CN114965004B - Patterning test method for interface binding force of device-level nano film layer - Google Patents
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Abstract
The invention relates to the technical field of material sample detection, in particular to a patterning test method for interface binding force of a device-level nano film layer, which comprises the following steps: (a) preparing a sample to be tested; (b) Performing nanoscale accurate delamination on the sample to be tested by the FIB to expose an upper film layer for testing the film layer binding force; (c) Pressurizing the upper layer film layer to perform nano film layer interface binding force test; (d) And observing the change of the film to be tested in the test process, and obtaining a binding force test result. The patterned interface stripping test scheme based on the FIB technology provides a solution for testing and analyzing the interface bonding force between process film layers in a nano device.
Description
Technical Field
The invention relates to the technical field of mechanical property detection of material samples, in particular to a patterning test method for interface binding force of a device-level nano film layer.
Background
Testing of micro-domain mechanical properties of nano-or micro-sized thin film materials or other two-dimensional materials (fibers, tubes, etc.) is an important characterization test means in modern manufacturing and scientific research. Over the past 30 years, many corresponding testing techniques and equipment have been commercialized.
The reported testing methods of the mechanical properties of the micro-areas are numerous and can be mainly divided into two major types of mechanical and non-mechanical methods. The former includes a direct peeling method, a laser peeling method, an indentation method, a scoring method, a stretching method, a bending and expanding method, an abrasion method, a tape sticking method, and the like; the latter includes thermal methods, nucleation methods, capacitance methods, X-ray diffraction methods, and the like. Compared with non-mechanical methods, mechanical methods have stronger practicability, and most commonly used mechanical methods include indentation, scoring and stretching methods, and corresponding combinations of theoretical and test methods have been widely used in the industry.
For measurement of interfacial bonding force between thin film materials, methods commonly used include indentation, scoring, stretching, and the like. The commercial test equipment in the market at present, the measurement equipment of interface binding force is mostly a nanometer scratch instrument integrated on a platform of an optical microscope or a scanning probe microscope, and also has a test instrument based on a Scanning Electron Microscope (SEM) platform. In-SEM nanometer manipulator LF-2000 comprehensive In-situ nanometer manipulator, such as Hysicon PI 89SEM PicoIndexter In Bruker In-situ mechanical tester. These SEM-based testers can enable SEM in-situ observation and analysis during mechanical testing.
These commercial test equipment have been widely used for mechanical property testing of single layer films, non-patterned films.
For the measurement of the bonding force between the film layers, the currently adopted technology comprises a three-point bending method, a four-point bending method, an indentation method, a stretching method, a nano scratch method and the like. The indentation method is mainly used for measuring samples with weaker interface binding force. For those samples with high binding forces, the nano-scratch method is generally used.
The nano scratch test is a commercially more mature test method at present. The method is characterized in that a certain normal force is applied to a hard scriber (probe) with small curvature, the scriber (probe) is used for loading scratches along the surface of a film material to be tested, and the interface binding force is tested when the film layer is peeled off by measuring the stress and the curve of scratch displacement during loading. The nano scratch test generally adopts a linear variable load test mode to measure a normal load stress and indentation position change curve or a scratch depth and scratch position change curve. When the scratch load increases to a certain extent, peeling (delamination) starts to occur between the film layer to be tested and the substrate, at this time, the transverse force scratch curve noise becomes large, the corresponding load is defined as critical load at this moment, the corresponding stress is interface binding force, and the value is normal force, as shown in fig. 1. The transverse force is an integrated indicator, representing the integrated load-bearing capacity of the film-based system, which is mainly determined by factors such as the film-based bonding strength, the hardness and modulus of the film and the substrate, the structure and thickness of the film, and the like.
The limitation is that:
(1) The scratch testers in the current market are only suitable for testing the mechanical properties of large-area, non-patterned and surface film layers, and are not suitable for testing and analyzing the interface bonding force between the nano film layers in devices.
(2) The process layers in the device are typically complex in structure and patterned, and are small in size to the nanometer scale. Some assays require testing of specific interlayer interfacial bonding forces for those underlying layers. Such as an analysis of the binding force of M1 and the overlying dielectric layer in a CMOS device. In this case, no corresponding technical solution is currently available on the market.
(3) Scratch distance of scratch tester in the market at present is generally in micron level, namely more than 1 micron. While the process layers in nano-devices are typically nano-sized. Many process layers are not suitable for conventional scratch testing methods.
Disclosure of Invention
In order to solve the stress test of the nano device film, the invention provides a patterned interface stripping test scheme based on the FIB technology, and provides a solution for the test analysis of the interface bonding force between process film layers in the nano device.
The technical solution of the nano-patterned film testing provided by the invention is to utilize Scanning Electron Microscope (SEM) and Focused Ion Beam (FIB) equipment and related technologies to conduct stripping and patterning on the film layer in the device to be tested, and utilize commercial nano scratch instrument and other testing equipment (such as a nano scratch instrument based on an SEM platform) to conduct mechanical testing so as to realize analysis and testing on interface bonding force between various nano film layers in the nano device.
Specifically, the patterning test method for the interface binding force of the device-level nano film layer provided by the invention comprises the following steps:
(a) Preparing a sample to be tested;
(b) Carrying out nanoscale accurate delamination on the sample to be tested to expose an upper layer film of a film interface to be tested;
(c) Patterning the upper film layer to form a test module suitable for interface test binding force;
(d) Pressurizing the test module to perform a binding force test of the film interface to be tested;
(e) And observing the change of the interface of the film layer to be tested in the test process, and obtaining a binding force test result.
In some possible embodiments, in step (a), the sample to be tested is further mechanically polished and/or chemically etched to delaminate to expose the film layer adjacent to the upper film layer at the interface of the film layer to be tested.
In some possible embodiments, in step (b), nanoscale precision delamination is performed on the sample to be tested using SEM-based FIB;
and/or
In step (c), the upper layer film layer is patterned by using an SEM-based FIB.
In some possible embodiments, the upper membrane layer is patterned to define the size and shape of the test module according to the physical characteristics of the upper membrane layer material.
Further, the test modules may be the same or different in shape; and/or
The test modules may be the same or different in size.
In some possible embodiments, the shape of the test module includes any one or more of the following: round cylinder, oval cylinder, square, cuboid.
In some possible embodiments, the film layer to be tested is made of brittle material or easily deformable material, and the test module is a circular cylinder or an elliptical cylinder;
the film layer to be tested belongs to a non-brittle material and a non-deformable material, and the test module is a cuboid or a cube.
In some possible embodiments, between step (c) and step (d) further comprises: and arranging a nano notch at the interface of the film to be tested, and then pressurizing a testing module at the nano notch to test the binding force of the interface of the film to be tested.
In some possible embodiments, steps (b) through (e) are performed in FIB and SEM (scanning electron microscope) based equipment.
In some possible embodiments, in step (d) and step (e), using a tester based on an SEM platform, in-situ observation of dynamic strain and microstructure changes of the film interface material to be tested is achieved during the testing process, while obtaining relevant experimental data.
In some possible embodiments, the sample to be tested is a semiconductor device having multiple patterned film layers.
Compared with the prior art, the invention has the following beneficial effects:
(1) The technical solution of the nano-patterned film testing provided by the invention is to utilize Scanning Electron Microscope (SEM) and Focused Ion Beam (FIB) equipment and related technologies to conduct stripping and patterning on the film layer in the device to be tested, and utilize commercial nano scratch instrument and other testing equipment (such as a nano scratch instrument based on an SEM platform) to conduct mechanical testing so as to realize analysis and testing on interface bonding force between various nano film layers in the nano device.
(2) For the analysis of the film binding force with larger interface binding strength, the invention also provides a nano-notch solution. The FIB technology is utilized to form a nano-sized notch at the interface to be tested, so that the interface stripping of the high-strength interface binding force can be realized, and the purpose of measuring and analyzing the binding force is achieved.
(3) The method for testing the mechanical property of the interlayer interface bonding force of the nano film in the nano device, namely the technology and the method for testing the peeling of the patterned interface, can realize the testing and the analysis of the interlayer bonding force of different process films in various nano devices.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
FIG. 1 shows a graph of normal or lateral force versus scratch position as described in the background of the invention;
FIG. 2 shows the use of mechanical and chemical delamination techniques to delaminate a sample adjacent to a film to be tested, and the use of FIB for nanoscale precision delamination to expose the surface of the film to be tested;
FIG. 3 illustrates patterning of a film to be tested using FIB techniques, resulting in different test modules;
FIG. 4 illustrates an interfacial peel test analysis using a special test probe;
FIG. 5 illustrates a nanopatterned lift-off test procedure;
FIG. 6 shows the formation of nanonotches in the interface to be stripped using the FIB, followed by a trampling interface binding force test;
fig. 7 shows a nano-lift-off test procedure.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will be more clearly understood, a more particular description of the invention will be rendered by reference to the appended drawings and appended detailed description. It should be noted that, in the case of no conflict, the embodiments of the present application and the features in the embodiments may be combined with each other.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced in other ways than those described herein, and the scope of the invention is therefore not limited to the specific embodiments disclosed below.
The patterning test scheme based on the FIB technology provided by the invention realizes the test of the interface bonding force between the device-level process film layers, and provides a new solution for the nano/micron-level mechanical test.
Specifically, the patterning test method for the interface binding force of the device-level nano film layer provided by the embodiment of the invention comprises the following steps:
(a) Preparing a sample to be tested;
(b) Carrying out nanoscale accurate delamination on the sample to be tested to expose an upper layer film of a film interface to be tested;
(c) Patterning the upper film layer to form a test module suitable for interface test binding force;
(d) Pressurizing the test module to perform a binding force test of the film interface to be tested;
(e) And observing the change of the interface of the film layer to be tested in the test process, and obtaining a binding force test result.
In the step (a), the sample to be measured may be a direct sample feeding sample or a sample to be measured subjected to delamination, and the delamination may be performed mechanically and/or chemically. Mechanical delamination such as grinding; chemical stripping such as RIE (reactive ion etch)). The sample to be tested is mechanically and/or chemically peeled to expose the film layer close to the upper film layer at the interface of the film layer to be tested, wherein the approach mainly means that: in the case of the upper layer of the interface of the layers of the sample to be measured, the upper layer of the sample to be measured may have other materials or other layers of the film other than those, and the layers may be one layer, two layers, three layers, and so on.
In some possible embodiments, in step (b), the FIB performs accurate delamination of the sample to be tested, and the FIB is used to perform nanoscale accurate delamination, and the process also relies on the SEM, i.e. a higher accuracy resolution is used to achieve a more accurate delamination result for the FIB.
In the invention, the interface bonding force of the film layers is the bonding force of two adjacent film layers, and the lower film layer relates to various film layers because the film layer structure is complex, so after FIB (fiber-based) accurate stripping, the upper film layer of the interface of the film layer to be tested is exposed, then the upper film layer is subjected to patterning treatment to form a test module suitable for interface test, the obtained test module is positioned in a corresponding measurement area on the lower film layer, and the test module is pressurized to carry out the film layer interface bonding force test.
In the invention, patterning refers to processing a film layer by using a FIB (focused ion beam) technology or other similar technologies to form test modules with different shapes and sizes so as to realize the test of the interface binding force of the film layer.
In some possible embodiments, the upper layer patterning process is performed using SEM-based FIB. The high resolution of SEM allows for accuracy of FIB processing.
In the invention, at least the upper and lower film layers of the interface of the film layer to be detected are nano-scale film layers.
In the invention, the upper layer film is patterned according to the physical characteristics of the upper layer film material to define the size and shape of the test module. Wherein the test modules are identical or different in shape; and/or the test modules may be the same or different in size.
Further, the shape of the test module includes any one or more of the following: round cylinder, oval cylinder, square, cuboid.
The shape of the test modules differs somewhat for different materials.
For example, the film layer on the interface to be tested is made of brittle material or friction material (such as SiNx) with small breaking strength or easily deformable material, and the test module can be defined as a circular cylinder or an elliptical cylinder so as to reduce stress concentration and facilitate subsequent interface stripping mechanical test.
The film layer to be tested belongs to a non-brittle material and a non-deformable material (such as a metal layer), and the test module can be defined as a cuboid or cube or other shaped test module.
In addition, the patterning structure of the device such as the semiconductor of the sample to be tested has a repeated structure, and a plurality to dozens of patterned test module structures with various shapes and/or various sizes can be formed by utilizing the FIB automatic patterning technology.
Further, for film binding force analysis with high interface binding strength, the invention also provides a nano-notch solution. The FIB technology is utilized to form a nano-sized notch at the interface to be tested, so that the interface stripping of the high-strength interface binding force can be realized, and the measurement and analysis of the binding force can be realized.
The detection mechanism utilizes the local stress concentration effect of the nano notch in the stress test process, thereby realizing the definition of a peeling interface and effectively improving the success rate of the film interlayer peeling test.
In addition, the shape and the size of the FIB patterned test module can be consistent in height, so that the nano stripping test provided by the invention can realize the high normalization processing of test data, thereby realizing the purpose of high-precision test.
In different embodiments of the invention, the interface binding force test mode of the nano film layer can be in various forms, such as detection in a nano scratch instrument, and the test purpose can be achieved by applying force to a mechanical arm arranged in a sample stage by using a sample stage of an SEM; etc.
In the present invention, steps (b) to (e) are performed in FIB and SEM (scanning electron microscope) based equipment. The purpose of more precisely realizing each step is achieved by high precision and patterning processing by FIB and high precision resolution of SEM.
And (b) to (e), using a tester based on an SEM platform, and in the testing process, realizing in-situ observation of dynamic strain and microstructure change of the interface material of the film layer to be tested, and simultaneously obtaining relevant experimental data.
For example, an observation probe of the SEM is used for observing the interface of the film layer to be tested, and a change picture in the test process is obtained. The observation of the part is realized based on the strong high-precision resolution of the SEM, and the observation can be continuously performed, and a change picture is reserved, so that good basic data is provided for further analysis.
The sample to be tested involved in the invention is a semiconductor device with multiple patterned film layers.
In summary, the interface bonding force testing technology and method based on the nano film patterning provided by the invention realize the mechanical property testing of bonding forces between different films in the nano device.
The following examples are given by way of illustration.
Example 1
Specifically, as shown in fig. 2, there may be several tens of process layers in a semiconductor or the like, and are patterned, interwoven. If the interface of the film layer to be tested is in the underlying process layer of the device (as indicated by the arrow in fig. 2 (a)), a corresponding technical solution is required.
The invention provides a patterning test method for interface binding force of a device-level nano film layer, which comprises the following specific detection steps:
(1) The specific size and position of the film to be tested in the device structure are known (as shown in fig. 2 (a)).
(2) The sample to be tested is subjected to mechanical and chemical delamination techniques (mechanical delamination: e.g., grinding; chemical delamination: e.g., RIE (reactive ion etch)) to a point close to the membrane layer to be tested.
(3) After mechanical and chemical delamination, the nanoscale precision delamination is performed by Focused Ion Beam (FIB) technology, and the upper process film layer closest to the film layer to be tested is removed to expose the film layer to be tested (dielectric layer, as shown in fig. 2 (b)).
(4) Patterning the film to be tested by using the FIB technology to form test modules with various shapes suitable for interface test. Such as the cylindrical test module in fig. 3 (b) and the rectangular parallelepiped test module in fig. 3 (c).
a. If the film layer on the interface to be tested is a brittle material, the test module can be defined as a cylinder shape so as to facilitate the subsequent interface peeling mechanical test.
b. If the film layer on the interface to be tested is a non-brittle material, the test module may be defined as a cuboid or other test module.
Since the patterning structure of a device such as a semiconductor has a repeating structure in many cases, it is possible to form a plurality of test module structures of various shapes to several tens of patterns using FIB automatic patterning technology, as shown in fig. 3 (b) and (c).
And (5) putting the sample into a matched nano scratch instrument for nano peeling test analysis. And carrying out interface peeling test analysis by using a matched proper test probe such as an arc test probe, a plane test probe and the like. As shown in fig. 4 (a) and 4 (b).
Fig. 5 (a) - (d) are examples of interfacial delamination (easy-to-peel) test-1 after nanopatterning, i.e., a delamination test analysis for Cu/Al interfaces. Fig. 5 (a) to (c): a test process of a peeling experiment; fig. 5 (d) SEM observations of the delamination interface after the delamination test. The surface exfoliation interface is the interface of nano-metal Al and metal Cu and the interfacial separation is along the interface of metal Al/Cu as seen from the results of the exfoliation experiment. For the Al/Cu nano-metal layer, the nano-Al layer of about 60-70 nanometers is successfully stripped, and the stripping interface can be observed in situ under the SEM. Therefore, the stress test result of the related interface bonding force can be verified by SEM analysis.
Example 2
For analysis of the film binding force with larger interface binding strength, based on the content of the embodiment 1, the invention also provides a nano-notch solution. The mechanism is to utilize the local stress concentration effect of the nano notch in the stress test process, thereby realizing the definition of the peeling interface and effectively improving the success rate of the film interlayer peeling test. As shown in FIG. 6, a nano-sized notch is formed at the interface to be tested by using the FIB technology, so that the interface stripping of the high-strength interface binding force can be realized, and the purpose of measuring and analyzing the binding force is achieved.
Fig. 7 (a) - (c) show interfacial delamination experiments under patterning and nanonotch techniques. Wherein, fig. 7 (a) FIB patterned dimensions; FIG. 7 (b) initiation of FIB patterning and lift-off test; results of the peel test of fig. 7 (c): the nano-notch successfully realizes the definition of the peeling direction of the peeling interface. From the results, the peeling interface proceeds along the nano-notch, indicating the feasibility of this technique.
The patterning test method for the interface binding force of the device-level nano film layer of the sample to be tested comprises the following specific steps:
and knowing the specific size and position of the film to be tested in the device structure.
The sample to be tested is subjected to mechanical and chemical delamination techniques (mechanical delamination: e.g., grinding; chemical delamination: e.g., RIE (reactive ion etch)) to a point close to the membrane layer to be tested.
After mechanical and chemical stripping, a Focused Ion Beam (FIB) technology is adopted to carry out nanoscale accurate stripping, and an upper process film layer closest to the film layer to be detected is removed to expose the film layer to be detected.
Patterning the film to be tested by using the FIB technology to form test modules with various shapes suitable for interface test.
Forming a nanometer-sized notch at the interface to be tested by utilizing the FIB technology.
And placing the patterned sample to be tested with the nano notch into corresponding testing equipment (such as a nano scratch meter) for interface stripping and stress measurement.
The nano-peeling test is also a test mode adopting linear loading, and when an interface is peeled, a critical stress appears on a test curve, and the critical stress corresponds to the interface binding force.
The shape and the size of the FIB patterned test module can be highly consistent, so that the nano stripping test provided by the invention can realize the high normalization processing of test data so as to realize the purpose of high-precision test.
If the nano-peeling test is performed in the tester based on the SEM platform, the observation of the fracture interface can be directly performed on the SEM, and whether the interface of the film peeling is between the interfaces to be tested can be accurately judged, so that high-precision test data can be obtained.
In the invention, the steps (a), (b), (c), (d) and (e) are only used for distinguishing different steps, and cannot be understood as indicating or suggesting the sequence of the steps; the term "plurality" means two or more, unless expressly defined otherwise. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the description of this specification, the terms "some embodiments," "some possible implementations," "particular embodiments," and the like, are used to describe particular features, structures, materials, or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The patterning test method of the interface binding force of the device-level nano film layer is characterized by comprising the following steps of:
(a) Preparing a sample to be tested;
(b) Performing nanoscale accurate delamination on the sample to be tested by the FIB based on SEM to expose an upper layer film of the interface of the film to be tested;
(c) Patterning the upper film layer by the SEM-based FIB to form a test module suitable for interface test binding force;
if the film layer on the interface to be tested belongs to a brittle material, the test module is defined as a cylinder shape so as to facilitate the subsequent interface stripping mechanical test;
if the film layer on the interface to be tested belongs to a non-brittle material, the test module is defined as a cuboid-shaped test module;
putting the sample into a matched nano scratch instrument for nano peeling test analysis; performing interface peeling test analysis by using a matched arc test probe or plane test probe;
placing the sample to be tested with the patterning and the nano notch into a corresponding nano scratch instrument for interface stripping and stress measurement;
setting a nano notch at the interface to be tested;
(d) Pressurizing the test module at the nano notch to test the binding force of the interface of the film to be tested;
(e) And observing the change of the interface of the film layer to be tested in the test process, and obtaining a binding force test result.
2. The method according to claim 1, wherein in the step (a), the sample to be tested is further mechanically polished and/or chemically etched to remove the layer of the upper layer of the interface layer of the layer to be tested.
3. The patterning test method of device-scale nanomembrane layer interface bonding force of claim 1, wherein the upper layer film is patterned according to physical characteristics of the upper layer film material to define a size and shape of the test module.
4. The patterning test method of device-level nanomembrane layer interface bonding force according to claim 3, wherein the test modules have the same or different shapes; and/or
The test modules may be the same or different in size.
5. The patterning test method of device-scale nanomembrane layer interface bonding force of claim 1, wherein the shape of the test module includes any one or more of: round cylinder, oval cylinder, square, cuboid.
6. The patterning test method for the interface bonding force of the device-level nano film layer according to claim 5, wherein the film layer to be tested belongs to brittle materials or easily deformable materials, and the test module is a circular cylinder or an elliptic cylinder;
the film layer to be tested belongs to a non-brittle material and a non-deformable material, and the test module is a cuboid or a cube.
7. The method of claim 1, wherein steps (b) through (e) are performed in a FIB and SEM based device.
8. The patterning test method of device-level nanomembrane layer interface bonding force according to claim 7, wherein in step (d) and step (e), an SEM platform-based tester is used to realize in-situ observation of dynamic strain and microstructure variation of the film layer interface material to be tested in the test process, and obtain related experimental data.
9. The method for patterning the interfacial bonding force of a device-scale nanomembrane layer according to any one of claims 1-8, wherein the sample to be tested is a semiconductor device having multiple patterned layers.
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