CN113865915B - Slice sample detection method - Google Patents
Slice sample detection method Download PDFInfo
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- CN113865915B CN113865915B CN202111098258.6A CN202111098258A CN113865915B CN 113865915 B CN113865915 B CN 113865915B CN 202111098258 A CN202111098258 A CN 202111098258A CN 113865915 B CN113865915 B CN 113865915B
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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
Abstract
Disclosed is a method of detecting 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 face; obtaining an elemental species or elemental signal of the target region from the energy loss spectrum; and estimating the degree of offset of the slice sample according to the deviation of the element type or element signal obtained from the target region and the expected element type or element signal. According to the invention, the deviation degree of the slice sample is judged by analyzing the element type or element signal in the slice sample target area.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a slice sample detection method.
Background
Metal interconnect lines in semiconductor devices are very important conductive paths. The growth quality directly affects the stability of the device operation. And therefore is critical for the growth monitoring of metal bond wires.
The monitoring of the metal connecting wire of the semiconductor device mainly comprises the growth outline of the metal connecting wire, the oxidation degree of the bottom interface of the metal connecting wire and the like. Cross-sectional sections of the metal bond wires are typically prepared and then their quality of growth is confirmed with a transmission electron microscope (Transmission electron microscope, TEM).
However, since the metal connecting wire is columnar, particularly has a diameter of nanometer scale, the sample preparation is very easy to deviate, and the monitoring of the subsequent metal connecting wire of the sample can be influenced.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a method for detecting a sliced sample, which analyzes an element type or an element signal in a target region of the sliced sample to determine a degree of displacement of the sliced sample.
The invention provides a method for detecting a slice sample, wherein the slice sample comprises a cutting surface, and the method comprises the following steps:
measuring an energy loss spectrum of a target region of the cutting face;
obtaining an elemental species or elemental signal of the target region from the energy loss spectrum; and
and estimating the deviation degree of the slice 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 wire comprising a core and an insulating layer surrounding the core, the cut surface being a longitudinal section of the metal wire.
Preferably, the element type or element signal corresponding to the core is an expected element type or element signal.
Preferably, the insulating layer of the core is surrounded by a dielectric layer.
Preferably, the slice sample is not shifted when there is no deviation between the elemental species or elemental signal obtained from the slice sample target region and the expected elemental species or elemental signal.
Preferably, if the element type or element signal obtained from the target region deviates from the expected element type or element signal, the slice sample is shifted.
Preferably, the slice is slightly shifted when the element type or element signal obtained from the target region deviates from the expected element type or element signal by one element type or element signal.
Preferably, the slice sample is severely shifted when the elemental species or elemental signal obtained by the target region deviates from the expected elemental species or elemental signal by more than one elemental species or elemental signal.
Preferably, the sliced sample is in the form of a sheet.
Preferably, the slice sample is prepared by a focused ion beam method.
According to the method for detecting the slice sample, the energy loss spectrum of the slice sample is obtained to analyze the element type or element signal of the target area, and the deviation degree of the slice sample is judged according to the element type or element signal in the target area, so that the slice sample meeting the requirements is screened.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent from the following description of embodiments of the present invention with reference to the accompanying drawings, in which:
fig. 1 shows a transmission electron microscope image of a semiconductor device under different scales;
FIG. 2 shows a cut sample cut schematic of a metal bond wire;
FIG. 3 shows a schematic structural diagram of a pedal spectrum of a cut surface of a slice sample;
FIG. 4 shows a schematic diagram of EELS;
FIG. 5 shows a schematic top view of a sliced sample without a cut-off;
FIG. 6 shows a schematic top view of a slightly off-cut slice sample;
FIG. 7 shows a schematic top view of a severely cut slice sample;
FIG. 8 shows electron energy loss spectra obtained by performing a step-on spectrum on a first slice sample;
FIG. 9 shows electron energy loss spectra obtained from a step on a second slice sample;
fig. 10 shows electron energy loss spectra obtained by stepping on the third slice sample.
Detailed Description
The invention will be described in more detail below with reference to the accompanying drawings. Like elements are denoted by like reference numerals throughout the various figures. For clarity, the various features of the drawings are not drawn to scale.
It will be understood that when a layer, an area, or a structure of a device is described as being "on" or "over" another layer, another area, it can be referred to as being directly on the other layer, another area, or further layers or areas can be included between the other layer, another area, etc. And if the device is flipped, the one layer, one region, will be "under" or "under" the other layer, another region.
If, for the purposes of describing a situation directly overlying another layer, another region, the expression "directly overlying … …" or "overlying … … and adjoining" will be used herein.
The following describes in further detail the embodiments of the present invention with reference to the drawings and examples.
Metal interconnect lines are important conductive channels of semiconductor devices that are typically formed in dielectric layers of semiconductor devices. Fig. 1 shows a transmission electron microscope image of a semiconductor device under different scales, wherein fig. 1 (a) is a transmission electron microscope image with a scale of 1000nm, fig. 1 (b) is a transmission electron microscope image with a scale of 100nm in length, and fig. 1 (c) is a transmission electron microscope image with a scale of 20 nm; as shown in fig. 1, the metal connection wire 100 includes a core 110, and an insulating layer 120 surrounding the core 110, the insulating layer 120 being externally surrounded by a dielectric layer 200. The metal connecting wire 100 has a columnar shape, the diameter of the core 110 of which is generally in the order of nanometers, and the diameter of the core 110 of the metal connecting wire 100 is 40nm as shown in fig. 3.
Monitoring the growth of the metal bond wires 100, and 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 slice sample 300 is prepared by a Focused Ion Beam (FIB) method. Fig. 2 shows a cut schematic of a sliced sample 300 of metal bond wires. As shown in fig. 2, the metal wire 100 is cut from the end face thereof in the column direction, thereby forming a sliced sample 300. The sliced sample 300 is sheet-shaped and comprises a transverse section 310 and a longitudinal section 320 perpendicular to the transverse section 310, wherein the longitudinal section 320 is a cutting surface, and represents the cross-sectional structure of the metal connecting wire 100.
In the process of preparing the sliced sample 300, since the metal connection wire 100 is columnar and has a diameter of typically nano-scale, it is easy to cut off during the process of cutting the nano-scale metal connection wire 100. The embodiment of the invention provides a method for detecting a slice sample, which is used for judging the offset degree of the slice sample. The detection method comprises the following steps.
S10: an energy loss spectrum of a target region of the cutting face is measured.
In this embodiment, the target area is a central area of the cutting surface. Specifically, fig. 3 shows a schematic structural diagram of a stepping spectrum of a cutting surface of a slice sample, and as shown in fig. 3, an energy loss spectrum of a target area is obtained by stepping spectrum of a central area of the cutting surface.
This example employs electron energy loss spectroscopy (Electron Energy Loss Spectroscopy, EELS) to obtain electron energy loss spectra in a target region of a sliced sample. EELS is used as an important element analysis means of a transmission electron microscope (Transmission electron microscope, TEM) and has the characteristics of high spatial resolution, strong signal and the like.
Fig. 4 shows a schematic diagram of EELS, in which an accelerated and concentrated electron beam is projected onto a sample, the incident electron beam is inelastically scattered in the sample, and the energy lost by the electrons directly reflects information such as a mechanism of scattering, chemical composition and thickness of the sample, so that analysis of elemental composition, chemical bonds, electronic structures and the like of a thin sample micro-area can be performed. EELS is more suitable for thin sample analysis such as metal wire slicing samples than energy dispersive X-Ray Spectroscopy (Energy Dispersive X-Ray Spectroscopy, EDX) and the like.
S20: an elemental species or elemental signal of the target region is obtained from the energy loss spectrum.
The energy loss spectrum can directly reflect the elemental species or elemental signals in the direction perpendicular to the cutting plane in the target area of the sliced sample 300. Under different offset conditions, the energy loss spectrum of the target region of the slice sample 300 yields different elemental species or elemental signals.
In particular, fig. 5-7 respectively show schematic top view structures of sliced samples with different degrees of offset; fig. 5 is a schematic top view of a sliced sample without offset, fig. 6 is a schematic top view of a sliced sample with slight offset, and fig. 5 is a schematic top view of a sliced sample with severe offset.
As shown in fig. 5, in the sliced sample in which no offset occurs, only the core 110 is distributed in the target area (shown at the square frame in the figure) in the direction perpendicular to the cutting plane; the energy loss spectrum at the target region of the sliced sample can only obtain the corresponding elemental species or elemental signature for the core 110.
As shown in fig. 6, in the slightly offset sliced sample, a core 110 and an insulating layer 120 are distributed in a target area (shown at a square frame 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 element type or element signal corresponding to the core 110 and the insulating layer 120.
As shown in fig. 7, in the severely-offset sliced sample, a core 110, an insulating layer 120 and a dielectric layer 200 are distributed in a direction perpendicular to the cutting plane in a target area (shown at a square frame in the figure); the energy loss spectrum of the target region of the sliced sample is used to obtain the element types or element 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 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 material is tungsten (W), and the corresponding element species or element signal is W; the insulating layer 120 is made ofTiN, the corresponding element type or element signal is Ti or N, and in this embodiment, one 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 be selected; the material of the dielectric layer 200 is SiO 2 The element type or element signal is Si or O, and one element type or element signal O is selected as the element type or element signal corresponding to the dielectric layer 200 in this embodiment, and in other embodiments, the element type or element signal Si may be selected.
It is to be understood that the present invention is not limited thereto, and the material of the core 110 may be copper, the material of the insulating layer 120 may be Ti, ta, taN, and the material of the dielectric layer 200 may be silicon nitride. The kind of element or the signal of element corresponding to each structure can be selected according to the requirement.
S30: estimating the degree of offset of the slice sample based on the expected elemental species or elemental signal of the target region and the deviation of the obtained elemental species or elemental signal.
In this embodiment, when the element type or element signal obtained from the target area of the slice sample is not deviated from the expected element type or element signal, the slice sample is not shifted. And if the element type or element signal obtained by the target area deviates from the expected element type or element signal, the slice sample is shifted.
Specifically, when the element type or element signal obtained from the target region deviates from the expected element type or element signal by one element type or element signal, the slice is slightly shifted. When the element type or element signal obtained by the target area deviates 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 detected respectively, specifically, the incident electron beam is projected into the target areas of the cut surfaces of the first slice sample, the second slice sample and the third slice sample respectively, so as to obtain energy loss spectra 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 stepping on the first slice sample, the stepping parameters being: the energy resolution is 0.15eV, the light spot size is 4 (200 PA), and the scanning step length is 1nm.
Wherein fig. 8 (a) shows the region of the pedal spectrum performed on the first specimen slice sample, fig. 8 (b) shows the high-loss energy spectrum in the pedal spectrum region in fig. 8 (a), and fig. 8 (c) shows the energy filtered image of the first specimen slice sample at different electron energies. As shown in fig. 8 (a), a high-loss energy spectrum as shown in fig. 8 (b) is obtained by performing stepping on a target area (shown in a square frame in the figure) of a first slice sample, in fig. 8 (b), no deviation is found between an element type or element signal Ti corresponding to the insulating layer 120 and an element type or element signal O corresponding to the dielectric layer 200, and the first slice sample has no deviation between the element type or element signal obtained in the target area of the first slice sample and an expected element type or element signal; fig. 8 (c) shows the filtered image at O, ti and W electron energies, respectively, to determine the presence of core 110, insulating layer 120, and dielectric layer 200 in the first slice sample.
Fig. 9 (a) -9 (c) show electron energy loss spectra obtained by stepping on the second slice sample, respectively, wherein fig. 9 (a) shows a region of stepping on the second slice sample, fig. 9 (b) shows a high loss energy spectrum in the region of stepping on the spectrum in fig. 9 (a), and fig. 9 (c) shows an energy filtered image of the second slice sample at different electron energies. As shown in fig. 9 (a), a high-loss energy spectrum as shown in fig. 9 (b) is obtained by stepping on a target area (shown in a square frame in the figure) of a second slice sample, in which the element type or element signal Ti corresponding to the insulating layer 120 is found in fig. 9 (b), the element type or element signal O corresponding to the dielectric layer 200 is not found, the second slice sample is shifted, and only the element type or element signal obtained in the target area of the second slice sample deviates from the expected element type or element signal by one element type or element signal, and the second slice sample is slightly shifted; in this case, the second slice sample may be thinned to reduce the influence of the second slice sample offset. Fig. 9 (c) shows the filtered image at the electron energy of O, ti, 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) show electron energy loss spectra obtained by stepping on the third slice sample, respectively, wherein fig. 10 (a) shows a region of stepping on the third slice sample, fig. 10 (b) shows a high loss energy spectrum in the region of stepping on the spectrum in fig. 10 (a), and fig. 10 (c) shows an energy filtered image of the third slice 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 stepping on a target area (shown in a square frame in the figure) of a third slice sample, an element type or element signal Ti corresponding to the insulating layer 120 and an element type or element signal O corresponding to the dielectric layer 200 are found in fig. 10 (b), the slice sample is shifted, the element type or element signal obtained in the target area of the third slice sample deviates from an expected element type or element signal by more than one element type or element signal, and the third slice sample is severely shifted; in this case, the sample preparation needs to be performed again. Fig. 10 (c) shows the filtered image at the electron energy of O, ti, respectively, to determine the presence of the insulating layer 120 and the dielectric layer 200 in the third sliced sample.
Embodiments in accordance with the present invention, as described above, are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. 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 modifications as are suited to the particular use contemplated. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (10)
1. The method for detecting the sliced sample is characterized in that 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 end face of the metal connecting wire is cut towards the column direction of the metal connecting wire to form the sliced sample; the slice sample is sheet-shaped and comprises a transverse section and a longitudinal section perpendicular to the transverse section, wherein the longitudinal section is a cutting surface and represents the cross-section structure of the metal connecting wire, and the method comprises the following steps:
measuring an energy loss spectrum of a target area of the cutting surface, wherein the target area is a central area of the cutting surface;
obtaining an elemental species or elemental signal species of the target region from the energy loss spectrum; and
and estimating the offset degree of the slice sample according to the deviation of the element type or element signal type obtained by the target area and the expected element type or element signal type.
2. The method according to claim 1, wherein only core portions are distributed in the target region in a direction perpendicular to the cutting plane in the sliced sample in which no offset occurs.
3. The method according to claim 1, wherein the element type or the element signal type corresponding to the core is an expected element type or an element signal type.
4. A method of testing according to any one of claims 1 to 3, wherein the insulating layer of the core is surrounded by a dielectric layer.
5. The method according to claim 1, wherein the sliced sample is not shifted when there is no deviation between the type of element or the type of element signal obtained from the target area of the sliced sample and the type of expected element or the type of element signal.
6. The method according to claim 1, wherein the slice sample is shifted when the element type or element signal type obtained in the target region deviates from the expected element type or element signal type.
7. The method according to claim 6, wherein the slice is slightly shifted when the type of element or the type of element signal obtained from the target region deviates from the expected type of element or the type of element signal by one type of element or the type of element signal.
8. The method according to claim 6, wherein the slice sample is severely shifted when the element type or element signal type obtained in the target region deviates from the expected element type or element signal type by one or more element types or element signal types.
9. The method of claim 1, wherein the sliced sample is in the form of a sheet.
10. The method of claim 1, wherein the slice sample is prepared by a focused ion beam method.
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