0 | 14,770 | 14,450 | 17,303 | |
| 88 | Ra | 88,470 | 85,430 | 100,130 | 12,339.7 | 12,196.2 | 15,235.8 | 14,841.4 | 17,849 | |
| 89 | Ac | 90,884 | 87,670 | 102,850 | 12,652.0 | 12,500.8 | 15,713 | | 18,408 | |
| 90 | Th | 93,350 | 89,953 | 105,609 | 12,968.7 | 12,809.6 | 16,202.2 | 15,623.7 | 18,982.5 | 2,996.1 |
| 91 | Pa | 95,868 | 92,287 | 108,427 | 13,290.7 | 13,122.2 | 16,702 | 16,024 | 19,568 | 3,082.3 |
| 92 | U | 98,439 | 94,665 | 111,300 | 13,614.7 | 13,438.8 | 17,220.0 | 16,428.3 | 20,167.1 | 3,170.8 |
| 93 | Np | | | | 13,944.1 | 13,759.7 | 17,750.2 | 16,840.0 | 20,784.8 | |
| 94 | Pu | | | | 14,278.6 | 14,084.2 | 18,293.7 | 17,255.3 | 21,417.3 | |
| 95 | Am | | | | 14,617.2 | 14,411.9 | 18,852.0 | 17,676.5 | 22,065.2 | |
* SEM SOP
** Stopping the Microscope
- Switch off the high voltage by clicking on the HV button in the Electron Beam panel.
- Remove your samples from the microscope.
- Pump the microscope.
- Close the program (use Exit from the File menu) select the Switch off (the microscope) and exit (the application) option.
- Wait until the VegaTC program closes itself. The microscope configuration will be automatically saved on the hard drive.
- Shut down OS Windows in the usual way.
- Turn the main switch to the left (OFF position).
** Loading of the sample
- Use only one gloved hand when handling samples and holders
- Avoid letting the sample holder or any part of the sample exchange rod touch non-clean surfaces which may be contaminated with hand-oil
- Never "blow on" or exhale on samples to dry them, use the IR lamp instead
- Always make sure all screws are tight and that you always have a sure grip
- Always ask if you have a question
** Images at Low Magnification
There are four factory presets for the accelerating voltage (5 kV, 10 kV, 20 kV, 30 kV), one
for each HV index. The user does not need to make any further adjustments by switching
among them and using magnification up to 4000x.
Click on the PUMP button in the Vacuum panel to start the pumping procedure
(Figure 2). It usually takes around 3 minutes to reach vacuum ready - status which
means that the microscope is ready to use. If there is a need to exchange the
specimen, follow the instructions in chapter 8.2.
[[download:20240310-112336_screenshot.png]]
In the SEM Detectors & Mixer panel select the appropriate detector from the list box
(Figure 3). We recommend using the SE or BSE detector. When the BSE detector is
used, make sure that the detector is not retracted! See chapter 6 for detailed infor-
mation
[[download:20240310-112456_screenshot.png]]
[[download:20240310-112616_screenshot.png]]
3. Select the accelerating voltage (30 kV recommended) using the combo box in the
Electron Beam panel (Figure 5).
4. Clicking on the HV button in the Electron Beam panel turns the high voltage on and
starts the heating of the tungsten filament (see Figure 5).
5. Right-click in the SEM Scanning window to open the menu and select the Minimum
Magnification function (Figure 6)
[[download:20240310-112645_screenshot.png]]
[[download:20240310-112723_screenshot.png]]
7 Select RESOLUTION mode (click on the Scan Mode function in the Info Panel (see
Figure 10) and select RESOLUTION or use the Continual Wide Field option – switches
automatically between WIDE FIELD and RESOLUTION mode and vice versa when
increasing or decreasing magnification)
Focus the image by clicking on the WD icon in the Toolbar and turning the
Trackball from left to right (or vice versa). Alternatively use the Auto WD function for
focusing (see Figure 6). Double-clicking (left mouse button) in the SEM Scanning
window opens the Focus window. To remove the Focus window double-click
anywhere in the SEM Scanning window.
To select beam intensity (BI 10 recommended), first left-click on the BI icon
on the Toolbar and then use the arrows in the Pad panel (Figure 8).
[[download:20240310-113043_screenshot.png]]
10. To select the sample position in the Stage Control panel, click on the appropriate
number button on the carousel (Figure 9) or use the manual knobs in the case of the
SB microscope type.
11. Placing the cursor over the SEM Scanning window and clicking the mouse wheel
moves that area on the stage into the centre of the image. See chapter 7.2 for other
mouse actions.
12. To magnify the image click on the Magnification icon on the Toolbar and turn
the Trackball from left to right.
13. Once the area of interest is magnified and focused as desired, right-click on the
Speed icon on the Toolbar and select the appropriate scanning speed.
14. Clicking on the Acquire button in the Info Panel (Figure 10) or on the icon
on the Toolbar saves the image. Fill in the note, sign and description field
if necessary. Choose a folder in which to store the image. To change the parameters
of the image use the Image Parameters function in the main SEM menu
[[download:20240310-113153_screenshot.png]]
[[download:20240310-113251_screenshot.png]]
5. Clicking on the icon opens the dialogue for saving the actual adjustment of the
microscope. It is possible to restore the saved adjustment of the microscope later.
** Images at High Magnification
The best resolution is achieved at the highest accelerating voltage (30 kV) of the primary
electrons.
1. Insert an appropriate sample for high magnification images (e.g. tin on carbon
sample, Figure 18).
2. Select the fourth HV index using the combo box in the Electron Beam panel (20 kV -
30 kV) and turn on the high voltage.
3. Focus the image in RESOLUTION mode (click on the Scan Mode function in the Info
Panel and select RESOLUTION or use the Continual Wide Field option).
Note: Use the Degauss column function by means of the icon before changing WD&Z or WD. The image should remain in focus.
Check the spot size, which is determined by the BI value. Right-click in the SEM
Scanning window to select the optimum BI value – Auto BI OptiMag.
5. For the best resolution, it is necessary to work at a short working distance (WD). The
optimum WD is about 5 mm for the SE detector (in the case that the BSE is not
mounted underneath the objective lens). For BSE images the optimum WD is about
8.5 mm. To change the working distance together with Z-axis, without defocusing
the image, use the WD&Z function in the Stage Control panel (Figure 15).
WARNING: Moving the manipulator with the specimen can cause it to collide with other inner
components of the microscope and can cause damage to the microscope. Control the
movements of the manipulator by video camera imaging (open the Chamber View by clicking
on the
icon). The manipulator's movement can be stopped by clicking on the Stop
button in the Stage Control panel (see Figure 15).
[[download:20240310-113624_screenshot.png]]
Gradually magnify and focus the image to achieve 10kx magnification. In the case
that the image is moving during focusing, it is necessary to check the centering
of the objective. Select the Manual Column Centering function using the combo box
in the Electron Beam panel after clicking on the Adjustment >>> button (Figure 16).
The Manual Centering Wizard window will appear (Figure 17). Clicking on the WOB
button opens the Focus window in the SEM Scanning window. Click on the Next>>
button to obtain the next instructions. The function of the centering has two adjust-
able values. To be sure just one value is changing, hold down the F12 key to change
only X movement at the Trackball, and the F11 key to change only Y movement.
7. Each time that the image is too dark or light it is necessary to use the Auto Signal
function (see Figure 6 or use the icon ). To set the contrast and brightness
manually, click on the icon and use the Trackball.
[[download:20240310-113731_screenshot.png]]
[[download:20240310-113752_screenshot.png]]
At higher magnifications (>10kx) it is necessary to check if astigmatism (Figure 18
(a), (b)) is precisely corrected (Figure 18 (c)). To correct astigmatism click on the
Stigmator function in the Info Panel (Figure 19). For precise correction use the Focus
window (in the SEM Scanning window) and the F11 and F12 keys in the same way
as in point 6.
[[download:20240310-113907_screenshot.png]]
9. Select the appropriate scanning speed and save the image.
10. Clicking on the icon opens the dialog for saving the current adjustment of the
microscope. It is possible to restore the saved adjustment of the microscope later.
[[download:20240310-113937_screenshot.png]]
** Specimen Exchange
The specimen should somehow be fixed or glued to the specimen stub before it is inserted into the chamber. It is possible to use 12.5 mm specimen stubs or any other specimen holders, delivered as microscope accessories (see chapter 9.7).
If the specimen is examined in high vacuum mode, it must be conductive or must be made conductive using one of the methods described in the technical information. The conductive surface of the specimen must be conductive contacted to the stub.
Non-conductive samples can be investigated in low vacuum mode.
Instructions:
1. Vent the microscope by using the VENT button in the Vacuum panel. Wait until the pressure is at atmospheric level.
2. Set the tilt of the specimen stage to zero.
3. Open the chamber door by gently pulling it.
4. The automatic positions set up in the Stage Control panel can be used, which are intended for specimen position exchange. To select the sample position click on the appropriate number button on the carousel. At this time the button background is red to indicate the specimen exchange mode.
#+TITLE: SEM & EDS
Things to do
https://github.com/BAMresearch/automatic-sem-image-segmentation/tree/master
https://link.springer.com/article/10.1007/s13632-023-01020-7
https://github.com/IDEAsLab-Computational-Microstructure/EDS-PhaSe
* SEM
Honestly, a really good introduction to SEM
- Concepts
- [[https://youtu.be/d7ch1XSmOgI?si=v2Eb6ujTmoDv--o9][Scanning Electron Microscopy (SEM) Foundation Lecture (30 min)]]
yt:d7ch1XSmOgI
- [[https://www.youtube.com/watch?v=eOyfoMRHfgE][Connecting SEM Concepts to practice (16 min)]]
[[yt:eOyfoMRHfgE]]
- Basic Operations
- [[https://www.youtube.com/watch?v=luC-5TgNPsQ&t=0s][Basic SEM Alignment (Source Tilt, Focus, Astigmatism, Lens Alignment) (7 min)]]
[[yt:luC-5TgNPsQ]]
- [[https://www.youtube.com/watch?v=YeukVt1Fyi0&t=317s][Details of Astigmatism Correction (8 min)]]
[[yt:YeukVt1Fyi0]]
- [[https://www.youtube.com/watch?v=1syySgnTEqU][Fixing the Stigmator Alignment (5 min)]]
[[yt:1syySgnTEqU]]
- Specific to Tescan Vega
- [[https://www.youtube.com/watch?v=ypD_fqO4ptI][Tescan Vega SEM Operation (13 min)]]
[[yt:ypD_fqO4ptI]]
** Detectors
The detection system may contain a set of detectors designed for detecting various signals resulting from electron beam interaction with the sample surface. The microscope is always delivered with the SE detector
*** SE detector
The detector works in high vacuum only.
Secondary electrons enhance topographic contrast contrary to material contrast of back-scattered electrons. The secondary electron (SE) detector is a basic standard detector always present in the microscope.
The SE detector is of an Everhart-Thornley type. The grid on the front part of the detector has positive potential. This attracts and accelerates the low-energy secondary electrons arising on the specimen surface and focuses them onto the scintillator. The light flashes, which result from the impingement of the electrons on the scintillator, are transferred through the light guide to the photo-multiplier outside the chamber of the microscope.
*** BSE detector
The detector works in high and low vacuum.
Back-scattered electrons (BSE) enhance material contrast of the sample. The BSE detector is of the scintillation type. An annular (YAG) mono-crystal scintillator with a conductive surface is placed in the optical axis directly under the lower pole extension of the objective. The high energy back-scattered electrons impinge the scintillator without any additional acceleration and excite the scintillator atoms that emit visible radiation photons successively. The photons are carried, by means of the light guide, through the side outlet of the scintillator to the cathode of the photo-multiplier. They are then processed in the same way as the signal coming from the secondary electrons.
The BSE detector is manufactured in an R-BSE (Retractable BSE) version. This modification allows the retraction of the detector from under the pole piece position if the detector is not used. This enables the specimens to be moved as close as possible to the objective when viewed by other detectors.
** Considerations for Optimal SEM Imaging Results
- Beam Settings
- Voltage
Is specimen conductive (high) or non-conductive (low)?
Beam-sensitive (low) or not?
From what depth do you want signal to emerge, and which signal?
- Current
Is specimen conductive (high) or non-conductive (low)? Beam-sensitive (low) or not?
Optimize signal (high) vs. resolution (low), choose small aperture (imaging) or large (x-ray).
- Working Distance
If not constrained by geometry of application, optimize resolution (low) vs. depth of field (high);
signal may decrease at too long or too short W; when in doubt, operate at eucentric height.
EDX should be done with a working distance of 15 mm
- Detector Settings
Detector Type:
- SE (topographic contrast, some Z)
- BSE (atomic #, aka Z)
- EDS/WDS (elemental composition).
Using detector Bias, you can switch between different modes, please do not do so. Take one picture SE and one picture BSE. One might argue that the acquisition process for both are the same, but do it anyway, it makes life so much easier when you're trying to plot it on a report.
- Alignments
- Basic Technique:
After gun tilt, iteratively adjust focus, astigmatism, lens alignment based on visual cues.
- 1st Approximation (Focus/Stig):
Use reduced area window w/longest dwell time that gives near-live refresh rate.
- Perfected:
Make comparisons using “alignment rectangle” in full frame or reduced window (integrate 1 frame).
- Scan Settings
- Brightness & Contrast:
Optimize using Videoscope at dwell/pixel capture settings.
(try in full frame or line scan).
- Live (single frame) vs. frame & line averaging/integration
Frame averaging spreads out dose to mitigate charging artifacts, by averaging out the effects of a sudden flash. However, it does not overcome the general effects of charging and should be seen as a last ditch effort.
Note: This is unusual for thermal spray coatings and anything conductive.
- Scan Orientation:
Change scan rotation to scan perpendicular vs. parallel to features;
evaluate scan artifacts (is there image compression/stretching due to beam drift?) and mitigate charging artifacts.
* EDX
Energy-dispersive X-ray spectroscopy (EDS, EDX, or XEDS), sometimes called energy dispersive X-ray analysis (EDXA) or energy dispersive X-ray microanalysis (EDXMA), is an analytical technique used for the elemental analysis or chemical characterization of a sample. The EDS analysis can be used to determine the elemental composition of individual points or to map out the lateral distribution of elements from the imaged area.
The energy dispersive spectroscopy (EDS) technique is mostly used for qualitative analysis of materials but is capable of providing semi-quantitative results as well. Typically, SEM instrumentation is equipped with an EDS system to allow for the chemical analysis of features being observed in SEM monitor. Simultaneous SEM and EDS analysis is advantageous in failure analysis cases where spot analysis becomes extremely crucial in arriving at a valid conclusion. Signals produced in an SEM/EDS system includes secondary and backscattered electrons that are used in image forming for morphological analysis as well as X-rays that are used for identification and quantification of chemicals present at detectable concentrations. The detection limit in EDS depends on sample surface conditions, smoother the surface the lower the detection limit. EDS can detect major and minor elements with concentrations higher than 10 wt% (major) and minor concentrations (concentrations between 1 and 10 wt%). The detection limit for bulk materials is 0.1 wt% therefore EDS cannot detect trace elements (concentrations below 0.01 wt%) [1].
[[https://youtu.be/y75CAupTmUo?si=5D96lFYpyjykaQ4A][Tutorial on using the AZtecLive software]]
[[https://www.youtube.com/watch?v=XxrGunKAL0o&t=1s][Introduction to Energy Dispersive Spectroscopy (EDS)]]
EDS Mapping displays the X-ray data as individual elemental images for different energy ranges. Mapping gives a quick understanding of the scanned area. Unlike Point Analysis, it shows the elements distribution across the scanned area.
Construct Maps
- Map
- TruMap
Performs deconvolution to separate the images
- QuantMap
Image Scan Size - 1024
Dwell Time 10 um
Input Signal [ ] SE [ ] BSE
AutoLock On
Fixed Duration
Energy Range 20 kEV
Number of channels 2048
Process Time 2
Pixel Dwell Time us 50
Frame Live Time 10
Would suggest Line Spectra to show the change in composition from the top surface to the
Change the colors by selecting AutoLayer to really bring out the image
[[https://www.unamur.be/services/microscopie/sme-documents/Energy-20table-20for-20EDS-20analysis-1.pdf][Great PDF with EDS specific Periodic Table]]. Need to eventually make our own using https://tikz.net/periodic-table/
** Displaying Outset
Use outset graphs in EDX in order to show the change in composition
https://mmore500.com/outset/index.html
* Stellite Composition
#+CAPTION: The chemical compositions of the HIPed Stellite alloys and blends A, B and C in wt.%
|---------+----------+------------------------+-------+-------+-------+------+------+------+------+------+------|
| | Stellite | Description | Co | Cr | W | Mo | C | Fe | Ni | Si | Mn |
|---------+----------+------------------------+-------+-------+-------+------+------+------+------+------+------|
| Blend A | A1 | (Stellite 6 (HS6)) | 58.46 | 29.50 | 4.60 | 0.22 | 1.09 | 2.09 | 2.45 | 1.32 | 0.27 |
| | A3 | (50% HS6 + 50% HS20) | 50.80 | 30.68 | 10.45 | 0.25 | 1.72 | 2.30 | 2.37 | 1.16 | 0.27 |
| | A5 | (Stellite 20 (HS20)) | 43.19 | 31.85 | 16.30 | 0.27 | 2.35 | 2.50 | 2.28 | 1.00 | 0.26 |
|---------+----------+------------------------+-------+-------+-------+------+------+------+------+------+------|
| Blend B | B1 | (Stellite 1 (HS1)) | 46.84 | 31.70 | 12.70 | 0.29 | 2.47 | 2.30 | 2.38 | 1.06 | 0.26 |
| | B2 | (75% HS1 + 25% HS12) | 48.93 | 31.19 | 11.56 | 0.27 | 2.23 | 2.24 | 2.30 | 1.02 | 0.26 |
| | B3 | (50% HS1 + 50% HS12) | 51.00 | 30.68 | 10.43 | 0.25 | 1.98 | 2.19 | 2.21 | 0.99 | 0.27 |
| | B4 | (25% HS1 + 75% HS12) | 53.11 | 30.16 | 9.29 | 0.22 | 1.74 | 2.13 | 2.13 | 0.95 | 0.27 |
| | B5 | (Stellite 12 (HS12)) | 55.22 | 29.65 | 8.15 | 0.2 | 1.49 | 2.07 | 2.04 | 0.91 | 0.27 |
|---------+----------+------------------------+-------+-------+-------+------+------+------+------+------+------|
| Blend C | C1 | (Stellite 4 (HS4)) | 48.53 | 31.00 | 14.40 | 0.12 | 0.67 | 2.16 | 1.82 | 1.04 | 0.26 |
| | C2 | (75% HS4 + 25% HS190) | 48.57 | 30.06 | 14.40 | 0.14 | 1.31 | 2.15 | 2.07 | 1.03 | 0.27 |
| | C3 | (50% HS4 + 50% HS190) | 48.61 | 29.13 | 14.40 | 0.16 | 1.94 | 2.13 | 2.32 | 1.02 | 0.29 |
| | C4 | (25% HS4 + 75% HS190) | 48.66 | 28.19 | 14.40 | 0.18 | 2.58 | 2.12 | 2.56 | 1.01 | 0.3 |
| | C5 | (Stellite 190 (HS190)) | 48.72 | 27.25 | 14.40 | 0.20 | 3.21 | 2.1 | 2.81 | 1.00 | 0.31 |
|---------+----------+------------------------+-------+-------+-------+------+------+------+------+------+------|
|--------------+-------+------+-------+-------+------+------+------+------+------+------|
| | | Co | Cr | W | Mo | C | Fe | Ni | Si | Mn |
|--------------+-------+------+-------+-------+------+------+------+------+------+------|
| Stellite 6 | HS6 | Bal. | 29.50 | 4.60 | 0.22 | 1.09 | 2.09 | 2.45 | 1.32 | 0.27 |
| Stellite 20 | HS20 | Bal. | 31.85 | 16.30 | 0.27 | 2.35 | 2.50 | 2.28 | 1.00 | 0.26 |
| Stellite 1 | HS1 | Bal. | 31.70 | 12.70 | 0.29 | 2.47 | 2.30 | 2.38 | 1.06 | 0.26 |
| Stellite 12 | HS12 | Bal. | 29.65 | 8.15 | 0.20 | 1.49 | 2.07 | 2.04 | 0.91 | 0.27 |
| Stellite 4 | HS4 | Bal. | 31.00 | 14.40 | 0.12 | 0.67 | 2.16 | 1.82 | 1.04 | 0.26 |
| Stellite 190 | HS190 | Bal. | 27.25 | 14.40 | 0.20 | 3.21 | 2.10 | 2.81 | 1.00 | 0.31 |
|--------------+-------+------+-------+-------+------+------+------+------+------+------|
* EDS
#+BEGIN_SRC jupyter-python :var tbl=EDS_Energy_Table :results output :session py
print(tbl)
#+end_src
** EDS Energy Table
#+NAME: EDS_Energy_Table
#+CAPTION: Energy table for EDS analysis
| atomicNumber | name | Kalpha1 | Kalpha2 | Kbeta1 | Lalpha1 | Lalpha2 | Lbeta1 | Lbeta2 | Lgamma1 | Malpha1 |
|--------------+------+-----------+----------+----------+----------+-----------+----------+----------+----------+---------|
| 3 | Li | 54.3 | | | | | | | | |
| 4 | Be | 108.5 | | | | | | | | |
| 5 | B | 183.3 | | | | | | | | |
| 6 | C | 277 | | | | | | | | |
| 7 | N | 392.4 | | | | | | | | |
| 8 | O | 524.9 | | | | | | | | |
| 9 | F | 676.8 | | | | | | | | |
| 10 | Ne | 848.6 | 848.6 | | | | | | | |
| 11 | Na | 1040.98 | 1040.98 | 1071.1 | | | | | | |
| 12 | Mg | 1253.60 | 1253.60 | 1302.2 | | | | | | |
| 13 | Al | 1486.70 | 1486.27 | 1557.45 | | | | | | |
| 14 | Si | 1739.98 | 1739.38 | 1835.94 | | | | | | |
| 15 | P | 2013.7 | 2012.7 | 2139.1 | | | | | | |
| 16 | S | 2307.84 | 2306.64 | 2464.04 | | | | | | |
| 17 | Cl | 2622.39 | 2620.78 | 2815.6 | | | | | | |
| 18 | Ar | 2957.70 | 2955.63 | 3190.5 | | | | | | |
| 19 | K | 3313.8 | 3311.1 | 3589.6 | | | | | | |
| 20 | Ca | 3691.68 | 3688.09 | 4012.7 | 341.3 | 341.3 | 344.9 | | | |
| 21 | Sc | 4090.6 | 4086.1 | 4460.5 | 395.4 | 395.4 | 399.6 | | | |
| 22 | Ti | 4510.84 | 4504.86 | 4931.81 | 452.2 | 452.2 | 458.4 | | | |
| 23 | V | 4952.20 | 4944.64 | 5427.29 | 511.3 | 511.3 | 519.2 | | | |
| 24 | Cr | 5414.72 | 5405.509 | 5946.71 | 572.8 | 572.8 | 582.8 | | | |
| 25 | Mn | 5898.75 | 5887.65 | 6490.45 | 637.4 | 637.4 | 648.8 | | | |
| 26 | Fe | 6403.84 | 6390.84 | 7057.98 | 705.0 | 705.0 | 718.5 | | | |
| 27 | Co | 6930.32 | 6915.30 | 7649.43 | 776.2 | 776.2 | 791.4 | | | |
| 28 | Ni | 7478.15 | 7460.89 | 8264.66 | 851.5 | 851.5 | 868.8 | | | |
| 29 | Cu | 8047.78 | 8027.83 | 8905.29 | 929.7 | 929.7 | 949.8 | | | |
| 30 | Zn | 8638.86 | 8615.78 | 9572.0 | 1011.7 | 1011.7 | 1034.7 | | | |
| 31 | Ga | 9251.74 | 9224.82 | 10264.2 | 1097.92 | 1097.92 | 1124.8 | | | |
| 32 | Ge | 9886.42 | 9855.32 | 10982.1 | 1188.00 | 1188.00 | 1218.5 | | | |
| 33 | As | 10543.72 | 10507.99 | 11726.2 | 1282.0 | 1282.0 | 1317.0 | | | |
| 34 | Se | 11222.4 | 11181.4 | 12495.9 | 1379.10 | 1379.10 | 1419.23 | | | |
| 35 | Br | 11924.2 | 11877.6 | 13291.4 | 1480.43 | 1480.43 | 1525.90 | | | |
| 36 | Kr | 12649 | 12598 | 14112 | 1586.0 | 1586.0 | 1636.6 | | | |
| 37 | Rb | 13395.3 | 13335.8 | 14961.3 | 1694.13 | 1692.56 | 1752.17 | | | |
| 38 | Sr | 14165 | 14097.9 | 15835.7 | 1806.56 | 1804.74 | 1871.72 | | | |
| 39 | Y | 14958.4 | 14882.9 | 16737.8 | 1922.56 | 1920.47 | 1995.84 | | | |
| 40 | Zr | 15775.1 | 15690.9 | 17667.8 | 2042.36 | 2039.9 | 2124.4 | 2219.4 | 2302.7 | |
| 41 | Nb | 16,615.1 | 16,521.0 | 18,622.5 | 2,165.89 | 2,163.0 | 2,257.4 | 2,367.0 | 2,461.8 | |
| 42 | Mo | 17,479.34 | 17,374.3 | 19,608.3 | 2,293.16 | 2,289.85 | 2,394.81 | 2,518.3 | 2,623.5 | |
| 43 | Tc | 18,367.1 | 18,250.8 | 20,619 | 2,424 | 2,420 | 2,538 | 2,674 | 2,792 | |
| 44 | Ru | 19,279.2 | 19,150.4 | 21,656.8 | 2,558.55 | 2,554.31 | 2,683.23 | 2,836.0 | 2,964.5 | |
| 45 | Rh | 20,216.1 | 20,073.7 | 22,723.6 | 2,696.74 | 2,692.05 | 2,834.41 | 3,001.3 | 3,143.8 | |
| 46 | Pd | 21,177.1 | 21,020.1 | 23,818.7 | 2,838.61 | 2,833.29 | 2,990.22 | 3,171.79 | 3,328.7 | |
| 47 | Ag | 22,162.92 | 21,990.3 | 24,942.4 | 2,984.31 | 2,978.21 | 3,150.94 | 3,347.81 | 3,519.59 | |
| 48 | Cd | 23,173.6 | 22,984.1 | 26,095.5 | 3,133.73 | 3,126.91 | 3,316.57 | 3,528.12 | 3,716.86 | |
| 49 | In | 24,209.7 | 24,002.0 | 27,275.9 | 3,286.94 | 3,279.29 | 3,487.21 | 3,713.81 | 3,920.81 | |
| 50 | Sn | 25,271.3 | 25,044.0 | 28,486.0 | 3,443.98 | 3,435.42 | 3,662.80 | 3,904.86 | 4,131.12 | |
| 51 | Sb | 26,359.1 | 26,110.8 | 29,725.6 | 3,604.72 | 3,595.32 | 3,843.57 | 4,100.78 | 4,347.79 | |
| 52 | Te | 27,472.3 | 27,201.7 | 30,995.7 | 3,769.33 | 3,758.8 | 4,029.58 | 4,301.7 | 4,570.9 | |
| 53 | I | 28,612.0 | 28,317.2 | 32,294.7 | 3,937.65 | 3,926.04 | 4,220.72 | 4,507.5 | 4,800.9 | |
| 54 | Xe | 29,779 | 29,458 | 33,624 | 4,109.9 | | | | | |
| 55 | Cs | 30,972.8 | 30,625.1 | 34,986.9 | 4,286.5 | 4,272.2 | 4,619.8 | 4,935.9 | 5,280.4 | |
| 56 | Ba | 32,193.6 | 31,817.1 | 36,378.2 | 4,466.26 | 4,450.90 | 4,827.53 | 5,156.5 | 5,531.1 | |
| 57 | La | 33,441.8 | 33,034.1 | 37,801.0 | 4,650.97 | 4,634.23 | 5,042.1 | 5,383.5 | 5,788.5 | 833 |
| 58 | Ce | 34,719.7 | 34,278.9 | 39,257.3 | 4,840.2 | 4,823.0 | 5,262.2 | 5,613.4 | 6,052 | 883 |
| 59 | Pr | 36,026.3 | 35,550.2 | 40,748.2 | 5,033.7 | 5,013.5 | 5,488.9 | 5,850 | 6,322.1 | 929 |
| 60 | Nd | 37,361.0 | 36,847.4 | 42,271.3 | 5,230.4 | 5,207.7 | 5,721.6 | 6,089.4 | 6,602.1 | 978 |
| 61 | Pm | 38,724.7 | 38,171.2 | 43,826 | 5,432.5 | 5,407.8 | 5,961 | 6,339 | 6,892 | |
| 62 | Sm | 40,118.1 | 39,522.4 | 45,413 | 5,636.1 | 5,609.0 | 6,205.1 | 6,586 | 7,178 | 1,081 |
| 63 | Eu | 41,542.2 | 40,901.9 | 47,037.9 | 5,845.7 | 5,816.6 | 6,456.4 | 6,843.2 | 7,480.3 | 1,131 |
| 64 | Gd | 42,996.2 | 42,308.9 | 48,697 | 6,057.2 | 6,025.0 | 6,713.2 | 7,102.8 | 7,785.8 | 1,185 |
| 65 | Tb | 44,481.6 | 43,744.1 | 50,382 | 6,272.8 | 6,238.0 | 6,978 | 7,366.7 | 8,102 | 1,240 |
| 66 | Dy | 45,998.4 | 45,207.8 | 52,119 | 6,495.2 | 6,457.7 | 7,247.7 | 7,635.7 | 8,418.8 | 1,293 |
| 67 | Ho | 47,546.7 | 46,699.7 | 53,877 | 6,719.8 | 6,679.5 | 7,525.3 | 7,911 | 8,747 | 1,348 |
| 68 | Er | 49,127.7 | 48,221.1 | 55,681 | 6,948.7 | 6,905.0 | 7,810.9 | 8,189.0 | 9,089 | 1,406 |
| 69 | Tm | 50,741.6 | 49,772.6 | 57,517 | 7,179.9 | 7,133.1 | 8,101 | 8,468 | 9,426 | 1,462 |
| 70 | Yb | 52,388.9 | 51,354.0 | 59,370 | 7,415.6 | 7,367.3 | 8,401.8 | 8,758.8 | 9,780.1 | 1,521.4 |
| 71 | Lu | 54,069.8 | 52,965.0 | 61,283 | 7,655.5 | 7,604.9 | 8,709.0 | 9,048.9 | 10,143.4 | 1,581.3 |
| 72 | Hf | 55,790.2 | 54,611.4 | 63,234 | 7,899.0 | 7,844.6 | 9,022.7 | 9,347.3 | 10,515.8 | 1,644.6 |
| 73 | Ta | 57,532 | 56,277 | 65,223 | 8,146.1 | 8,087.9 | 9,343.1 | 9,651.8 | 10,895.2 | 1,710 |
| 74 | W | 59,318.24 | 57,981.7 | 67,244.3 | 8,397.6 | 8,335.2 | 9,672.35 | 9,961.5 | 11,285.9 | 1,775.4 |
| 75 | Re | 61,140.3 | 59,717.9 | 69,310 | 8,652.5 | 8,586.2 | 10,010.0 | 10,275.2 | 11,685.4 | 1,842.5 |
| 76 | Os | 63,000.5 | 61,486.7 | 71,413 | 8,911.7 | 8,841.0 | 10,355.3 | 10,598.5 | 12,095.3 | 1,910.2 |
| 77 | Ir | 64,895.6 | 63,286.7 | 73,560.8 | 9,175.1 | 9,099.5 | 10,708.3 | 10,920.3 | 12,512.6 | 1,979.9 |
| 78 | Pt | 66,832 | 65,112 | 75,748 | 9,442.3 | 9,361.8 | 11,070.7 | 11,250.5 | 12,942.0 | 2,050.5 |
| 79 | Au | 68,803.7 | 66,989.5 | 77,984 | 9,713.3 | 9,628.0 | 11,442.3 | 11,584.7 | 13,381.7 | 2,122.9 |
| 80 | Hg | 70,819 | 68,895 | 80,253 | 9,988.8 | 9,897.6 | 11,822.6 | 11,924.1 | 13,830.1 | 2,195.3 |
| 81 | Tl | 72,871.5 | 70,831.9 | 82,576 | 10,268.5 | 10,172.8 | 12,213.3 | 12,271.5 | 14,291.5 | 2,270.6 |
| 82 | Pb | 74,969.4 | 72,804.2 | 84,936 | 10,551.5 | 10,449.5 | 12,613.7 | 12,622.6 | 14,764.4 | 2,345.5 |
| 83 | Bi | 77,107.9 | 74,814.8 | 87,343 | 10,838.8 | 10,730.91 | 13,023.5 | 12,979.9 | 15,247.7 | 2,422.6 |
| 84 | Po | 79,290 | 76,862 | 89,800 | 11,130.8 | 11,015.8 | 13,447 | 13,340.4 | 15,744 | |
| 85 | At | 81,520 | 78,950 | 92,300 | 11,426.8 | 11,304.8 | 13,876 | | 16,251 | |
| 86 | Rn | 83,780 | 81,070 | 94,870 | 11,727.0 | 11,597.9 | 14,316 | | 16,770 | |
| 87 | Fr | 86,100 | 83,230 | 97,470 | 12,031.3 | 11,895.0 | 14,770 | 14,450 | 17,303 | |
| 88 | Ra | 88,470 | 85,430 | 100,130 | 12,339.7 | 12,196.2 | 15,235.8 | 14,841.4 | 17,849 | |
| 89 | Ac | 90,884 | 87,670 | 102,850 | 12,652.0 | 12,500.8 | 15,713 | | 18,408 | |
| 90 | Th | 93,350 | 89,953 | 105,609 | 12,968.7 | 12,809.6 | 16,202.2 | 15,623.7 | 18,982.5 | 2,996.1 |
| 91 | Pa | 95,868 | 92,287 | 108,427 | 13,290.7 | 13,122.2 | 16,702 | 16,024 | 19,568 | 3,082.3 |
| 92 | U | 98,439 | 94,665 | 111,300 | 13,614.7 | 13,438.8 | 17,220.0 | 16,428.3 | 20,167.1 | 3,170.8 |
| 93 | Np | | | | 13,944.1 | 13,759.7 | 17,750.2 | 16,840.0 | 20,784.8 | |
| 94 | Pu | | | | 14,278.6 | 14,084.2 | 18,293.7 | 17,255.3 | 21,417.3 | |
| 95 | Am | | | | 14,617.2 | 14,411.9 | 18,852.0 | 17,676.5 | 22,065.2 | |
* SEM SOP
** Stopping the Microscope
- Switch off the high voltage by clicking on the HV button in the Electron Beam panel.
- Remove your samples from the microscope.
- Pump the microscope.
- Close the program (use Exit from the File menu) select the Switch off (the microscope) and exit (the application) option.
- Wait until the VegaTC program closes itself. The microscope configuration will be automatically saved on the hard drive.
- Shut down OS Windows in the usual way.
- Turn the main switch to the left (OFF position).
** Loading of the sample
- Use only one gloved hand when handling samples and holders
- Avoid letting the sample holder or any part of the sample exchange rod touch non-clean surfaces which may be contaminated with hand-oil
- Never "blow on" or exhale on samples to dry them, use the IR lamp instead
- Always make sure all screws are tight and that you always have a sure grip
- Always ask if you have a question
** Images at Low Magnification
There are four factory presets for the accelerating voltage (5 kV, 10 kV, 20 kV, 30 kV), one
for each HV index. The user does not need to make any further adjustments by switching
among them and using magnification up to 4000x.
Click on the PUMP button in the Vacuum panel to start the pumping procedure
(Figure 2). It usually takes around 3 minutes to reach vacuum ready - status which
means that the microscope is ready to use. If there is a need to exchange the
specimen, follow the instructions in chapter 8.2.
[[download:20240310-112336_screenshot.png]]
In the SEM Detectors & Mixer panel select the appropriate detector from the list box
(Figure 3). We recommend using the SE or BSE detector. When the BSE detector is
used, make sure that the detector is not retracted! See chapter 6 for detailed infor-
mation
[[download:20240310-112456_screenshot.png]]
[[download:20240310-112616_screenshot.png]]
3. Select the accelerating voltage (30 kV recommended) using the combo box in the
Electron Beam panel (Figure 5).
4. Clicking on the HV button in the Electron Beam panel turns the high voltage on and
starts the heating of the tungsten filament (see Figure 5).
5. Right-click in the SEM Scanning window to open the menu and select the Minimum
Magnification function (Figure 6)
[[download:20240310-112645_screenshot.png]]
[[download:20240310-112723_screenshot.png]]
7 Select RESOLUTION mode (click on the Scan Mode function in the Info Panel (see
Figure 10) and select RESOLUTION or use the Continual Wide Field option – switches
automatically between WIDE FIELD and RESOLUTION mode and vice versa when
increasing or decreasing magnification)
Focus the image by clicking on the WD icon in the Toolbar and turning the
Trackball from left to right (or vice versa). Alternatively use the Auto WD function for
focusing (see Figure 6). Double-clicking (left mouse button) in the SEM Scanning
window opens the Focus window. To remove the Focus window double-click
anywhere in the SEM Scanning window.
To select beam intensity (BI 10 recommended), first left-click on the BI icon
on the Toolbar and then use the arrows in the Pad panel (Figure 8).
[[download:20240310-113043_screenshot.png]]
10. To select the sample position in the Stage Control panel, click on the appropriate
number button on the carousel (Figure 9) or use the manual knobs in the case of the
SB microscope type.
11. Placing the cursor over the SEM Scanning window and clicking the mouse wheel
moves that area on the stage into the centre of the image. See chapter 7.2 for other
mouse actions.
12. To magnify the image click on the Magnification icon on the Toolbar and turn
the Trackball from left to right.
13. Once the area of interest is magnified and focused as desired, right-click on the
Speed icon on the Toolbar and select the appropriate scanning speed.
14. Clicking on the Acquire button in the Info Panel (Figure 10) or on the icon
on the Toolbar saves the image. Fill in the note, sign and description field
if necessary. Choose a folder in which to store the image. To change the parameters
of the image use the Image Parameters function in the main SEM menu
[[download:20240310-113153_screenshot.png]]
[[download:20240310-113251_screenshot.png]]
5. Clicking on the icon opens the dialogue for saving the actual adjustment of the
microscope. It is possible to restore the saved adjustment of the microscope later.
** Images at High Magnification
The best resolution is achieved at the highest accelerating voltage (30 kV) of the primary
electrons.
1. Insert an appropriate sample for high magnification images (e.g. tin on carbon
sample, Figure 18).
2. Select the fourth HV index using the combo box in the Electron Beam panel (20 kV -
30 kV) and turn on the high voltage.
3. Focus the image in RESOLUTION mode (click on the Scan Mode function in the Info
Panel and select RESOLUTION or use the Continual Wide Field option).
Note: Use the Degauss column function by means of the icon before changing WD&Z or WD. The image should remain in focus.
Check the spot size, which is determined by the BI value. Right-click in the SEM
Scanning window to select the optimum BI value – Auto BI OptiMag.
5. For the best resolution, it is necessary to work at a short working distance (WD). The
optimum WD is about 5 mm for the SE detector (in the case that the BSE is not
mounted underneath the objective lens). For BSE images the optimum WD is about
8.5 mm. To change the working distance together with Z-axis, without defocusing
the image, use the WD&Z function in the Stage Control panel (Figure 15).
WARNING: Moving the manipulator with the specimen can cause it to collide with other inner
components of the microscope and can cause damage to the microscope. Control the
movements of the manipulator by video camera imaging (open the Chamber View by clicking
on the
icon). The manipulator's movement can be stopped by clicking on the Stop
button in the Stage Control panel (see Figure 15).
[[download:20240310-113624_screenshot.png]]
Gradually magnify and focus the image to achieve 10kx magnification. In the case
that the image is moving during focusing, it is necessary to check the centering
of the objective. Select the Manual Column Centering function using the combo box
in the Electron Beam panel after clicking on the Adjustment >>> button (Figure 16).
The Manual Centering Wizard window will appear (Figure 17). Clicking on the WOB
button opens the Focus window in the SEM Scanning window. Click on the Next>>
button to obtain the next instructions. The function of the centering has two adjust-
able values. To be sure just one value is changing, hold down the F12 key to change
only X movement at the Trackball, and the F11 key to change only Y movement.
7. Each time that the image is too dark or light it is necessary to use the Auto Signal
function (see Figure 6 or use the icon ). To set the contrast and brightness
manually, click on the icon and use the Trackball.
[[download:20240310-113731_screenshot.png]]
[[download:20240310-113752_screenshot.png]]
At higher magnifications (>10kx) it is necessary to check if astigmatism (Figure 18
(a), (b)) is precisely corrected (Figure 18 (c)). To correct astigmatism click on the
Stigmator function in the Info Panel (Figure 19). For precise correction use the Focus
window (in the SEM Scanning window) and the F11 and F12 keys in the same way
as in point 6.
[[download:20240310-113907_screenshot.png]]
9. Select the appropriate scanning speed and save the image.
10. Clicking on the icon opens the dialog for saving the current adjustment of the
microscope. It is possible to restore the saved adjustment of the microscope later.
[[download:20240310-113937_screenshot.png]]
** Specimen Exchange
The specimen should somehow be fixed or glued to the specimen stub before it is inserted into the chamber. It is possible to use 12.5 mm specimen stubs or any other specimen holders, delivered as microscope accessories (see chapter 9.7).
If the specimen is examined in high vacuum mode, it must be conductive or must be made conductive using one of the methods described in the technical information. The conductive surface of the specimen must be conductive contacted to the stub.
Non-conductive samples can be investigated in low vacuum mode.
Instructions:
1. Vent the microscope by using the VENT button in the Vacuum panel. Wait until the pressure is at atmospheric level.
2. Set the tilt of the specimen stage to zero.
3. Open the chamber door by gently pulling it.
4. The automatic positions set up in the Stage Control panel can be used, which are intended for specimen position exchange. To select the sample position click on the appropriate number button on the carousel. At this time the button background is red to indicate the specimen exchange mode.

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Excellent lectures by Dr Jeffrey C Grossman that describes the ideas behind X-ray really well.
[[https://youtu.be/AqCz_b7VJK8?si=jPZq8In1ABTT4xnI][MIT 3.091 | 21. X-ray Diffraction Techniques I (Intro to Solid-State Chemistry)]]
[[https://youtu.be/S1kqa_qGmHs?si=b8_KITp6ivQIpCQF][MIT 3.091 | 22. X-ray Diffraction Techniques II (Intro to Solid-State Chemistry)]]
Copper K-α is an x-ray energy frequently used on labscale x-ray instruments. The energy is 8.04 keV, which corresponds to an x-ray wavelength of 1.5406 Å.
This causes the prefactor in the scattering equation to be:
k = 2 π λ = 4.0784 Å − 1 {\displaystyle k={\frac {2\pi }{\lambda }}=4.0784\,\mathrm {\AA} ^{-1}}
X-Ray Diffraction
A Practical Approach
Authors:
C. Suryanarayana , M. Grant Norton
Excellent lectures by Dr Jeffrey C Grossman that describes the ideas behind X-ray really well.
[[https://youtu.be/AqCz_b7VJK8?si=jPZq8In1ABTT4xnI][MIT 3.091 | 21. X-ray Diffraction Techniques I (Intro to Solid-State Chemistry)]]
[[https://youtu.be/S1kqa_qGmHs?si=b8_KITp6ivQIpCQF][MIT 3.091 | 22. X-ray Diffraction Techniques II (Intro to Solid-State Chemistry)]]
Copper K-α is an x-ray energy frequently used on labscale x-ray instruments. The energy is 8.04 keV, which corresponds to an x-ray wavelength of 1.5406 Å.
This causes the prefactor in the scattering equation to be:
k = 2 π λ = 4.0784 Å − 1 {\displaystyle k={\frac {2\pi }{\lambda }}=4.0784\,\mathrm {\AA} ^{-1}}
X-Ray Diffraction
A Practical Approach
Authors:
C. Suryanarayana , M. Grant Norton