CN113865915A - Detection method of sliced sample - Google Patents
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- CN113865915A CN113865915A CN202111098258.6A CN202111098258A CN113865915A CN 113865915 A CN113865915 A CN 113865915A CN 202111098258 A CN202111098258 A CN 202111098258A CN 113865915 A CN113865915 A CN 113865915A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
- G01N1/06—Devices for withdrawing samples in the solid state, e.g. by cutting providing a thin slice, e.g. microtome
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
- G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
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Abstract
Disclosed is a method of testing a sliced sample, the sliced sample including a cut surface, the method comprising: measuring an energy loss spectrum of a target region of the cutting surface; obtaining an element type or an element signal of the target region from the energy loss spectrum; and estimating the deviation degree of the sliced sample according to the deviation of the element type or element signal obtained by the target area and the expected element type or element signal. The method and the device judge the deviation degree of the sliced sample by analyzing the element types or element signals in the target area of the sliced sample.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a detection method of a slice sample.
Background
Metal interconnect lines in semiconductor devices are very important conductive paths. The growth quality of the crystal directly influences the stability of the device operation. Therefore, the growth monitoring of the metal connecting line is crucial.
The monitoring of the metal connecting wire of the semiconductor device mainly comprises the growth profile of the metal connecting wire, the oxidation degree of the bottom interface of the metal connecting wire and the like. Cross-sectional slices of the metal connecting wires are generally prepared and then the growth quality thereof is confirmed with a Transmission Electron Microscope (TEM).
However, since the metal connection line is cylindrical, especially the diameter is nanometer, the sample preparation is very easy to shift, and the subsequent monitoring of the metal connection line of the sample is affected.
Disclosure of Invention
In view of the above-described problems, an object of the present invention is to provide a method for detecting a sliced sample, which analyzes the type of an element or an element signal in a target region of the sliced sample to determine the degree of displacement of the sliced sample.
The invention provides a method for detecting a section sample, wherein the section sample comprises a cutting surface, and the method comprises the following steps:
measuring an energy loss spectrum of a target region of the cutting surface;
obtaining an element type or an element signal of the target region from the energy loss spectrum; and
and estimating the deviation degree of the sliced sample according to the deviation of the element type or element signal obtained by the target area and the expected element type or element signal.
Preferably, the sliced sample is a metal connecting wire, the metal connecting wire comprises a core part and an insulating layer surrounding the core part, and the cutting surface is a longitudinal section of the metal connecting wire.
Preferably, the element type or element signal corresponding to the core is a desired element type or element signal.
Preferably, the dielectric layer surrounds the insulating layer of the core.
Preferably, when there is no deviation between the element type or element signal obtained from the target region of the sliced sample and the expected element type or element signal, the sliced sample is not shifted.
Preferably, if there is a deviation between the element type or element signal obtained from the target region and the expected element type or element signal, the sliced sample is shifted.
Preferably, when the element type or element signal obtained by the target area and the expected element type or element signal are deviated from one element type or element signal, the slice sample is slightly deviated.
Preferably, the sliced sample is heavily biased when the acquired elemental species or elemental signals of the target region deviate from expected elemental species or elemental signals by more than one elemental species or elemental signals.
Preferably, the sliced sample is in the form of a sheet.
Preferably, the sliced sample is prepared by a focused ion beam method.
According to the detection method of the sliced sample, the element type or the element signal of the target area is analyzed by acquiring the energy loss spectrum of the sliced sample, and the deviation degree of the sliced sample is judged according to the element type or the element signal in the target area so as to screen the sliced sample meeting the requirement.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent from the following description of the embodiments of the present invention with reference to the accompanying drawings, in which:
fig. 1 shows transmission electron micrographs of a semiconductor device on different scales;
FIG. 2 shows a schematic view of a cut sample of metal connecting wires cut;
FIG. 3 is a schematic structural diagram showing a treading spectrum of a cut surface of a cut piece sample;
FIG. 4 shows a schematic diagram of an EELS;
FIG. 5 shows a schematic top view of a sliced sample without bias cut;
FIG. 6 shows a schematic top view of a slightly off-cut sliced sample;
FIG. 7 shows a schematic top view of a severely miscut sliced sample;
FIG. 8 shows an electron energy loss spectrum resulting from performing a tap spectrum on a first sliced sample;
FIG. 9 shows an electron energy loss spectrum resulting from performing a tap spectrum on a second sliced sample;
fig. 10 shows an electron energy loss spectrum obtained by performing a treading spectrum on a third sliced sample.
Detailed Description
The invention will be described in more detail below with reference to the accompanying drawings. Like elements in the various figures are denoted by like reference numerals. For purposes of clarity, the various features in the drawings are not necessarily drawn to scale.
It will be understood that when a layer or region is referred to as being "on" or "over" another layer or region in describing the structure of the device, it can be directly on the other layer or region or intervening layers or regions may also be present. And, if the device is turned over, that layer, region, or regions would be "under" or "beneath" another layer, region, or regions.
If for the purpose of describing the situation directly above another layer, another area, the expression "directly above … …" or "above and adjacent to … …" will be used herein.
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples.
Metal interconnect lines are important conductive paths of semiconductor devices, which are typically formed in dielectric layers of semiconductor devices. FIG. 1 shows TEM images of a semiconductor device on different scales, where FIG. 1(a) is a TEM image with a scale of 1000nm, FIG. 1(b) is a TEM image with a scale of 100nm, and FIG. 1(c) is a TEM image with a scale of 20 nm; as shown in fig. 1, the metal connection line 100 includes a core 110 and an insulating layer 120 surrounding the core 110, and a dielectric layer 200 is surrounded outside the insulating layer 120. The metal connection line 100 has a cylindrical shape, and the diameter of the core 110 is generally on the nanometer scale, as shown in fig. 3, the diameter of the core 110 of the metal connection line 100 is 40 nm.
Monitoring the growth of the metal connection line 100, mainly the growth profile of the core 110, requires preparing a sliced sample 300 representing the cross-sectional structure of the core 110 and the insulating layer 120.
The sliced sample 300 is prepared by a Focused Ion Beam (FIB) method. Fig. 2 shows a schematic cut of a sliced sample 300 of metal connecting wires. As shown in fig. 2, the metal connecting wire 100 is cut from its end surface toward its cylindrical direction to form a cut sample 300. The sliced sample 300 is a sheet and includes a transverse section 310 and a longitudinal section 320 perpendicular to the transverse section 310, wherein the longitudinal section 320 is a cut surface, which represents a cross-sectional structure of the metal connection line 100.
In the preparation process of the sliced sample 300, since the metal connection line 100 is cylindrical and the diameter thereof is generally nano-scale, the metal connection line 100 can be easily cut off in the cutting process. The embodiment of the invention provides a detection method of a sliced sample, which is used for judging the deviation degree of the sliced sample. The detection method comprises the following steps.
S10: measuring an energy loss spectrum of a target region of the cutting face.
In this embodiment, the target area is a central area of the cutting surface. Specifically, fig. 3 shows a structural diagram of a stepping spectrum performed on a cutting surface of a slice sample, and as shown in fig. 3, an energy loss spectrum of a target region is obtained by stepping a spectrum on a central region of the cutting surface.
This example uses Electron Energy Loss Spectroscopy (EELS) to obtain Electron Energy Loss spectra in the target region of the sliced sample. EELS is an important element analysis means of a Transmission Electron Microscope (TEM), and has the characteristics of high spatial resolution, strong signal and the like.
Fig. 4 shows a schematic diagram of an EELS, and as shown in fig. 4, the EELS projects an accelerated and focused electron beam onto a sample, the incident electron beam generates inelastic scattering in the sample, and the energy lost by the electron directly reflects information such as a scattering mechanism, a chemical composition and a thickness of the sample, so that the elemental composition, the chemical bond, the electronic structure, and the like of a thin sample micro-region can be analyzed. Compared with Energy Dispersive X-Ray Spectroscopy (EDX) and the like, EELS is more suitable for analysis of thin samples, such as metal link sliced samples.
S20: obtaining an elemental species or elemental signal of the target region from the energy loss spectrum.
The energy loss spectrum can directly reflect the element types or element signals in the target area of the slice sample 300 in the direction vertical to the cutting surface. Under different offset states, the energy loss spectra of the target region of the sliced sample 300 obtain different elemental species or elemental signals.
Specifically, fig. 5-7 respectively show schematic top-view structural diagrams of different degrees of deflection of sliced samples; fig. 5 is a schematic top view of a sliced sample without deviation, fig. 6 is a schematic top view of a sliced sample with slight deviation, and fig. 5 is a schematic top view of a sliced sample with severe deviation.
As shown in fig. 5, in the section sample without the shift, only the core portion 110 is distributed in the target region (shown in the frame in the figure) in the direction perpendicular to the cutting plane; the energy loss spectrum in the target region of the sliced sample can only obtain the element type or element signal corresponding to the core 110.
As shown in fig. 6, in the slightly deviated sliced sample, a core portion 110 and an insulating layer 120 are distributed in a target area (shown at a block in the figure) in a direction perpendicular to the cutting plane; the energy loss spectrum of the target region of the sliced sample is used to obtain the elemental species or elemental signals corresponding to the core 110 and the insulating layer 120.
As shown in fig. 7, in the heavily-deviated sliced sample, a core portion 110, an insulating layer 120 and a dielectric layer 200 are distributed in a target region (shown at a block in the figure) in a direction perpendicular to the cutting plane; the energy loss spectra in the target region of the sliced sample are used to obtain the elemental species or elemental signals corresponding to the core 110, the insulating layer 120, and the dielectric layer 200.
In this embodiment, the element type or element signal corresponding to the core portion 110 is W, the element type or element signal corresponding to the insulating layer 120 is Ti, and the element type or element signal corresponding to the dielectric layer 200 is O.
Specifically, the core 110 is made of tungsten (W), and the corresponding element type or element signal is W; the insulating layer 120 is made of TiN, and the corresponding element type or element signal is Ti or N, in this embodiment, one of the element type or element signal Ti is selected as the element type or element signal corresponding to the insulating layer 120, and in other embodiments, the element type or element signal N may also be selected; the material of the dielectric layer 200 is SiO2The element type or the element signal is Si or O, and one of the element type or the element signal O is selected as the element type or the element signal corresponding to the dielectric layer 200 in this embodiment.
It is understood that the present invention is not limited thereto, the core 110 may be made of copper, the insulating layer 120 may be made of Ti, Ta, TaN, or the like, and the dielectric layer 200 may be made of silicon nitride, or the like. The element types or element signals corresponding to the structures can be selected according to requirements.
S30: and estimating the deviation degree of the sliced sample according to the expected element type or element signal of the target area and the deviation of the obtained element type or element signal.
In this embodiment, when there is no deviation between the element type or element signal obtained from the target region of the sliced sample and the expected element type or element signal, the sliced sample is not shifted. And if the element type or the element signal obtained by the target area is deviated from the expected element type or the element signal, the slice sample wafer is deviated.
Specifically, when the element type or element signal obtained by the target area and the expected element type or element signal are deviated from one element type or element signal, the slice sample is slightly shifted. When the element type or element signal obtained by the target area is deviated from the expected element type or element signal by more than one element type or element signal, the slice sample is severely deviated.
In a specific embodiment, the first slice sample, the second slice sample and the third slice sample are respectively inspected, and specifically, incident electron beams are respectively projected into target areas of cut surfaces of the first slice sample, the second slice sample and the third slice sample to acquire energy loss spectrums in the target areas of the cut surfaces of the first slice sample, the second slice sample and the third slice sample.
Fig. 8(a) -8 (c) respectively show electron energy loss spectra obtained by performing a treading spectrum on the first slice sample, wherein the treading spectrum parameters are as follows: energy resolution 0.15eV, spot size 4(200PA), scanning step size 1 nm.
Wherein, fig. 8(a) shows the region of the treading spectrum performed on the first sample slice sample, fig. 8(b) shows the high loss energy spectrum in the treading spectrum region in fig. 8(a), and fig. 8(c) shows the energy filtering image of the first slice sample under different electron energies. As shown in fig. 8(a), a step-on spectrum is performed on a target region (shown in a block in the figure) of a first slice sample, so as to obtain a high-loss energy spectrum as shown in fig. 8(b), an element type or an element signal Ti corresponding to the insulating layer 120 and an element type or an element signal O corresponding to the dielectric layer 200 are not found, there is no deviation between the element type or the element signal obtained by the target region of the first slice sample and an expected element type or an element signal, and the first slice sample is not shifted; fig. 8(c) shows the filtered images at O, Ti and W electron energies, respectively, to determine the presence of the core 110, insulating layer 120, and dielectric layer 200 in the first slice sample.
Fig. 9(a) -9 (c) respectively show electron energy loss spectra obtained by performing the stepping spectrum on the second sliced sample, wherein fig. 9(a) shows the region of the stepping spectrum on the second sliced sample, fig. 9(b) shows the high-loss energy spectrum in the stepping spectrum region in fig. 9(a), and fig. 9(c) shows the energy filtered images of the second sliced sample at different electron energies. From fig. 9(a), a tread spectrum is performed on a target region (shown in a block in the figure) of a second sliced sample, so as to obtain a high loss energy spectrum as shown in fig. 9(b), an element species or an element signal Ti corresponding to the insulating layer 120 is found, an element species or an element signal O corresponding to the dielectric layer 200 is not found, the second sliced sample is shifted, and the element species or the element signal obtained from the target region of the second sliced sample and the expected element species or the element signal are deviated by one element species or one element signal, and the second sliced sample is slightly shifted; in this case, the second sliced sample may be thinned to reduce the influence of the offset of the second sliced sample. Fig. 9(c) shows the filtered images at O, Ti electron energies, respectively, to determine the presence of the insulating layer 120 and the dielectric layer 200 in the second sliced sample.
Fig. 10(a) -10 (c) respectively show electron energy loss spectra obtained by performing the stepping spectrum on the third sliced sample, wherein fig. 10(a) shows the region of the stepping spectrum on the third sliced sample, fig. 10(b) shows the high-loss energy spectrum in the stepping spectrum region in fig. 10(a), and fig. 10(c) shows energy filtered images of the third sliced sample at different electron energies. As shown in fig. 10(a), a high loss energy spectrum as shown in fig. 10(b) is obtained by performing a tap spectrum on a target region (shown by a square in the figure) of a third sliced sample, in which an element type or an element signal Ti corresponding to the insulating layer 120 and an element type or an element signal O corresponding to the dielectric layer 200 are found in fig. 10(b), the sliced sample is shifted, and the element type or the element signal obtained from the target region of the third sliced sample is deviated from an expected element type or an expected element signal by more than one element type or one element signal, and the third sliced sample is heavily shifted; in which case re-sampling is required. Fig. 10(c) shows the filtered images at O, Ti electron energies, respectively, to determine the presence of the insulating layer 120 and the dielectric layer 200 in the third sliced sample.
While embodiments in accordance with the invention have been described above, these embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments described. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention and various embodiments with various modifications as are suited to the particular use contemplated. The invention is limited only by the claims and their full scope and equivalents.
Claims (10)
1. A method of testing a sliced sample, wherein the sliced sample comprises cut surfaces, the method comprising:
measuring an energy loss spectrum of a target region of the cutting surface;
obtaining an element type or an element signal of the target region from the energy loss spectrum; and
and estimating the deviation degree of the sliced sample according to the deviation of the element type or element signal obtained by the target area and the expected element type or element signal.
2. The detection method according to claim 1, wherein the sliced sample is a metal connection wire including a core portion and an insulating layer surrounding the core portion, and the cut surface is a longitudinal section of the metal connection wire.
3. The method of claim 2, wherein the core corresponds to an element species or element signal that is an expected element species or element signal.
4. The inspection method of claim 2 or 3, wherein the insulating layer of the core is surrounded by a dielectric layer.
5. The detection method according to claim 1, wherein when there is no deviation between the elemental species or elemental signal obtained from the target region of the sliced sample and the expected elemental species or elemental signal, the sliced sample is not shifted.
6. The method according to claim 1, wherein if there is a deviation between the element type or element signal obtained from the target region and the expected element type or element signal, the sliced sample is shifted.
7. The detection method according to claim 6, wherein when the element type or element signal obtained by the target area and the expected element type or element signal are deviated by one element type or element signal, the sliced sample wafer is slightly shifted.
8. The detection method of claim 6, wherein the sliced sample is heavily biased when the elemental species or elemental signals acquired for the target region deviate from expected elemental species or elemental signals by more than one elemental species or elemental signals.
9. The detection method according to claim 1, wherein the sliced sample is in a sheet form.
10. The detection method according to claim 1, wherein the sliced sample is prepared by a focused ion beam method.
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