WO2011159264A1 - A thickness determination method - Google Patents
A thickness determination method Download PDFInfo
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- WO2011159264A1 WO2011159264A1 PCT/TR2010/000113 TR2010000113W WO2011159264A1 WO 2011159264 A1 WO2011159264 A1 WO 2011159264A1 TR 2010000113 W TR2010000113 W TR 2010000113W WO 2011159264 A1 WO2011159264 A1 WO 2011159264A1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B15/00—Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons
- G01B15/02—Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons for measuring thickness
Definitions
- This invention is about a method for measuring thickness with electron microscopes using energy dispersive X-ray spectrometer.
- Electron microscopes used today are used to analyze all kinds of material surfaces and the elements contained in these materials. Elemental analysis can especially be used for detection of the contents of mixtures of unknown content, or of unknown ratios.
- Said electron microscopes use electrons with different powers to perform their duties explained above by capturing electrons penetrating into the depths of the material and scattering back out and photons at different wavelengths, generated by the excited electrons.
- what the depth that the electrons penetrate is or what the depth of atoms that the electrons interact with to cause emission of photons is not known.
- EP1867949B1 a method using electron beams of precise energies that will only interact with the layer to be examined is explained. Use of electron beams accelerated with 3-6kV on coatings of 10-lOOnm thickness is explained. This method also makes use of wavelength dispersive X-ray spectroscopy, limiting its use.
- the invention described in the document numbered DE4211394A1 makes use of energy dispersive X-ray spectroscopy. This method is based on the proportions between the l coating and substrate interaction volumes corresponding to the measured X-ray intensities. It is assumed that the interaction volume of the substrate is hemispherical and the interaction volume of the coating is relatively small. Because of this assumption, only an approximate result can be obtained. Moreover, since, as the thickness increase, this approximation will further deviate, this method can be applied to limited thicknesses.
- the invention is related to a method to be used for thickness determination of thin films with an electron microscope, which makes use energy dispersive X-ray spectroscopy.
- a spectrum of X-rays resulting from the interaction of the coated substrate to be investigated with an electron beam of known energy is built up by an energy dispersive X- ray spectroscope and the element ratios are obtained. From these data, elemental ratio vs. electron beam energy curves are obtained. These curves, which are unique for each specific element and thickness of coating, allows the creation of reference curves to determine the coating thickness from known samples.
- Figure 1 is an example table of the measurement table contained in the thickness determination method according to the invention.
- Figure 2 is an example graph of reference curves of voltage vs. gold ratio corresponding to eight different thicknesses of gold layers, obtained using the thickness determination method according to the invention.
- Figure 3 is an example graph with three reference curves of voltage vs. thickness for a specific coating obtained using the thickness determination method according to the invention, where a measurement curve produced by interpolation of three different points corresponding to measurements is shown.
- Figure 4 is an example graph where three reference curves of voltage vs. thickness for a specific coating and a measurement curve obtained using the thickness determination method according to the invention are shown intersected by a ratio line parallel to the horizontal axis.
- Figure 5 is an example graph where the Voltage-Thickness (VT) curves produced by interpolation of thickness vs. voltage data obtained by intersecting the reference curves obtained using the thickness determination method according to the invention with the horizontal ratio line, are shown.
- VT Voltage-Thickness
- Figure 6 is the appearance of a projection modeling of the electron orbits following bombardment by electron beams of three different energies obtained by the Monte Carlo simulations contained in the thickness determination method according to the invention.
- the thickness determination method essentially, an electron microscope, an energy dispersive X-ray spectrometer (EDS) and a control unit executing this method are required.
- EDS energy dispersive X-ray spectrometer
- the thickness determination method on the material whose thickness is to be measured is not any different than any measurement performed with an electron microscope; since like other measurements and investigations performed with electron microscopy the procedures concerning placement of the material to be examined into the electron microscope, the process of sending electrons onto the material and the subsequent X-ray analysis are the same. However this invention makes a difference in investigating the X-ray data retrieved from the material.
- the operating method of the electron microscope that is already known and used with the thickness determination method according to the present invention is performed as follows. Analysis of materials using scanning electron microscopes involves targeting a sample with beams of energetic electrons acquired by applying a voltage. The results of the interaction between the sample and the beam are then investigated to provide for the desired data. The volume of the penetrated region is determined by the energy of the beam as seen in Figure 1.
- the X-rays are counted by a detector and a spectrum is constructed.
- the energy dispersive X-ray spectrometer normalizes and corrects the data using the ZAF coefficients. From these data, since they are unique for each element, the atomic ratios of the elements present in the penetrated region of the sample are obtained.
- the element/compound whose thickness is to be measured or the element/compound that it was coated on is not necessarily known as the spectrum obtained from the EDS already shows the peaks corresponding to the contained elements.
- the thickness determination method operates using the information on determined elements and the ratios of these elements. As well as this information, the energies of electrons sent to the material are also required to be known.
- the device to determine the steps of said method and the thickness using the data mentioned above is the control unit. This unit in order to execute steps of the thickness determination method can be a programmed/programmable electronic circuit or a computer software running on a computer with an operating system.
- the thickness determination method operates as follows.
- determining the kinds and ratios of the elements/compounds contained in the material and from these values determining the ratio of the coating material more accurately can be achieved from the measurement data such as Oi or 0 2 obtained from the X-ray data, when being recorded to the table, using various correction coefficients.
- the invention in relevance to the problem of producing a reference table according to the application above, there also exists a second application allowing construction of the reference table by modeling.
- the mentioned application is the modeling data generation method Penetration .into the sample consisting of layers of certain elements varies in proportion to the electron energy and in inverse proportion to the density of the element. For many elements, said variations are known and various computational tools making use of certain modeling techniques constructed using these variation rates that statistically demonstrate the penetration depth into the sample according to the electron energy are known.
- One of these is the Monte Carlo simulation. With such simulations penetration depth of each electron can be determined, using random numbers.
- a modeling graph similar to the reference graph can be constructed.
- merely modeling graphs to be taken as reference can be constructed by modeling.
- the reference curves contained in said modeling graphs can be used as those described in the steps of the thickness determination method.
Abstract
This invention is about a method for measuring the thickness with electron microscopes using energy dispersive X-ray spectrometer. A spectrum of X-rays resulting from the interaction of the coated substrate to be investigated with an electron beam of known energy is built up by an energy dispersive X-ray spectroscope and the element ratios are obtained. From these data, elemental ratio vs. electron beam energy curves are obtained. These curves, which are unique for each specific element and thickness of coating, allows the creation of reference curves to determine the thickness of the coating from known samples.
Description
A THICKNESS DETERMINATION METHOD
Technical Field
This invention is about a method for measuring thickness with electron microscopes using energy dispersive X-ray spectrometer.
Prior Art
Electron microscopes used today are used to analyze all kinds of material surfaces and the elements contained in these materials. Elemental analysis can especially be used for detection of the contents of mixtures of unknown content, or of unknown ratios.
Said electron microscopes use electrons with different powers to perform their duties explained above by capturing electrons penetrating into the depths of the material and scattering back out and photons at different wavelengths, generated by the excited electrons. However in this process, what the depth that the electrons penetrate is or what the depth of atoms that the electrons interact with to cause emission of photons is not known.
In industries relating to electronic semiconductors, optical coatings and photovoltaic cells, etc. thin films have found important application fields. The high quality requirements of these industries can be met with high precision measurements of thin films thicknesses. In this context, some methods that make use of X-rays obtained by electron excitation are discussed below.
In the document numbered WO0195365A1, use of a wavelength dispersive X-ray spectroscope for testing the thickness of specific layered products is described. Therefore, using the relevant apparatus, measurements relating only to known materials can be performed.
In the document numbered EP1867949B1 a method using electron beams of precise energies that will only interact with the layer to be examined is explained. Use of electron beams accelerated with 3-6kV on coatings of 10-lOOnm thickness is explained. This method also makes use of wavelength dispersive X-ray spectroscopy, limiting its use.
The invention described in the document numbered DE4211394A1, makes use of energy dispersive X-ray spectroscopy. This method is based on the proportions between the l
coating and substrate interaction volumes corresponding to the measured X-ray intensities. It is assumed that the interaction volume of the substrate is hemispherical and the interaction volume of the coating is relatively small. Because of this assumption, only an approximate result can be obtained. Moreover, since, as the thickness increase, this approximation will further deviate, this method can be applied to limited thicknesses.
Brief Description of the Invention
The invention is related to a method to be used for thickness determination of thin films with an electron microscope, which makes use energy dispersive X-ray spectroscopy.
A spectrum of X-rays resulting from the interaction of the coated substrate to be investigated with an electron beam of known energy, is built up by an energy dispersive X- ray spectroscope and the element ratios are obtained. From these data, elemental ratio vs. electron beam energy curves are obtained. These curves, which are unique for each specific element and thickness of coating, allows the creation of reference curves to determine the coating thickness from known samples.
Detailed Description of the Invention
The method realized and the graphs produced and used according to this method to achieve the objectives of the invention, are shown in the attached drawings where;
Figure 1 is an example table of the measurement table contained in the thickness determination method according to the invention.
Figure 2 is an example graph of reference curves of voltage vs. gold ratio corresponding to eight different thicknesses of gold layers, obtained using the thickness determination method according to the invention.
Figure 3 is an example graph with three reference curves of voltage vs. thickness for a specific coating obtained using the thickness determination method according to the invention, where a measurement curve produced by interpolation of three different points corresponding to measurements is shown.
Figure 4 is an example graph where three reference curves of voltage vs. thickness for a specific coating and a measurement curve obtained using the thickness determination method according to the invention are shown intersected by a ratio line parallel to the horizontal axis.
Figure 5 is an example graph where the Voltage-Thickness (VT) curves produced by interpolation of thickness vs. voltage data obtained by intersecting the reference curves obtained using the thickness determination method according to the invention with the horizontal ratio line, are shown.
Figure 6 is the appearance of a projection modeling of the electron orbits following bombardment by electron beams of three different energies obtained by the Monte Carlo simulations contained in the thickness determination method according to the invention.
For the thickness determination method to be applied, essentially, an electron microscope, an energy dispersive X-ray spectrometer (EDS) and a control unit executing this method are required.
Using the thickness determination method on the material whose thickness is to be measured is not any different than any measurement performed with an electron microscope; since like other measurements and investigations performed with electron microscopy the procedures concerning placement of the material to be examined into the electron microscope, the process of sending electrons onto the material and the subsequent X-ray analysis are the same. However this invention makes a difference in investigating the X-ray data retrieved from the material.
The operating method of the electron microscope that is already known and used with the thickness determination method according to the present invention is performed as follows. Analysis of materials using scanning electron microscopes involves targeting a sample with beams of energetic electrons acquired by applying a voltage. The results of the interaction between the sample and the beam are then investigated to provide for the desired data. The volume of the penetrated region is determined by the energy of the beam as seen in Figure 1.
When the sample is exposed by the beam, energy is transferred from the beam to the sample, exciting inner electrons of the atoms to be analyzed. As the electrons rearrange in favor of lower energy levels, atoms emit X-rays with atom-specific wavelengths from their Κα, Κβ, , etc. shells which are of interest when incorporating energy dispersive X-ray spectroscopy.
The X-rays are counted by a detector and a spectrum is constructed. The energy dispersive X-ray spectrometer normalizes and corrects the data using the ZAF coefficients. From these data, since they are unique for each element, the atomic ratios of the elements present in the penetrated region of the sample are obtained.
In a preferred application of the invention, the element/compound whose thickness is to be measured or the element/compound that it was coated on is not necessarily known as the spectrum obtained from the EDS already shows the peaks corresponding to the contained elements.
The thickness determination method according to the invention operates using the information on determined elements and the ratios of these elements. As well as this information, the energies of electrons sent to the material are also required to be known. The device to determine the steps of said method and the thickness using the data mentioned above is the control unit. This unit in order to execute steps of the thickness determination method can be a programmed/programmable electronic circuit or a computer software running on a computer with an operating system.
The thickness determination method operates as follows.
1. Sending an electron beam with an energy predetermined according to the kind of the material whose thickness is to be determined or the type of the electron microscope, or preferably at a 3-30 keV range, and recording this electron value in the measurement table as Ei.
2. Collecting data of X-rays scattered to the surroundings from the excited electrons resulting from the interaction of the electron beam with the material.
3. Determining the kinds and ratios of the elements/compounds present in the material using the X-ray data obtained and various correction factors, and among these values recording the ratio of the coating material to the measurement table as Oi.
4. Directing an electron beam of energy E2 different from the electron energy value of the first step, Ei on the material and recording this E2 value to the measurement table.
5. Collecting data of X-rays scattered to the surroundings from the excited electrons resulting from the interaction of the electron beam with the material.
6. Determining the kinds and ratios of the elements/compounds present in the material using the second X-ray data obtained and various correction factors, and among these values recording the ratio of the coating material to the measurement table as 02.
Directing an , electron beam of energy E3 different from the electron energy value of the first and fourth steps, Ei and E2 on the material and recording this E3 value to the measurement table.
Collecting data of X-rays scattered to the surroundings from the excited electrons resulting from the interaction of the electron beam with the material.
Determining the kinds and ratios of the elements/compounds present in the material using the third X-ray data obtained and various correction factors, and among these values recording the ratio of the coating material to the measurement table as 03. Producing the reference graph by inserting the element/compound ratios obtained by sending onto samples, coated with the element or compound, whose thickness is being measured, of thickness of preferably 1000-3000 nm with a certain difference with each other and of at least two and preferably eight different thicknesses, electron beams of energy preferably in the range 3 keV to 30 keV of at least three and preferably eight different energies.
For every thickness, drawing the eight reference curves passing through determined points on the reference graph by using interpolation.
Producing a measurement curve, using the reference table containing the corresponding ratios and the Oi, 02 and 03 values corresponding to the Ei, E2 and E3 values, having a similar curvature to the eight reference curves, between two different reference curves by interpolation.
Drawing a horizontal line at a particular ratio value On, preferably between 20 % and 80 % on the reference graph.
Marking every VT point on the voltage-thickness graph using the keV values ERi-8 of the eight points Ri-8 on the reference curves corresponding to the intersections with the horizontal ratio line OU and the thickness values KRI.
Producing the voltage-thickness (VT) curve by interpolation between the determined points.
Determining the voltage value Emi on the reference graph intersected by the horizontal ratio line OU.
Determining the thickness value Ki on the VT curve in the VT graph corresponding to the value Emi.
18. Drawing a horizontal line at a particular ratio value Or2 different from the ratio On, preferably between 20 % and 80 % on the reference graph.
19. Marking every VT point on the voltage-thickness graph using the keV values E s of the eight points RVs on the reference curves corresponding to the intersections with the horizontal ratio line OL2 and the thickness values KRI.
20. Producing the voltage-thickness (VT) curve by interpolation between the determined points.
21. Determining the voltage value Em2 on the reference graph intersected by the horizontal ratio line OL2.
22. Determining the thickness value K2 on the VT curve in the VT graph corresponding to the value Em2.
23. Obtaining the average K that is the coating thickness value by taking the arithmetic average of the values Ki and K2.
The thickness value "K" obtained from the average of Ki and K2 which were found by executing the method steps listed above, is the thickness of our sample with unknown thickness. By increasing the number of these repetitive steps of measuring and calculating, the accuracy of determination can be increased.
For this purpose, by finding more than two Kn values through repetition of the steps for determination of Ki and K2 values more than twice and taking the arithmetic average of these Kn values, a more accurate thickness determination can be performed. Moreover using the Kn values obtained, standard deviation can also be determined that is the margin of error can also be found.
In order to improve the precision of determination, determining the kinds and ratios of the elements/compounds contained in the material and from these values determining the ratio of the coating material more accurately can be achieved from the measurement data such as Oi or 02 obtained from the X-ray data, when being recorded to the table, using various correction coefficients.
The invention, in relevance to the problem of producing a reference table according to the application above, there also exists a second application allowing construction of the reference table by modeling. The mentioned application is the modeling data generation method
Penetration .into the sample consisting of layers of certain elements varies in proportion to the electron energy and in inverse proportion to the density of the element. For many elements, said variations are known and various computational tools making use of certain modeling techniques constructed using these variation rates that statistically demonstrate the penetration depth into the sample according to the electron energy are known. One of these is the Monte Carlo simulation. With such simulations penetration depth of each electron can be determined, using random numbers.
However, for the Monte Carlo simulation to be applied, a range or a probabilistic distribution is needed from which the random numbers are to be selected; since for each electron sent onto the material, the probability for it to reach a depth of the material is different from that of another depth. Also, these probabilities will change together with the electron energy. The reason for this is the electron's penetration into the depths of the material after colliding with atoms with elastic and inelastic collisions after entering the material. Said collisions and the number of collisions during the progress are directly proportional to the electron energies. The number of these collisions and the possible orientations inside the material in advance, according to the above, especially the density, can be estimated.
Using said density and collision number along with an average collision value to be determined, the atoms to which the electron will collide and at an atom at which last depth it will stop after energy transfers happening consequently, can be found with an electron projection determination study put together using the Monte Carlo simulation.
Moreover using this simulation, how the electron will pass through layers of different thicknesses and at which depth and at which element it will transfer its energy can also be determined statistically. With this modeling, instead of a reference table to be constructed by conducting 3000 different experiments, it is possible to construct a modeling data table by a modeling data generation method performing merely mathematical calculations in, relatively, a very short time.
The modeling data generation method described above in detail is described below step by step.
1. Determining the element or for compounds the elements with relative ratios of the material whose thickness is to be measured.
2. If there are no other layers in between, determining the element or for compounds the elements with relative ratios of the substrate.
3. If there are other layers in between, before the substrate determining the element or for compounds the elements with relative ratios of these layers.
4. Executing the modeling containing the Monte Carlo simulation to determine how much an electron will penetrate into the material proportional to its energy.
5. Recording all the thickness and energy values close to the possible thicknesses of the material whose thickness is investigated and to the electron energy values used during the thickness measurements, obtained using the model, with the code Mxkevynm in the modeling table, for example, the element ratio obtained from the X-rays scattered to the surroundings by an electron beam transmitted with a lOkeV of energy penetrating a material of thickness lOnm is recorded in the cell Mi0kevionm-
6. In order to compare the corresponding ratios in the steps above with the Oi and 02 ratios corresponding to the Ei value used;
a. Finding the thickness values corresponding to two different ratios, the closest smaller Mxkev ynm and the closest larger M(x +i)kev (y +i)nm from the ratio Oi corresponding to energy value Ei.
b. Defining the arithmetic average of the thickness value corresponding to Mxke ynm and the thickness value corresponding to M X +i)kev (y -n)nm as Ki. c. Finding the thickness values corresponding to two different ratios, the closest smaller M'xkev ynm and the closest larger M'x +i)keV (y +i)nm from the ratio 02 corresponding to energy value E2.
d. Defining the arithmetic average of the thickness value corresponding to 'xkev ynm and the thickness value corresponding to M'(x +1)keV (y +1)nm as K2. e. Obtaining the average K that is the coating thickness value by taking the arithmetic average of the values Ki and K2.
Since the modeling data table obtained by using the steps listed above is prepared on a computer, using various algorithms from the results of mathematical calculations, it will both be fast and more target-oriented, requiring less computation. This target-oriented modeling data is therefore given in the example in the figure to display 4*6 that is 24 different data.
Using the generated modeling data table, a modeling graph similar to the reference graph can be constructed. In this way, instead of producing different thicknesses of the samples, merely modeling graphs to be taken as reference can be constructed by modeling.
The reference curves contained in said modeling graphs can be used as those described in the steps of the thickness determination method.
Using the data obtained with intervals of 5nm and IkeV or data obtained with even larger intervals in the first application of the thickness determination method according to the invention, it has been disclosed that, will increase measurement errors. In order to decrease said measurement errors, intermediate values must be found. These values, instead of being found by experimenting, can be found by the modeling data generation method.
The thickness determination method according to the invention cannot be limited to the above examples employed for a better explanation of the subject. The invention is essentially as stated in the claims.
Claims
1. A thickness determination method characterized by the steps;
- sending an electron beam with an energy predetermined according to the kind of the material whose thickness is to be determined or the type of the electron microscope, or preferably at a 3-30 keV range, and recording this electron value in the measurement table as Ei,
- collecting data of X-rays scattered to the surroundings from the excited electrons resulting from the interaction of the electron beam with the material,
- determining the kinds and ratios of the elements/compounds present in the material using the X-ray data obtained and among these values recording the ratio of the coating material to the measurement table as Oi,
- directing an electron beam of energy E2 different from the electron energy value of the first step, Ei on the material and recording this E2 value to the measurement table,
- collecting data of X-rays scattered to the surroundings from the excited electrons resulting from the interaction of the electron beam with the material,
- determining the kinds and ratios of the elements/compounds present in the material using the second X-ray data obtained and among these values recording the ratio of the coating material to the measurement table as 02,
- directing an electron beam of energy E3 different from the electron energy value of the first and fourth steps, Ei and E2 on the material and recording this E3 value to the measurement table,
- collecting data of X-rays scattered to the surroundings from the excited electrons resulting from the interaction of the electron beam with the material,
- determining the kinds and ratios of the elements/compounds present in the material using the third X-ray data obtained and among these values recording the ratio of the coating material to the measurement table as 03,
- producing the reference graph by inserting the element/compound ratios obtained by sending onto samples, coated with the element or compound, whose thickness is being measured, of thickness of preferably 1000-3000 nm with a certain difference with each other and of at least two and preferably eight different thicknesses, electron beams of energy preferably in the range 3 keV to 30 keV of at least three and preferably eight different energies,
- for every thickness, drawing the eight reference curves passing through determined points on the reference graph by using interpolation,
- producing a measurement curve, using the reference table containing the corresponding ratios and the Oi, 02 and 03 values corresponding to the Ei, E2 and E3 values, having a similar curvature to the eight reference curves, between two different reference curves by interpolation,
- drawing a horizontal line at a particular ratio value On, preferably between 20 % and 80 % on the reference graph,
- marking every VT point on the voltage-thickness graph using the keV values ERi-8 of the eight points Ri-8 on the reference curves corresponding to the intersections with the horizontal ratio line OU and the thickness values KRI,
- producing the voltage-thickness (VT) curve by interpolation between the determined points,
- determining the voltage value Emi on the reference graph intersected by the horizontal ratio line OU,
- determining the thickness value Ki on the VT curve in the VT graph corresponding to the value Emi,
- drawing a horizontal line at a particular ratio value Or2 different from the ratio On, preferably between 20 % and 80 % on the reference graph,
- marking every VT point on the voltage-thickness graph using the keV values EVs of the eight points R'i-8 on the reference curves corresponding to the intersections with the horizontal ratio line OL2 and the thickness values KRI,
- producing the voltage-thickness (VT) curve by interpolation between the determined points,
- determining the voltage value Em2 on the reference graph intersected by the horizontal ratio line OL2,
- determining the thickness value K2 on the VT curve in the VT graph corresponding to the value Em2, - obtaining the average K that is the coating thickness value by taking the arithmetic average of the values Ki and K2,
for thickness measurements to be performed with an electron microscope.
2. A thickness determination method as in Claim 1, characterized by the step;
- determining the kinds and ratios of the elements/compounds present in the material and, from these values, the ratio of the coating material more precisely using various correction coefficients when recording the third X-ray data such as Oi or 02 in the table,
to increase measurement precision.
3. A thickness determination method as in Claim 1 or 2, characterized by the step;
- finding more than two K„ values by repeating the steps related to finding K i and K 2 values more than twice and performing a more precise thickness determination by finding the arithmetic average of the Kn values,
to increase measurement precision.
4. A thickness determination method characterized by the steps;
- sending an electron beam with an energy predetermined according to the kind of the material whose thickness is to be determined or the type of the electron microscope, or preferably at a 3-30 keV range, and recording this electron value in the measurement table as Ei,
- collecting data of X-rays scattered to the surroundings from the excited electrons resulting from the interaction of the electron beam with the material,
- determining the kinds and ratios of the elements/compounds present in the material using the X-ray data obtained and among these values recording the ratio of the coating material to the measurement table as Oi,
- directing an electron beam of energy E2 different from the electron energy value of the first step, Ei on the material and recording this E2 value to the measurement table,
- collecting data of X-rays scattered to the surroundings from the excited electrons resulting from the interaction of the electron beam with the material, determining the kinds and ratios of the elements/compounds present in the material using the second X-ray data obtained and among these values recording the ratio of the coating material to the measurement table as 02,
directing an electron beam of energy E3 different from the electron energy value of the first and fourth steps, Ei and E2 on the material and recording this E3 value to the measurement table,
collecting data of X-rays scattered to the surroundings from the excited electrons resulting from the interaction of the electron beam with the material,
determining the kinds and ratios of the elements/compounds present in the material using the third X-ray data obtained and among these values recording the ratio of the coating material to the measurement table as 03,
in order to construct a modeling table for the elements subject to measurement;
• determining the element or for compounds the elements with relative ratios of the material whose thickness is to be measured,
• if there are no other layers in between, determining the element or for compounds the elements with relative ratios of the substrate,
• executing the modeling containing the Monte Carlo simulation to determine how much an electron will penetrate into the material proportional to its energy,
• recording all the thickness and energy values close to the possible thicknesses of the material whose thickness is investigated and to the electron energy values used during the thickness measurements, obtained using the model, with the code MxkeVynm in the modeling table,
constructing a modeling graph using the modeling table,
producing a measurement curve, using the reference table containing the corresponding ratios and the Oi, 02 and 03 values corresponding to the Ei, E2 and E3 values, having a similar curvature to the reference curves of the modeling table between two different reference curves by interpolation,
drawing a horizontal line at a particular ratio value Orl, preferably between 20 % and 80 % on the reference graph, - marking every VT point on the voltage-thickness graph using the keV values ERi-8 of the eight points Ri-8 on the reference curves corresponding to the intersections with the horizontal ratio line OU and the thickness values KRI,
- producing the voltage-thickness (VT) curve by interpolation between the determined points,
- determining the voltage value Emi on the reference graph intersected by the horizontal ratio line OI_i,
- determining the thickness value Ki on the VT curve in the VT graph corresponding to the value Emi,
- drawing a horizontal line at a particular ratio value Or2 different from the ratio Ori, preferably between 20 % and 80 % on the reference graph,
- marking every VT point on the voltage-thickness graph using the keV values E'RI-S of the eight points R'i-8 on the reference curves corresponding to the intersections with the horizontal ratio line OL2 and the thickness values KRI,
- producing the voltage-thickness (VT) curve by interpolation between the determined points,
- determining the voltage value EM2 on the reference graph intersected by the horizontal ratio line OL2,
- determining the thickness value K2 on the VT curve in the VT graph corresponding to the value EM2,
- obtaining the average K that is the coating thickness value by taking the arithmetic average of the values Ki and K2,
for thickness measurements to be performed with an electron microscope.
5. A thickness determination method as in Claim 4 characterized by the step;
- determining the element or for compounds the elements with relative ratios of these layers,
if there are other layers in between, before the substrate.
6. A thickness determination method as in Claim 4, characterized by the step;
- determining the kinds and ratios of the elements/compounds present in the material and, from these values, the ratio of the coating material more precisely using various correction coefficients when recording the third X-ray data such as Oi or 02 in the table,
to increase measurement precision.
7. A thickness determination method as in Claim 4 or 6, characterized by the step;
- finding more than two Kn values by repeating the steps related to finding K i and K 2 values more than twice and performing a more precise thickness determination by finding the arithmetic average of the K„ values,
to increase measurement precision.
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| PCT/TR2010/000113 WO2011159264A1 (en) | 2010-06-15 | 2010-06-15 | A thickness determination method |
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| PCT/TR2010/000113 WO2011159264A1 (en) | 2010-06-15 | 2010-06-15 | A thickness determination method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103759680A (en) * | 2013-12-31 | 2014-04-30 | 中国石油天然气股份有限公司 | Method for measuring occurrence thickness of oil film in tight reservoir micro-nano pore throat |
| CN103954243A (en) * | 2014-04-22 | 2014-07-30 | 北京理工大学 | Rotation seal boundary film thickness measuring method |
| CN113916924A (en) * | 2021-10-11 | 2022-01-11 | 中南大学 | Composite steel joint surface defining method, evaluation method, device and storage medium |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103759680A (en) * | 2013-12-31 | 2014-04-30 | 中国石油天然气股份有限公司 | Method for measuring occurrence thickness of oil film in tight reservoir micro-nano pore throat |
| CN103954243A (en) * | 2014-04-22 | 2014-07-30 | 北京理工大学 | Rotation seal boundary film thickness measuring method |
| CN113916924A (en) * | 2021-10-11 | 2022-01-11 | 中南大学 | Composite steel joint surface defining method, evaluation method, device and storage medium |
| CN113916924B (en) * | 2021-10-11 | 2023-02-17 | 中南大学 | Composite steel joint surface defining method, evaluation method, device and storage medium |
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