SJ/T 10457-1993 Standard Guide for Depth Profiling by Auger Electron Spectroscopy SJ/T10457-1993 Standard download decompression password: www.bzxz.net

Electronic Industry Standard of the People's Republic of China
SJ/T10457--93
Standard guide for depth profiling in auger electron spectroscopyIssued on December 17, 1993
Implemented on June 1, 1994
Issued by the Ministry of Electronics Industry of the People's Republic of ChinaInternational Standard of the Electronic Industry of the People's Republic of China
Standard guide for depth profiling in augerelectron spectroscopy1 Content and scope of application
1.1 Subject content
This international standard specifies the implementation rules for depth profiling in auger electron spectroscopy. 1.2 Scope of application
SI/T 1C657--93
This standard guideline is for the use of the intermittent electron spectroscopy deep attenuation analysis method using the cross-sectional method, the ball precipitation method, the ion beam method, and the non-destructive depth analysis method.
This standard guideline may involve hazardous items, operations and equipment. However, it does not describe all related safety issues. Users should establish appropriate safety and health measures and determine the scope of application of this guideline before using this guideline. 2 Summary of methods
2.1 Ionization and cross-sectional method: The sample surface is ground or irradiated at a certain degree to improve the depth analysis ability compared with the cross-sectional method.
2.2 The ball pit method uses a rotating ball to form a spherical pit on the sample surface, and the ball pit is inclined to improve the depth analysis ability. 2.3 Ion sputtering method: combined with Auger separation, it uses ion bombardment to peel off the surface of the product. 2.4 Non-destructive depth analysis method refers to a non-destructive method to obtain information at different depths of various product surfaces. 3 Significance and application
3.1 Electron spectroscopy provides information on the chemical and physical state of the near-surface area of ​​the solid, so non-destructive depth analysis is limited to this near-surface area.
3.2 Ion emission method is mainly used for a depth of 2um. 3.3 Angle grinding method or ball pit method is mainly used for a depth greater than 1μm. 3.4 When using the depth analysis method to study the interface, the depth analysis method should be selected according to the surface roughness, interface roughness and film thickness. 4 Angle grinding and surface grinding method
4.1 The grinding method is a method of polishing a sample at an angle to improve the depth resolution, as shown in Figure 1; while in the cross-section method, the sample is polished and polished. Diamond paper, diamond paste and white steel are often used as polishing materials. The particle size of the polishing material is gradually refined to obtain the desired surface smoothness. However, these two methods have certain advantages in obtaining a clear interface and a smooth surface.
Approved by the Ministry of Electronics Industry of the People's Republic of China on December 17, 1993 and implemented on June 1, 1994
SI/T 1C457-93
Multiple angle grinding sample cross-section diagram
Note: In fact, the angle is much smaller than the previous angle, which is an order of magnitude. 4.2 In the angle operation, the sample is fixed on a flat plate and the angle is measured with a straightener. The accuracy depends on the flatness of the sample. In practical applications, the measurement accuracy can reach 0.14.3 Depth (as shown in Figure 1), given by formula (1): d = Y.tar
In the formula, 9 is the angle of induction;
Y is the horizontal distance from the analysis point to the upper edge of the grinding surface. nm. 4.4 Depth analysis capability 4d, given by formula (2): Ad - AY.tano
In the formula: AY.... is the position error between the electron beam and the sample and the ground beam am (1)
4.5 The analysis includes line scanning analysis and point analysis along the grinding surface. These analyses can be performed by adjusting the moving sample with a micrometer or by moving the electrons with electrons.
4.6 The centrifugal-sputtering method is often combined with the grinding method to remove contamination and study the interface under the grinding surface. 5 Ball pit method
51 First, the sample is fixed on a device that can touch the surface of the rotating steel ball, and then ground. The rotation speed of the steel ball and the force exerted on the sample can be controlled. 5.2 Coating the ball with abrasive can increase the grinding rate. Abrasive paste with a particle size of 0.1 μm to 1 μm is used. Using a relatively large particle size can achieve a very high grinding rate, and using a relatively fine particle size can obtain a very smooth pit. First, a coarse abrasive paste is used to form the pit, and then a fine abrasive paste is used to form the pit. 5.3 The geometric shape of the pit is shown in Figure 2. The depth of the pit d is given by (3): D—diameter of the pit, nm:
R—radius, nm: R>t.
t - 1*/8R
SJ/T 10457—93
Figure 2 A cross-sectional view of a pit with a depth of R obtained on a sample using a ball with a radius of R 5.4 Intermittent analysis is the same as described in 4.5 and 4.6. 5.5 The depth of any point in the analysis is given by (4): Z - (R-X3 + D.X - D/4)12- (R-D\/4):/2 where X is the horizontal distance from the analysis point to the edge of the crater, nm. The depth can also be approximated by (5):
Z = X.(D-X)/2RwwW.bzxz.Net
5.6 The depth resolution A is given by (6): AZ-AX.tang
where AX is the sum of the electron beam diameter and other position errors in the horizontal direction, nm6 is the wrinkle angle.
Different from the angle grinding method, the slope angle is defined as the angle between the sample surface and the tangent line of the crater wall. The slope angle changes along the pit wall, and its value can be given by equation (7):
Sine = 2(0. SD - X)/R
is the smallest at the bottom of the sphere, where the best resolution is achieved. 6 Ion sputtering method
6.1 First, place the sample in a vacuum chamber equipped with an Auger analyzer and an ion sputtering gun, and shoot the ion beam at the target or Faraday cup. Place the sample in front of the Auger analyzer and make the ion gun face the analysis area so that the analysis area is within the ion sputtering area. If the ion beam and the sample are not aligned, the shadow effect of the ion beam on the analysis area must be considered. During the sputtering process, rotating the sample stage can improve the uniformity of the ion sputtering and improve the depth resolution during depth to depth analysis. 5.2 Select the elements to be tested based on experience or from the initial full spectrum scan. Select the energy window of the transition peak for each element and record the peak-to-peak height of the intermittent differential spectrum or the peak height of the N(E) spectrum during the depth analysis. The above data collection can be performed during the continuous sputtering process or in the interval between sputtering. The results of these two data collection methods may be different. During the depth analysis of the unloaded sample, full-scale scanning should be performed regularly to check whether new elements appear and to determine whether there are enough energy peaks to move out of the specified window. 6.3 For the edges of the arc craters generated by sputtering, line scanning can be used for analysis. This method is similar to the ball crater analysis. For arc craters with different shapes, the presence of ion damage and arc asymmetry increase the complexity of analysis. 6.4 For each sample, it should be determined whether the ionization will cause composition changes or other sputtering effects. In some cases, these effects can be minimized by adjusting the condensation time. SI/T 10457 93
6.5 Ions used for Auger analysis are usually complete devices that produce a focused ion beam without using the sample as the anode of the gun. Many ion guns can scan the ion beam, and the ion beam can produce a relatively uniform ion flow rate in the analysis area close to the sample surface.
F.6 If an ion gun is equipped with a flow restriction hole for the sputtering gas flow, most of the sputtering gas can be removed by vacuum during sputtering. Otherwise, the high vacuum chamber will inevitably be backfilled with sputtering gas, so measures must be considered to remove these sputtering active gases. Turbomolecular pumps, or ion recorders, etc. can effectively remove these gases. 6.7 Radiation shielding usually uses inert gases, the most commonly used is argon. If high-energy radiation is required to accelerate the radiation, fluorine gas can be used. In special cases, inert gases such as oxygen and metal ions can be used. 6.7.1 The ion energy of the inert gas used for deep analysis is usually in the range of 500eV to 5keV. 6.7.2 Measure the ion beam density using a Faraday cup. 5.7.3 When using ion sputtering for depth analysis, the depth scale is calibrated using the sputtering rate. Standard samples such as tantalum pentoxide films with thicknesses of 30 nm and 130 nm or nickel-chromium films with thicknesses of 6 nm and 53 nm can be used to determine the sputtering rate. 7 Nondestructive depth profiling methods
7.1 Nondestructive Auger electron spectroscopy depth profiling can be performed by changing the effective escape depth of the excited electrons. This method is limited to characterizing the outermost range of 2 nm to 5 nm of the sample. 7.2 For some elements.The energy-depth relationship can be obtained by detecting the energy-independent transitions. The Auger electrons with lower energy have a smaller exit depth than the Auger electrons with higher energy. Therefore, different transitions of the same element should have different sampling depths.
7.3 The change in the energy of the emitted electrons can cause a slight change in the sample analysis signal source depth. Therefore, by changing the energy of the emitted electrons, the sampling depth can be changed to some extent. 7.1 By changing the concentration of the emitted electrons, angle-resolved Auger electron spectroscopy depth analysis can be performed. However, this method is limited by the roughness of the surface and the angular anisotropy of the signal intensity of the whole band.
The standard was drafted by the Standardization Institute of the Ministry of Electronics Industry. The main drafters of the standard are: Li Yansong, Liu Yongmei, Luo Xinghua, Yan Rupin, and Hua Qingheng. This standard is equivalent to the American Society for Testing and Materials standard ASTME1127-86 "Standard Guide for Depth Analysis of Auger Electron Spectroscopy".
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