CN114965004A - Patterning test method for interface bonding force of device-level nano film layer - Google Patents
Patterning test method for interface bonding force of device-level nano film layer Download PDFInfo
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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 bonding force of a device-level nano film layer, which comprises the following steps: (a) preparing a sample to be detected; (b) FIB carries out nano-scale accurate stripping on the sample to be tested, and exposes an upper film layer for testing the bonding force of the film layer; (c) carrying out a nano film interface bonding force test on the upper film layer under pressure; (d) and observing the change of the film layer to be tested in the testing process, and obtaining a binding force testing result. The FIB technology-based patterned interface peeling test scheme provided by the invention provides a solution for the test and analysis of the interface bonding force between process film layers in a nanometer 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 bonding force of a device-level nano film layer.
Background
The testing of the mechanical properties of the micro-domains of nano-or micro-sized thin film materials or other two-dimensional materials (fibers, tubes, etc.) is an important characterization test in modern manufacturing and scientific research. Over the past 30 years, a number of corresponding testing techniques and equipment have been commercialized.
At present, many methods for testing the mechanical properties of the micro-area are reported, and the methods can be mainly divided into two types, namely mechanical methods and non-mechanical methods. The former includes a direct peeling method, a laser peeling method, an indentation method, a scratching method, a stretching method, a bending and spreading 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 the non-mechanical method, the mechanical method has stronger practicability, the most common mechanical methods comprise an indentation method, a scratching method and a stretching method, and the combination of the corresponding theory and the testing method is widely applied in the industry.
For measuring the interfacial bonding force between film materials, methods including an indentation method, a scratching method, and a stretching method are generally used. Most of the commercially available test equipment in the market at present is a nano scratch tester integrated on the platform of an optical microscope or a scanning probe microscope, and also a tester based on a Scanning Electron Microscope (SEM) platform. Such as the In-SEM nanomachiner LF-2000 Integrated In-situ nanomachiner, marketed by Shanghai Nateng instruments Inc., the Hysitron PI 89SEM PicoInder In-situ mechanical tester, marketed by Bruker. These SEM-based testers can enable SEM in-situ observation and analysis during mechanical testing.
These commercial testing devices have been widely used for mechanical testing of single layer, non-patterned films.
For the measurement of the interlayer bonding force of the film, the currently adopted technologies comprise a three-point and four-point bending method, an indentation method, a position stretching method, a nano scratching method and the like. The indentation method is mainly used for measuring samples with weak interface bonding force. For those samples with large binding force, the nano scratch method is usually adopted.
Nano scratch testing is currently a relatively mature test method of commercialization. The method is characterized in that a hard scriber (probe) with small curvature is used for applying a certain normal force, the scriber (probe) is used for loading scratches along the surface of a thin film material to be tested, and the interface bonding force test during the peeling of the film layers is realized by measuring the stress and scratch displacement curve during loading. The nano scratch test usually adopts a linear variable load test mode to measure the normal load stress and the variation curve of the indentation position, or the variation curve of the scratch depth and the scratch position. When the scratch load is increased to a certain degree, peeling (delamination) begins to occur between the film layer to be tested and the substrate, the noise of the scratch curve of the transverse force is increased, the corresponding load is defined as a critical load, the corresponding stress is the interface bonding force, and the value is the normal force, as shown in fig. 1. The transverse force is a comprehensive index, and represents that the comprehensive bearing capacity of the film-based system is mainly determined by the film-based bonding strength, the hardness and modulus of the film and the substrate, the structure and thickness of the film and other factors.
The limitations are as follows:
(1) the scratch testers in the market at present 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 and patterned and have dimensions as small as the nanometer scale. Some assays require testing of specific interfacial bonds between the films of those substrates. Such as analysis of the bonding force of M1 and the overlying dielectric layer in CMOS devices. In this case, no corresponding technical solution is available on the market at present.
(3) The scratch distance of the scratch tester on the market at present is generally micron-sized, namely more than 1 micron. While the process layers in nanodevices are typically of nanometer size. Many process layers are not suitable for conventional scratch testing methods.
Disclosure of Invention
In order to solve the stress test of the nanometer device film, the invention provides a patterned interface stripping test scheme based on an FIB technology, and provides a solution for the test and analysis of the interface bonding force between process film layers in the nanometer device.
The technical scheme for testing the nano-patterned film layer provided by the invention is that a Scanning Electron Microscope (SEM), a Focused Ion Beam (FIB) device and related technologies are utilized to strip and pattern the film layer in a device to be tested, and a commercial nano-scratch tester and other testing devices (such as a nano-scratch tester based on an SEM platform) are utilized to perform mechanical testing, so that the analysis and the test of the bonding force of various nano-film layer interfaces in the nano device are realized.
Specifically, the patterned testing method for the interface bonding force of the device-level nano film layer provided by the invention comprises the following steps of:
(a) preparing a sample to be detected;
(b) carrying out nanoscale accurate stripping on the sample to be detected to expose the upper film layer of the interface of the film layer to be detected;
(c) patterning the upper layer film layer to form a test module suitable for testing the bonding force of an interface;
(d) pressurizing the test module to test the bonding force of the interface of the film layer to be tested;
(e) and observing the change of the interface of the film layer to be tested in the testing process, and obtaining a binding force testing result.
In some possible embodiments, in step (a), the sample to be tested is further stripped by mechanical grinding and/or chemical etching to expose the film layer adjacent to the upper film layer of the interface of the film layer to be tested.
In some possible embodiments, in step (b), the sample to be tested is subjected to nanoscale precision stripping using SEM-based FIB;
and/or
In the step (c), the upper layer film layer is patterned by using an SEM-based FIB.
In some possible embodiments, the upper layer of film material is patterned to define the size and shape of the test module based on physical properties of the upper layer of film material.
Further, the test modules are the same or different in shape; and/or
The test modules may be the same size or different sizes.
In some possible embodiments, the shape of the test module comprises any one or more of: circular cylinder, oval cylinder, square, cuboid.
In some possible embodiments, the film to be tested belongs to a brittle material or a 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 testing module is a cuboid or a cube.
In some possible embodiments, between step (c) and step (d), further comprising: and arranging a nano notch at the interface of the film layer to be tested, and then pressurizing the testing module at the nano notch to test the bonding force of the interface of the film layer to be tested.
In some possible embodiments, steps (b) to (e) are performed in a FIB and SEM (scanning electron microscope) based apparatus.
In some possible embodiments, in the step (d) and the step (e), a tester based on an SEM platform is used to realize in-situ observation of the dynamic strain and microstructure change of the interface material of the film layer to be tested during the test, and obtain related experimental data.
In some possible embodiments, the sample to be tested is a semiconductor device having a plurality of patterned film layers.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the technical scheme for testing the nano-patterned film, a Scanning Electron Microscope (SEM), a Focused Ion Beam (FIB) device and related technologies are utilized to strip and pattern the film in the device to be tested, and a commercial nano-scratch tester and other testing devices (such as a nano-scratch tester based on an SEM platform) are utilized to perform mechanical testing, so that the analysis and the test of the bonding force of various nano-film interlayer interfaces in the nano device are realized.
(2) For the analysis of the membrane layer bonding force with larger interface bonding strength, the invention also provides a nano-notch solution. A nanometer-sized notch is formed on the interface to be measured by using the FIB technology, so that the interface peeling of the high-strength interface binding force can be realized, and the purpose of measuring and analyzing the binding force is achieved.
(3) The invention provides a mechanical property testing method of interface bonding force between nanometer film layers in nanometer devices, namely a testing technology and a method of patterned interface stripping.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 shows a graph of normal or lateral force versus scratch position as described in the background of the invention;
FIG. 2 illustrates stripping a sample close to a film layer to be measured using mechanical and chemical stripping techniques, and precise stripping at the nanoscale using FIB to expose the surface of the film layer to be measured;
FIG. 3 illustrates various test modules formed by using FIB techniques to pattern a film layer to be tested;
FIG. 4 illustrates an interface peel test analysis using a special test probe;
FIG. 5 illustrates a nanopatterned lift-off test procedure;
FIG. 6 shows that a nano-gap is formed at the interface to be stripped using FIB, and then an interface bonding force test is practiced;
fig. 7 shows a nano-strip test procedure.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, a more particular description of the invention will be rendered by reference to the appended drawings. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
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 specifically described herein, and therefore the scope of the present invention is not limited to the specific embodiments disclosed below.
The FIB technology-based patterning test scheme 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 nano/micron-level mechanical test.
Specifically, the method for testing the interface bonding 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 detected;
(b) carrying out nanoscale accurate stripping on the sample to be detected to expose the upper film layer of the interface of the film layer to be detected;
(c) patterning the upper layer film layer to form a test module suitable for testing the bonding force of an interface;
(d) pressurizing the test module to test the bonding force of the interface of the film layer to be tested;
(e) and observing the change of the interface of the film layer to be tested in the testing process, and obtaining a binding force testing result.
In the step (a), the sample to be tested is prepared by either directly feeding the sample or stripping the sample, and the stripping can be performed mechanically and/or chemically. Mechanical stripping such as grinding; chemical stripping such as RIE (reactive ion etch) stripping. Exposing a film layer close to an upper film layer of an interface of the film layer to be detected in a sample to be detected after being stripped in a mechanical and/or chemical mode, wherein the close mainly refers to the following steps: in addition to these, the upper layer film of the interface between the film to be measured of the sample to be measured has other film materials or other films, and the film may be one layer, two layers, three layers, and so on.
In some possible embodiments, in step (b), the FIB performs precise stripping on the sample to be tested, and the FIB performs nanoscale precise stripping, and the processing procedure also depends on SEM, that is, a more precise stripping result of the FIB is achieved by high-precision resolution.
According to the invention, the membrane interface binding force is the binding force of two adjacent membranes, and the membrane structure is relatively complex, and the lower membrane relates to multiple membranes, so that after FIB accurate stripping, the upper membrane of the membrane interface to be tested is exposed, and then the upper membrane is subjected to patterning treatment to form a testing module suitable for interface testing, the obtained testing module is positioned in a corresponding measuring area on the lower membrane, and the testing module is pressurized to test the membrane interface binding force.
In the present invention, the patterning process refers to processing the film layer by using FIB (focused ion beam) technology or other similar technologies to form test modules with different shapes and sizes, so as to implement the test of the interface bonding force of the film layer.
In some possible embodiments, the patterning of the upper layer is performed using SEM-based FIB. The high resolution of the SEM allows for accuracy of the FIB processing process.
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 present invention, the upper layer is patterned according to the physical properties of the upper layer material to define the size and shape of the test module. Wherein the test modules are the same or different in shape; and/or the test modules may be the same or different sizes.
Further, the shape of the test module includes any one or more of: circular cylinder, oval cylinder, square, cuboid.
The shape of the test module differs somewhat for different materials.
If the film layer on the interface to be tested belongs to a brittle material or a friction material (such as SiNx) with low breaking strength or an easily deformable material, the test module can be defined as a circular cylinder or an elliptical cylinder so as to reduce stress concentration and facilitate subsequent interface peeling mechanical test.
The film layer to be tested is made of 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 a cube or other shapes.
In addition, the patterned structure of a device such as a sample semiconductor to be tested mostly has a repetitive structure, and a plurality of to dozens of patterned test module structures with various shapes and/or sizes can be formed by using the FIB automatic patterning technology.
Further, for the analysis of the film bonding force with larger interface bonding strength, the invention also provides a nano-notch solution. A nanometer-sized notch is formed on the interface to be measured by using the FIB technology, so that the interface peeling 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 the stripping interface and effectively improving the success rate of the inter-film stripping test.
In addition, 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.
In different embodiments of the invention, the interface binding force test mode of the nano-film layer can adopt various modes, for example, the test can be carried out in a nano scratch instrument, and the test purpose can be achieved by applying force through a mechanical arm arranged in a sample platform by virtue of a sample platform of an SEM (scanning electron microscope); and so on.
In the present invention, steps (b) to (e) are performed in an apparatus based on FIB and SEM (scanning Electron microscope). The goal of more accurately achieving each step is achieved by high precision and patterning processing by the FIB and high resolution of the SEM.
And (b) to (e), using a tester based on an SEM platform to realize in-situ observation of the dynamic strain and microstructure change of the film interface material to be tested in the testing process, and simultaneously obtaining related experimental data.
For example, the interface of the film layer to be tested is observed by using an observation probe of the SEM, 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 electron microscope, the observation can be continued, the changed pictures are reserved, and good basic data are provided for further analysis.
The sample to be tested related to the invention is a semiconductor device with a plurality of 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 test of the bonding force between different films in a nano device.
The following examples are given for illustration.
Example 1
Specifically, as shown in fig. 2, there may be several tens of process layers in a semiconductor device or the like, and the layers are patterned and interleaved. If the interface of the film layer to be tested is in the bottom process layer of the device (as shown by the arrow in fig. 2 (a)), a corresponding technical solution is needed.
The invention provides a patterning test method for interface bonding force of a device-level nano film layer, which comprises the following specific detection steps:
(1) the film to be tested is known about the specific size and position of the device structure (as shown in fig. 2 (a)).
(2) The sample to be tested is subjected to mechanical and chemical stripping techniques (mechanical stripping such as grinding; chemical stripping such as RIE (reactive ion etch)) to remove the layer until the layer is close to the film layer to be tested.
(3) After mechanical and chemical stripping, a Focused Ion Beam (FIB) technique is used for nanoscale precise stripping, and the upper process film layer closest to the film layer to be tested is removed, so that the film layer to be tested (the dielectric layer, as shown in fig. 2 (b)) is exposed.
(4) And patterning the film layer to be tested by using an FIB technology to form test modules in various shapes suitable for interface test. Such as a cylindrical test module in fig. 3(b) and a rectangular parallelepiped test module in fig. 3 (c).
a. If the film layer on the interface to be tested belongs to a brittle material, the testing module can be defined as a cylinder shape so as to facilitate the subsequent interface peeling mechanical test.
b. If the film on the interface to be tested is a non-brittle material, the test module can be defined as a rectangular parallelepiped or other test module.
Since the patterned structure of a semiconductor device or the like mostly has a repetitive structure, it is possible to form a plurality of to several tens of patterned test module structures of various shapes using FIB automatic patterning technology, as shown in fig. 3(b) and (c).
And (3) putting the sample into a matched nano scratch instrument for nano stripping test analysis. And (3) carrying out interface stripping test analysis by using matched and appropriate test probes 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 interfacial peeling (easy peeling layer) test examples-1 after nano patterning, i.e., peeling test analysis for Cu/Al interface. In fig. 5(a) to (c): a test procedure of a peeling test; FIG. 5(d) SEM observation of the debond interface after the debond test. Surface exfoliation interface is the interface of the nanometal Al and the metal Cu from the results of the exfoliation experiment, the interface separation appears to be along the metal Al/Cu interface. For the Al/Cu nano metal layer, about 60-70 nm of nano Al layer is successfully stripped, and the stripping interface can be observed in situ under SEM. Therefore, the stress test result of the relevant interface bonding force can be verified by SEM analysis.
Example 2
For the analysis of the membrane layer bonding force with larger interfacial bonding strength, the invention also provides a nano-notch solution based on the content of example 1. The mechanism is that the local stress concentration effect of the nanometer notch in the stress test process is utilized, so that the definition of a stripping interface is realized, and the success rate of the stripping test between the film layers is effectively improved. As shown in fig. 6, a nanometer-sized gap is formed at the interface to be measured by using the FIB technology, so that interface peeling of high-strength interface bonding force can be realized, and the purpose of measuring and analyzing the bonding force can be achieved.
FIGS. 7(a) - (c) show the interfacial peeling experiments under patterning and nano-notching techniques. Wherein, FIG. 7(a) FIB patterned dimensions; FIG. 7(b) the beginning of FIB patterning and lift-off testing; FIG. 7(c) results of peel test: nano-notch successfully achieves the definition of the peeling direction of the peeling interface. From the results, the exfoliation interface was along the nano-scale indentations, indicating the feasibility of this technique.
Aiming at the sample to be tested, the patterning test method for the interface binding force of the device-level nano film layer comprises the following specific steps:
and knowing the specific size and position of the film layer to be detected in the device structure.
The sample to be tested is subjected to mechanical and chemical stripping techniques (mechanical stripping: such as grinding; chemical stripping: such as RIE (reactive ion etch)) to remove the layer until the layer is close to the film layer to be tested.
After mechanical and chemical stripping, a Focused Ion Beam (FIB) technology is adopted to carry out nanoscale accurate stripping, an upper process film layer closest to the film layer to be detected is removed, and the film layer to be detected is exposed.
And patterning the film layer to be tested by using FIB technology to form test modules in various shapes suitable for interface test.
And forming a nanometer-sized notch at the interface to be measured by using an FIB technology.
And (3) placing the patterned sample to be tested with the nano notch into corresponding testing equipment (such as a nano scratch tester) to carry out interface peeling and stress measurement.
The nano-strip test also adopts a linear loading test mode, and when the interface is stripped, the test curve has critical stress, and the critical stress corresponds to the interface bonding 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 carried out in a tester based on an SEM platform, the observation of a fracture interface can be directly carried out in the SEM, and whether the interface of film peeling is between the interfaces to be tested or not can be accurately judged, so that high-precision test data can be obtained.
In the present invention, steps (a), (b), (c), (d) and (e) are only used for distinguishing different steps, and cannot be understood as indicating or implying the sequence of steps; the term "plurality" means two or more unless expressly limited otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the description of the present specification, the description of the terms "some embodiments," "some possible implementations," "specific embodiments," etc. means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above 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 a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The patterning test method for the interface bonding force of the device-level nano film layer is characterized by comprising the following steps of:
(a) preparing a sample to be detected;
(b) carrying out nanoscale accurate stripping on the sample to be detected to expose the upper film layer of the interface of the film layer to be detected;
(c) patterning the upper layer film layer to form a test module suitable for testing the bonding force of an interface;
(d) pressurizing the test module to test the bonding force of the interface of the film layer to be tested;
(e) and observing the change of the interface of the film layer to be tested in the testing process, and obtaining a binding force testing result.
2. The method for patterned testing of interfacial bonding force of device-scale nanomembrane layer according to claim 1, wherein in step (a), the sample to be tested is further delaminated by mechanical grinding and/or chemical etching to expose a membrane layer adjacent to an upper membrane layer of the interface of the membrane layer to be tested.
3. The patterned testing method for interfacial bonding force of device-scale nanomembrane layer according to claim 1, wherein in step (b), the sample to be tested is subjected to nano-scale precise stripping by using SEM-based FIB;
and/or
In the step (c), the upper layer film layer is patterned by using an SEM-based FIB.
4. The patterned testing method of interfacial bonding force of device-level nanomembrane layer according to claim 1, wherein the upper film layer is patterned according to physical properties of the upper film layer material to define the size and shape of the testing module;
further, the test modules are the same or different in shape; and/or
The test modules may be the same size or different sizes.
5. The method for patterned testing of interfacial bonding force of device-scale nanomembrane layers according to claim 1, wherein the shape of the test module comprises any one or more of the following: circular cylinder, oval cylinder, square, cuboid.
6. The patterned testing method for interfacial bonding force of device-scale nanomembrane layer according to claim 5, wherein the film to be tested is a brittle material or a deformable material, and the testing 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 testing module is a cuboid or a cube.
7. The method for patterned testing of interfacial bonding force of device-scale nanomembrane layers according to claim 3, further comprising between step (c) and step (d): and arranging a nano notch at the interface of the film layer to be tested, and then pressurizing the testing module at the nano notch to test the bonding force of the interface of the film layer to be tested.
8. The method for patterned testing of interfacial bonding force of device-scale nanomembrane layers according to claim 1, wherein steps (b) to (e) are performed in an FIB and SEM (scanning Electron microscope) based apparatus.
9. The method for patterned testing of interfacial bonding force of device-scale nanomembrane layer according to claim 8, wherein in the step (d) and the step (e), a SEM platform-based tester is used to perform in-situ observation of dynamic strain and microstructure change of the interface material of the film layer to be tested during the testing process, and obtain related experimental data.
10. The method for patterned testing of interfacial bonding force of device-scale nanomembrane layer according to any one of claims 1 to 9, wherein the sample to be tested is a semiconductor device having a plurality of patterned film layers.
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