CN113984469A - Sample and method for preparing same - Google Patents

Sample and method for preparing same Download PDF

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Publication number
CN113984469A
CN113984469A CN202111247841.9A CN202111247841A CN113984469A CN 113984469 A CN113984469 A CN 113984469A CN 202111247841 A CN202111247841 A CN 202111247841A CN 113984469 A CN113984469 A CN 113984469A
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film layer
sample
substrate
prepared
notch
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王超
孙明琛
卫晓阳
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Yangtze Memory Technologies Co Ltd
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Yangtze Memory Technologies Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C26/00Coating not provided for in groups C23C2/00 - C23C24/00
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0095Semiconductive materials

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Abstract

The invention provides a sample and a preparation method thereof, wherein the preparation method of the sample comprises the following steps: providing a sample to be prepared, wherein the sample to be prepared comprises a first substrate, a first film layer arranged in the first substrate, a second substrate and a second film layer arranged in the second substrate, and the first substrate and the second substrate are connected together through the first film layer and the second film layer; the sample to be prepared is placed in the solution so as to form a notch on the longitudinal section of the first film layer and/or the second film layer on one end edge of the sample to be prepared. The sample formed by the method can be used for testing the bonding force between the membranes of the double cantilever beams, the sample preparation rate and the test success rate of the bonding force test between the membranes can be greatly improved, and meanwhile, the method can prepare samples in batches at one time and is simple and easy to implement.

Description

Sample and method for preparing same
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of semiconductors, in particular to a sample and a preparation method thereof.
[ background of the invention ]
Three-dimensional memory (3D NAND Flash) is widely applied to computers, solid state disks and electronic equipment due to the advantages of high storage density, high programming speed and the like. In the manufacturing process of semiconductor structures such as three-dimensional memories, complex stress states are encountered, such as residual stress, thermal stress generated by thermal processing, shear force during chemical mechanical polishing, impact force of scribing process on edges, bending stress during thinning of silicon substrates, and the like. These stresses may lead to inter-film delamination if the inter-film bonding forces in the three-dimensional memory are insufficient. In order to improve reliability of products and stabilize product standardization, it is necessary to evaluate inter-film bonding force in a three-dimensional memory. The key of the inter-membrane binding force test is the preparation of the sample, and the success rate of the inter-membrane binding force test is directly influenced by the quality of the prepared sample. Therefore, the preparation of the sample for testing the inter-membrane bonding force of the three-dimensional memory is very important, and the continuous improvement of the preparation method of the sample for the three-dimensional memory is needed to improve the success rate and the sample preparation efficiency of the inter-membrane bonding force test in the three-dimensional memory.
[ summary of the invention ]
The invention aims to provide a sample and a preparation method thereof, in particular to a sample for testing the membrane binding force and a preparation method thereof, so as to improve the success rate of the membrane binding force test and the sample preparation efficiency of the sample.
In order to solve the above problems, the present invention provides a method for preparing a sample, comprising: providing a sample to be prepared, wherein the sample to be prepared comprises a first substrate, a first film layer arranged in the first substrate, a second substrate and a second film layer arranged in the second substrate, and the first substrate and the second substrate are connected together through the first film layer and the second film layer; the sample to be prepared is placed in the solution so as to form a notch on the longitudinal section of the first film layer and/or the second film layer on one end edge of the sample to be prepared.
Wherein, after putting the sample to be prepared into the solution to form a gap on the longitudinal section of the first film layer and/or the second film layer on one end edge of the sample to be prepared, the method further comprises the following steps:
and attaching the first stressed connecting piece and the second stressed connecting piece to the first substrate and the second substrate at a first adhesion position and a second adhesion position respectively, wherein the longitudinal projections of the first adhesion position and the second adhesion position cover the notches, and a double-cantilever structure is formed at the end edge of the sample to be prepared.
The first stressed connecting piece and the first stressed connecting piece are respectively provided with an external force connecting part for measuring the membrane-to-membrane bonding force between the first substrate and the second substrate through the double-cantilever beam structure.
Wherein the solution is used for etching the first film layer and/or the second film layer.
Wherein, the material of the first film layer and/or the second film layer comprises oxide, and the solution comprises hydrofluoric acid.
Wherein the material of the first film layer and/or the second film layer comprises nitride, and the solution comprises phosphoric acid.
Wherein, after the sample to be prepared is put into the solution, the method further comprises the following steps:
cleaning a sample to be prepared;
and drying the sample to be prepared.
Wherein the first film layer and/or the second film layer comprises an adhesive layer.
Wherein the first film layer and/or the second film layer comprises one or more wire bonding layers.
In order to solve the above problem, an embodiment of the present application further provides a sample, including: the first film layer is arranged in the first substrate; the first substrate and the second substrate are connected together through the first film layer and the second film layer; and a notch is formed on one end edge of the sample and is positioned on the longitudinal section of the first film layer and/or the second film layer, and the notch is formed by etching the first film layer and/or the second film layer through solution.
Wherein the sample further comprises:
the first and second adhesive positions are respectively located on the first and second substrates, and projections of the first and second adhesive positions in the longitudinal direction cover the notch, and the first and second force-bearing connecting pieces are respectively attached to the first and second adhesive positions, thereby forming a double-cantilever structure at the end edge of the sample.
Wherein, the material of the first film layer and/or the second film layer comprises oxide, and the solution comprises hydrofluoric acid.
Wherein the material of the first film layer and/or the second film layer comprises nitride, and the solution comprises phosphoric acid.
Wherein the first film layer and/or the second film layer comprises an adhesive layer.
One of the first substrate and the second substrate comprises an array memory structure, the other substrate comprises peripheral circuits, the first film layer and/or the second film layer comprises one or more wire bonding layers, and the array memory structure is communicated with the peripheral circuits through the wire bonding layers.
The invention has the beneficial effects that: different from the prior art, the invention provides a sample and a preparation method thereof, wherein the preparation method of the sample comprises the following steps: providing a sample to be prepared, wherein the sample to be prepared comprises a first substrate, a first film layer arranged in the first substrate, a second substrate and a second film layer arranged in the second substrate, and the first substrate and the second substrate are connected together through the first film layer and the second film layer; the sample to be prepared is placed in the solution so as to form a notch on the longitudinal section of the first film layer and/or the second film layer on one end edge of the sample to be prepared. The method forms the notch on the longitudinal section of the first film layer and/or the second film layer, can greatly improve the sample preparation rate and the test success rate of the inter-film binding force test, and simultaneously can prepare samples in batches at one time, and is simple and easy to implement.
[ description of the drawings ]
FIG. 1 is a schematic structural diagram of a double cantilever experiment in the prior art;
FIG. 2 is an enlarged schematic view of the oval region of FIG. 1;
FIG. 3 is a schematic flow diagram of a sample preparation method according to an embodiment of the present invention;
FIG. 4 is a schematic structural diagram of a sample made in accordance with one embodiment of the present invention;
FIG. 5 is a schematic diagram of a notch formed in accordance with one embodiment of the present invention;
FIG. 6a is an image taken before a notch is formed according to one embodiment of the present invention;
FIG. 6b is an image taken after a notch has been formed in accordance with one embodiment of the present invention;
figure 7 is a structural schematic diagram of a dual cantilever structure formed in accordance with one embodiment of the present invention.
[ detailed description ] embodiments
The present invention will be described in further detail with reference to the accompanying drawings and examples. It is to be noted that the following examples are only illustrative of the present invention, and do not limit the scope of the present invention. Likewise, the following examples are only some but not all examples of the present invention, and all other examples obtained by those skilled in the art without any inventive step are within the scope of the present invention.
In addition, directional terms mentioned in the present invention, such as [ upper ], [ lower ], [ front ], [ rear ], [ left ], [ right ], [ inner ], [ outer ], [ side ], and the like, refer to directions of the attached drawings only. Accordingly, the directional terms used are used for explanation and understanding of the present invention, and are not used for limiting the present invention. In the various figures, elements of similar structure are identified by the same reference numerals. For purposes of clarity, the various features in the drawings are not necessarily drawn to scale. Moreover, some well-known elements may not be shown in the figures.
It should be understood that the relative arrangement of parts and steps, numerical expressions, and numerical values set forth in these embodiments should not be construed as limiting the scope of the present invention unless it is specifically stated otherwise. Further, the dimensions of the various elements shown in the figures are not necessarily drawn to scale relative to actual dimensions for ease of illustration, e.g., the thickness or width of some layers may be exaggerated relative to other layers. The following description of the exemplary embodiment(s) is merely illustrative and is not intended to limit the invention, its application, or uses in any way. Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification as applicable. It should be noted that like reference numerals and letters refer to like items in the following figures, and thus, once an item is defined or illustrated in one figure, further discussion thereof will not be required in the subsequent description of the figures.
In the prior art, Double Cantilever Beam (DCB) experiments are mostly adopted to test the membrane-to-membrane bonding force between membrane layers. As shown in fig. 1, which is a schematic structural diagram of a dual cantilever experiment in the prior art, a sample 100 to be tested includes a first substrate 110, a first film 120, a second film 130, a third film 140, and a second substrate 150, which are sequentially stacked and connected, and aluminum blocks 160 with circular holes are respectively adhered to the first substrate 110 and the second substrate 150 on the upper and lower sides of the leftmost end of the sample 100 to be tested, so as to form a dual cantilever structure. After the double cantilever beam structure is formed, a certain film layer between the first substrate 110 and the second substrate 150, for example, the second film layer 130 as shown in fig. 2, is torn by applying an upward force P1 and a downward force P2 to the aluminum blocks 160 on the first substrate 110 and the second substrate 150, respectively, so as to test the inter-film bonding force of the sample 100 to be tested.
In addition, the current double cantilever test also requires a notch (i.e., notch)170 to be prepared during the sample preparation process as a guide for the inter-membrane delamination (propagation), i.e., a notch 170 is prepared in the middle membrane layer between the first substrate 110 and the second substrate 150 in the sample 100 to be tested. In order to prepare a notch 170 in the middle film layer, a wire cutting grooving method is generally used at present, for example, a wire cutting diamond is used to form a notch 170 on a longitudinal (Y direction shown in fig. 1) section of one end of the sample 100 to be measured, however, the wire cutting grooving in the prior art has disadvantages: first, when diamond wire cutting is used, the grooves are easily cut askew, which may result in rejection of the test sample; second, the wire-cut notch 170 is too wide (width dimension greater than 0.36mm), which makes the crack propagation random, and easily causes micro-cracks to occur on the first substrate or the second substrate; thirdly, the wire cutting can only prepare one notch on the sample 100 to be measured at one time, but cannot prepare one notch on each of the samples 100 to be measured at the same time, and cannot meet the requirement of one-time batch production. The sample preparation efficiency of the test sample is low due to the three reasons, so that the test success rate of the double-cantilever experiment is low.
In view of this, as shown in fig. 3, the present invention provides a schematic flow chart of a method for preparing a sample 200, and the specific flow chart is compared with the structural charts of fig. 4 to fig. 7, and may include the following steps:
s101, a step: providing a sample to be prepared, wherein the sample to be prepared comprises a first substrate 210, a first film layer 211 arranged in the first substrate 210, a second substrate 220, and a second film layer 221 arranged in the second substrate 220, and the first substrate 210 and the second substrate 220 are connected together through the first film layer 211 and the second film layer 221.
Fig. 4 shows the structure formed in step S101, including: the first substrate 210, the first film 211 disposed in the first substrate 210, the second substrate 220, and the second film 221 disposed in the second substrate 220, wherein the first substrate 210 and the second substrate 220 are connected together through the first film 211 and the second film 221.
Specifically, the first base 210 and the second base 220 may include a substrate as a base for forming a semiconductor device, and the substrate is a semiconductor material, which may be silicon (Si), germanium (Ge), or silicon germanium (GeSi), silicon carbide (SiC), or the like, or may be another material. In addition, the first base 210 and the second base 220 may further include a substrate and one or more other film layers formed on the substrate, such as an oxide film layer (SiO film layer)2) The silicon nitride film (SiN), silicon oxynitride film (SiON), or the like, and may also include a substrate and an active device or a passive device formed on the substrate, which is not particularly limited.
Wherein the first film layer 211 and/or the second film layer 221 comprise an adhesive layer.
Specifically, the first substrate 210 and the second substrate 220 may be from two independent wafers (wafers), and in this case, the sample preparation process for forming the sample to be prepared may be: first, two bare wafers (i.e., control wafers, also referred to as CDWs) are selected, such as a first wafer and a second wafer. Subsequently, one or more layers are deposited on the first wafer and the second wafer, respectively, by a deposition process. The film formed on the first wafer is the first film 211, and the film formed on the second wafer is the second film 221. Then, the first film layer 211 and/or the second film layer 221 are bonded to the two wafers by an adhesive. And finally, performing one or more times of cutting, polishing, thinning and the like on the two bonded wafers to form a sample to be prepared. When the first film layer 211 and/or the second film layer 221 include an adhesive layer, the sample to be prepared may be sampled from a structure formed by two wafers after depositing some film layers and adhering them together by an adhesive, and when the sample 200 is subjected to the double cantilever test, the inter-film bonding force of the film layers between the first wafer and the second wafer is tested.
Wherein one of the first substrate 210 and the second substrate 220 includes an array memory structure, the other includes peripheral circuits, and the first film layer 211 and/or the second film layer 221 include one or more wire bonding layers, and the array memory structure is communicated with the peripheral circuits through the wire bonding layers.
Specifically, the first substrate 210 and the second substrate 220 may be from two independent wafers, and in this case, the sample preparation process for forming the sample to be prepared may be: first, two wafers that have completed all processes are selected, for example, a first wafer on which an Array memory cell (Array) has been formed and a second wafer on which a peripheral Circuit (peripheral Circuit) that controls the Array memory cell has been formed. The array memory structure is used for storing information, and the peripheral circuit can be positioned above or below the array memory structure and used for controlling the corresponding array memory structure. Then, the first wafer and the second wafer are wire bonded (Bonding) to form an integral structure, that is, the first film layer 211 and/or the second film layer 221 include one or more wire Bonding layers, and the array memory structure is communicated with the peripheral circuit through the wire Bonding layers. And finally, performing one or more times of cutting, grinding, thinning and the like on the two wafers which form an integral structure to form a sample to be prepared. When the first film 211 and/or the second film 221 includes one or more wire bonding layers, the sample to be prepared may be sampled from an integrated structure formed by wire bonding the first wafer and the second wafer, and when the sample 200 is subjected to the dual cantilever test, the inter-film bonding force between the bonding interfaces of the one or more wire bonding layers between the first wafer and the second wafer is tested.
In addition, it should be noted that the first substrate 210 and the second substrate 220 may be wafers from a control wafer or a wafer that has completed all process flows, or may be semi-finished wafers after any process flows, as long as testing of the film-to-film bonding force of the film layer between the first substrate 210 and the second substrate 220 is achieved, and the structure included in the first substrate 210 and the second substrate 220 is not particularly limited. Accordingly, the structures included in the first film layer 211 and the second film layer 221 are not particularly limited.
S102, a step: the sample to be prepared is placed in the solution to form a notch 230 in the longitudinal cross-section of the first film layer 211 and/or the second film layer 221 at one end edge of the sample to be prepared.
Fig. 5 shows the structure formed in step S102, which includes: the first substrate 210, the first film layer 211 disposed in the first substrate 210, the second substrate 220, the second film layer 221 disposed in the second substrate 220, and a notch 230 formed on an end edge of a sample to be prepared and located on a longitudinal (i.e., Y-direction as shown in fig. 5) cross section of the first film layer 211 and/or the second film layer 221, wherein the first substrate 210 and the second substrate 220 are connected together through the first film layer 211 and the second film layer 221. In addition, it should be noted that, for convenience of description, the notch 230 is only a schematic structural diagram.
Wherein the solution is used to etch the first film layer 211 and/or the second film layer 221.
Specifically, as can be seen from the above, in the sample preparation process of the dual cantilever test, the notch 230 needs to be prepared as a guide for the inter-membrane delamination, that is, a notch 230 needs to be formed on one end edge of the first membrane layer 211 and/or the second membrane layer 221, and compared to the problem of the prior art that the notch 230 formed by wire cutting has an excessively large width and cannot form an oriented notch 230, based on the advantages of simple process equipment, low cost, and high etching precision of wet etching, the first membrane layer 211 or the second membrane layer 221 can be etched by wet etching, such as by using the first solvent, to form a notch 230 on one end edge of the first membrane layer 211 or the second membrane layer 221, or the first membrane layer 211 and the second membrane layer 221 are etched by solution, to form a notch 230 on one end edge of the first membrane layer 211 and the second membrane layer 221.
Compared with the notch 230 formed by the wire-cutting grooving in the prior art, the notch 230 formed by the wet etching is smaller in size due to the fact that the accuracy of the wet etching is higher than that of the wire-cutting grooving, so that the nanoscale notch 230 can be formed, and the nanoscale notch 230 is very favorable for forming the notch 230 on a required film layer to obtain the required film-to-film bonding force. For example, the notch 230 may be formed on the directional film layer by selecting a wet etching solution having a higher selection ratio for the film layer to be etched than for other film layers, and the notch 230 formed on the directional film layer is beneficial to quickly finding the weakest cross section between the films after the crack is induced from the notch 230 to obtain the required inter-film bonding force, thereby greatly improving the sample preparation rate and the test success rate of the inter-film bonding force test. Meanwhile, the method for forming the notch 230 by wet etching is cheaper and simpler and easier to implement.
Specifically, a plurality of samples to be prepared may be put into the solution, for example, 6 to 8 samples to be prepared may be put into the solution at a time, so as to form a notch 230 on a longitudinal section of the first film layer 211 and/or the second film layer 221 on one end edge of each of the plurality of samples to be prepared, thereby realizing one-time mass sample preparation, and the method is simple and easy.
In addition, the solution may be any material that can react with the first film layer 211 and/or the second film layer 221 to form the notch 230, as long as one notch 230 can be formed on one end edge of the first film layer 211 and/or the second film layer 221 by the solution, and the material of the solution is not particularly limited. In addition, it should be noted that one or more samples to be prepared may be adhered to the beam by rosin to adjust the immersion depth of the one or more samples to be prepared into the solution, and correspondingly, the depth of the gap 230 may be adjusted.
The material of the first film layer 211 and/or the second film layer 221 includes an oxide, and the solution includes hydrofluoric acid.
Specifically, as can be seen from the above, no particular limitation is imposed on the structure of the first film layer 211 and/or the second film layer 221, and correspondingly, no particular limitation is imposed on the material of the first film layer 211 and/or the second film layer 221. Generally, the first film layer 211 and the second film layer 221 between the first substrate 210 and the second substrate 220 are mostly insulating materials, such as oxide. When the material of the first film 211 and the second film 221 is an oxide, such as silicon dioxide (SiO)2) At this time, the solution may be a solution containing hydrofluoric acid (HF).
Specifically, for example, the process of forming the notch 230 on the first film layer 211 and the second film layer 221 includes: firstly, selecting a certain number of samples to be prepared, such as 6 to 8 samples to be prepared, adhering a plurality of samples to be prepared on a beam by using rosin, and adhering the beam on a beaker by using the rosin, so that a part of the samples to be prepared are immersed in a solution, and the immersion depth of the samples to be prepared in the solution is adjustable; secondly, a certain volume (selected according to actual conditions, such as 30ml) of solution (the solution can be BOE etchant, and the BOE etchant is prepared from 49% HF aqueous solution and 40% NH in a volume ratio of 1:64Aqueous solution of F) was poured into a beaker, in which NH was in solution4F is used as a buffer by using NH4F fixes the concentration of H + to maintain a certain etching rate, and hydrofluoric acid is mainly used as an etching solution to chemically react with the silicon dioxide of the first film 211 and the second film 221, thereby forming a notch 230 on the first film 211 and the second film 221.
Specifically, the chemical equation of the above reaction is: SiO 22(s)+4HF(l)=SiF4(g)↑+2H2O (l) is an image of a longitudinal section of an end of a sample to be prepared before the sample is put into the solution as shown in FIG. 6a, in which the longitudinal section is free of the notch 230, and as shown in FIG. 6b, is an image of a longitudinal section of the sample to be preparedThe image of the longitudinal section after the solution is laterally placed for 24h, at this time, it can be seen that a gap 230 is formed on the longitudinal section, and the width dimension of the gap 230 can be found to be 300-600nm by measurement software, whereas the width dimension of the gap 230 formed by the wire cutting notch in the prior art is larger than 3.6um, and the dimension of the gap 230 formed by the BOE etchant is smaller and is nano-scale. Meanwhile, experiments show that compared with the prior art that the success rate of sample preparation obtained by a wire-electrode cutting grooving method is only 10%, the success rate of sample preparation for forming the notch 230 by using the BOE etching agent can be up to 70%, and the success rate of sample preparation is greatly improved. The hydrofluoric acid in the solution chemically reacts with the first film layer 211 and the second film layer 221, so that a notch 230 is formed at the interface where the first film layer 211 and the second film layer 221 contact the solution, and the depth of the notch 230 can be adjusted by adjusting the immersion depth.
Specifically, relative to prior art wire-cut trenching, the notch 230, which may be on the order of nanometers, is formed by hydrofluoric acid. Meanwhile, other film layers may exist in the first substrate 210 and the second substrate 220, such as the first substrate and the second substrate, generally, the material of the first substrate and the second substrate is silicon, hydrofluoric acid in a solution may rapidly chemically react with the first film layer 211 and the second film layer 221 to form the notch 230, but does not react with silicon in the first substrate 210 and the second substrate 220, and the notch 230 may be directionally formed on the first film layer 211 and the second film layer 221 by selecting the solution without damaging other film layers that do not need to form the notch 230, which is beneficial to rapidly finding the weakest cross section between films after a crack is induced from the notch 230, obtaining the required bonding force between films, and thus greatly improving the sample preparation rate and the test success rate of the bonding force test between films. In addition, the method of forming the notch 230 using hydrofluoric acid is cheaper and easier to implement.
In addition, the solution containing hydrofluoric acid is not particularly limited, and the solution may be other solutions besides the BOE etchant, as long as the solution contains hydrofluoric acid and can form the gap 230 in the first film layer 211 and/or the second film layer 221.
Wherein the material of the first film layer 211 and/or the second film layer 221 includes nitride, and the solution includes phosphoric acid.
Specifically, as can be seen from the above, in general, the first film layer 211 and the second film layer 221 located between the first substrate 210 and the second substrate 220 are mostly insulating materials, and different from the scheme that the material of the first film layer 211 and/or the second film layer 221 includes oxide, the material of the first film layer 211 and/or the second film layer 221 may also include nitride, for example, when the material of the first film layer 211 and the second film layer 221 is silicon nitride (SiN), the solution may be a solution containing phosphoric acid (H) and (H) may be silicon nitride (SiN)3PO4) The solution, such as hot phosphoric acid, reacts with the silicon nitride in the first film layer 211 and the second film layer 221 through the hot phosphoric acid, so that a nanoscale notch 230 is formed at the interface where the first film layer 211 and the second film layer 221 contact the solution, and the depth of the notch 230 can be adjusted by adjusting the immersion depth. From the above, it can be known that the gaps 230 can be directionally formed on the first film layer 211 and the second film layer 221 by selecting the hot phosphoric acid as the solution without damaging other film layers that do not need to form the gaps 230, which is beneficial to quickly find the weakest cross section between the films after the cracks are induced from the gaps 230 to obtain the required bonding force between the films, thereby greatly improving the sample preparation rate and the test success rate of the bonding force test between the films. In addition, the method of forming the notch 230 using hot phosphoric acid is cheaper and simpler and easier to implement.
In addition, since the experiment process and the principle of the solution containing hydrofluoric acid reacting with the first film layer 211 and/or the second film layer 221 to form the notch 230 have been described in detail above, the experiment process and the principle of the solution containing phosphoric acid reacting with the solution containing hydrofluoric acid are substantially the same, and will not be described herein again.
After the step S102, the method further includes:
s103, a step: the first force-receiving connector 240 and the second force-receiving connector 250 are attached to the first substrate 210 and the second substrate 220 at a first adhesion position and a second adhesion position, respectively, and projections of the first adhesion position and the second adhesion position in the longitudinal direction cover the notch 230, so as to form a double-cantilever structure at the edge of the sample to be prepared.
Fig. 7 shows the structure formed in step S103, which includes: the first substrate 210, the first film 211 disposed in the first substrate 210, the second substrate 220, the second film 221 disposed in the second substrate 220, a notch 230 formed on an end edge of a sample to be prepared and located on a longitudinal section of the first film 211 and/or the second film 221, a first force-receiving connector 240 and a second force-receiving connector 250 attached to the first adhesion position and the second adhesion position, respectively, wherein the first substrate 210 and the second substrate 220 are connected together through the first film 211 and the second film 221.
Specifically, as shown in fig. 7, the first adhesion position and the second adhesion position are respectively located above the edge of one end of the first substrate 210 and the second substrate 220, and the first force-receiving connector 240 and the second force-receiving connector 250 are adhered to the first substrate 210 and the second substrate 220, so as to form a double cantilever structure at the end edge of the sample to be prepared, and at the same time, the projections of the first adhesion position and the second adhesion position in the longitudinal direction cover the notch 230, i.e. the notch 230 on the sample to be prepared and the edges of the first force-receiving connector 240 and the second force-receiving connector 250 are located at the same end, and the projection of the notch 230 is within the range of the first force-receiving connector 240 and the second force-receiving connector 250. By adopting solution to etch the first film layer 211 and/or the second film layer 221, a nanoscale gap 230 is directionally formed on the longitudinal section of one end edge of the first film layer 211 and/or the second film layer 221, so that a chemical method is firstly applied to a sample preparation process of a double-cantilever beam experiment in the industry, directional layering can be promoted, inter-film binding force test can be realized, the method can also be applied to control wafers of different types and finished wafers with lead bonding layers, and meanwhile, compared with a method for preparing a sample by linear cutting slotting, the method provided by the embodiment of the application can prepare samples in batches at one time, and is simple and easy to implement.
The first force-receiving connector 240 and the second force-receiving connector 250 each have an external force connection portion for measuring the membrane-to-membrane bonding force between the first substrate 210 and the second substrate 220 by a dual cantilever beam structure.
Specifically, when an upward force P3 and a downward force P4 are applied to the first force-bearing link 240 and the second force-bearing link 250, respectively, such that one of the films between the first substrate 210 and the second substrate 220, for example, the first film 211 or the second film 221, is torn, the inter-film bonding force between the first substrate 210 and the second substrate 220 is measured by the double cantilever beam structure.
Wherein, after the sample to be prepared is put into the solution, the method further comprises the following steps:
cleaning a sample to be prepared;
and drying the sample to be prepared.
Specifically, in executing step S102: after the sample to be prepared is put into the solution to form a gap 230 on a longitudinal section of the first film layer 211 and/or the second film layer 221 at one end edge of the sample to be prepared, one or more times of washing processes are required to remove the residue on the surface of the sample to be prepared, for example, the sample to be prepared is washed with Deionized Water (also called DI Water, Deionized Water) for two minutes (the time can be adjusted according to actual conditions). Subsequently, the sample to be prepared may be subjected to a drying treatment, for example, the sample to be prepared may be placed in an oven to be baked at a temperature of 40 ℃ for ten minutes (the time and temperature may be adjusted according to actual conditions) to obtain a dried sample to be prepared.
Based on the preparation method of the sample described in the above embodiment, the embodiment of the present application further provides a sample, including: a first substrate 210 and a first film layer 211 disposed in the first substrate 210; a second substrate 220 and a second film 221 disposed in the second substrate 220, wherein the first substrate 210 and the second substrate 220 are connected together through the first film 211 and the second film 221; a notch 230 is formed on an edge of the sample 200, and is located on a longitudinal cross section of the first film 211 and/or the second film 221, and the notch 230 is formed by solution etching the first film 211 and/or the second film 221.
Wherein, sample 200 further comprises:
the first and second adhesion positions are located on the first and second substrates 210 and 220, respectively, and the projections of the first and second adhesion positions in the longitudinal direction cover the gap 230, and the first and second force-bearing connectors 240 and 250 are attached to the first and second adhesion positions, respectively, so as to form a double-cantilever structure at the end edge of the sample 200.
As shown in fig. 7, which is a schematic structural diagram of the dual cantilever structure formed in an embodiment of the present invention, compared to the gap 230 formed by the wire-cutting process in the prior art, the gap 230 formed by solution etching the first film layer 211 and/or the second film layer 221 (i.e., wet etching) is smaller in size, so that a nanoscale gap 230 can be formed, and the nanoscale gap 230 is very advantageous to directionally form the gap 230 in a desired film layer, so as to obtain a desired inter-film bonding force. For example, the notch 230 may be formed on the directional film layer by selecting a wet etching solution having a higher selection ratio for the film layer to be etched than for other film layers, and the notch 230 formed on the directional film layer is beneficial to quickly finding the weakest cross section between the films after the crack is induced from the notch 230 to obtain the required inter-film bonding force, thereby greatly improving the sample preparation rate and the test success rate of the inter-film bonding force test. Meanwhile, compared with a method for preparing a sample by cutting and slotting by a wire, the method for forming the notch 230 by wet etching is cheaper and simpler and easier to implement.
The material of the first film layer 211 and/or the second film layer 221 includes an oxide, and the solution includes hydrofluoric acid.
Specifically, when the material of the first film layer 211 and/or the second film layer 221 is an oxide, for example, the material of the first film layer 211 and/or the second film layer 221 is silicon oxide, based on the chemical principle, a solution (e.g., BOE etchant) containing hydrofluoric acid may be selected to react with the silicon oxide in the first film layer 211 and/or the second film layer 221, so as to form a notch 230 at the interface where the first film layer 211 and/or the second film layer 221 contacts the solution, and the depth of the notch 230 may be adjusted by adjusting the immersion depth of the sample 200 in the solution, as compared with the prior art of linear cutting, a notch 230 that may be formed in a nanometer scale by hydrofluoric acid may be formed, and at the same time, as can be known from the foregoing, by selecting the etching selection ratio of the solution, the notch 230 may be directionally formed on the first film layer 211 and/or the second film layer 221 without damaging other film layers that do not need to form the notch 230, the weakest cross section between the membranes can be found quickly after the cracks are induced from the notch 230, and the required binding force between the membranes can be obtained, so that the sample preparation rate and the test success rate of the binding force test between the membranes can be greatly improved. At the same time, the method of forming the notch 230 using hydrofluoric acid is cheaper and easier to implement.
Wherein the material of the first film layer 211 and/or the second film layer 221 includes nitride, and the solution includes phosphoric acid.
Specifically, when the material of the first film layer 211 and/or the second film layer 221 is a nitride, for example, the material of the first film layer 211 and/or the second film layer 221 is silicon nitride, based on the chemical principle, a solution containing phosphoric acid (for example, hot phosphoric acid) may be selected to react with silicon oxide in the first film layer 211 and/or the second film layer 221, so as to form a notch 230 at the interface where the first film layer 211 and/or the second film layer 221 contacts with the solution, and the depth of the notch 230 may be adjusted by adjusting the immersion depth of the sample 200 in the solution, and compared to the prior art of line cutting, the notch 230, which may be formed by hydrofluoric acid, may be formed in a nanometer scale, and at the same time, as can be known from the foregoing, the notch 230 may be directionally formed on the first film layer 211 and/or the second film layer 221 by selecting the etching selection ratio of the solution, without damaging other film layers that do not need to form the notch 230, the weakest cross section between the membranes can be found quickly after the cracks are induced from the notch 230, and the required binding force between the membranes can be obtained, so that the sample preparation rate and the test success rate of the binding force test between the membranes can be greatly improved. At the same time, the method of forming the notch 230 using phosphoric acid is cheaper and simpler and easier to implement.
Wherein the first film layer 211 and/or the second film layer 221 comprise an adhesive layer.
Specifically, when the first film 211 and/or the second film 221 include an adhesive layer, as described above, the sample 200 may be sampled from a structure formed by two wafers with some films deposited thereon and then glued together, and when the sample 200 is subjected to the double cantilever test, the inter-film bonding force of the films between the first wafer and the second wafer is tested.
Wherein one of the first substrate 210 and the second substrate 220 includes an array memory structure, the other includes peripheral circuits, and the first film layer 211 and/or the second film layer 221 include one or more wire bonding layers for connecting the array memory structure and the peripheral circuits.
Specifically, when the first film layer 211 and/or the second film layer 221 includes an adhesive layer, as can be seen from the above, the sample 200 may be sampled from a bulk structure formed by wire Bonding (Bonding) a first wafer and a second wafer, and when the sample 200 is subjected to the dual cantilever beam test, the inter-film Bonding force between the Bonding interfaces of one or more wire Bonding layers between the first wafer and the second wafer is tested.
In addition, it should be noted that the first substrate 210 and the second substrate 220 may be derived from a control wafer or a wafer that has completed all process flows, or may be derived from a semi-finished wafer after any process flows, as long as testing of the film-to-film bonding force between the first substrate 210 and the second substrate 220 can be achieved, and the structure included in the first substrate 210 and the second substrate 220 is not particularly limited, and correspondingly, the structure included in the first film layer 211 and the second film layer 221 is not particularly limited.
Different from the prior art, the sample and the preparation method thereof in this embodiment include: providing a sample to be prepared, wherein the sample to be prepared comprises a first substrate, a first film layer arranged in the first substrate, a second substrate and a second film layer arranged in the second substrate, and the first substrate and the second substrate are connected together through the first film layer and the second film layer; the sample to be prepared is placed in the solution so as to form a notch on the longitudinal section of the first film layer and/or the second film layer on one end edge of the sample to be prepared. The sample formed by the method can be used for testing the bonding force between the membranes of the double cantilever beams, the sample preparation rate and the test success rate of the bonding force test between the membranes can be greatly improved, and meanwhile, the method can prepare samples in batches at one time and is simple and easy to implement.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (15)

1. A method of preparing a sample, comprising:
providing a sample to be prepared, wherein the sample to be prepared comprises a first substrate, a first film layer arranged in the first substrate, a second substrate and a second film layer arranged in the second substrate, and the first substrate and the second substrate are connected together through the first film layer and the second film layer;
and putting the sample to be prepared into the solution so as to form a notch on the longitudinal section of the first film layer and/or the second film layer on one end edge of the sample to be prepared.
2. The method for preparing a sample according to claim 1, further comprising, after the step of placing the sample to be prepared in the solution to form a notch on a longitudinal cross section of the first film layer and/or the second film layer at an end edge of the sample to be prepared:
and attaching a first stressed connecting piece and a second stressed connecting piece to the first substrate and the second substrate at a first adhesion position and a second adhesion position respectively, wherein projections of the first adhesion position and the second adhesion position in the longitudinal direction cover the notch, and a double-cantilever structure is formed at the end edge of the sample to be prepared.
3. The method of claim 2, wherein the first force-bearing link and the first force-bearing link each have an external force link for measuring an inter-membrane bonding force between the first substrate and the second substrate via the dual cantilever beam structure.
4. The method of preparing a sample according to claim 1, wherein the solution is used to etch the first and/or second membrane layer.
5. The method of preparing a sample of claim 1, wherein the material of the first film layer and/or the second film layer comprises an oxide and the solution comprises hydrofluoric acid.
6. The method of preparing a sample according to claim 1, wherein the material of the first film layer and/or the second film layer comprises a nitride, and the solution comprises phosphoric acid.
7. The method for preparing a sample according to claim 1, further comprising, after the placing the sample to be prepared in a solution:
cleaning the sample to be prepared;
and drying the sample to be prepared.
8. The method of preparing a sample according to claim 1, wherein the first film layer and/or the second film layer comprises an adhesive layer.
9. The method of sample preparation of claim 1, wherein the first film layer and/or the second film layer comprises one or more wire bonding layers.
10. A sample, comprising:
the film comprises a first substrate and a first film layer arranged in the first substrate;
the first substrate and the second substrate are connected together through the first film layer and the second film layer;
and a notch is formed on one end edge of the sample and is positioned on the longitudinal section of the first film layer and/or the second film layer, and the notch is formed by etching the first film layer and/or the second film layer through solution.
11. The sample of claim 10, wherein the sample further comprises:
the first and second adhesion positions are respectively located on the first and second substrates, and projections of the first and second adhesion positions in the longitudinal direction cover the notch, and the first and second force-bearing connectors are respectively attached to the first and second adhesion positions, so that a double-cantilever structure is formed at the end edge of the sample.
12. The sample of claim 10, wherein the material of the first film layer and/or the second film layer comprises an oxide and the solution comprises hydrofluoric acid.
13. The sample of claim 10, wherein the material of the first membrane layer and/or the second membrane layer comprises a nitride and the solution comprises phosphoric acid.
14. The sample of claim 10, wherein the first film layer and/or the second film layer comprises an adhesive layer.
15. The sample of claim 10, wherein one of the first and second substrates comprises an array memory structure and the other comprises peripheral circuitry, and wherein the first and/or second film layers comprise one or more wire bonding layers through which the array memory structure is in communication with the peripheral circuitry.
CN202111247841.9A 2021-10-26 2021-10-26 Sample and method for preparing same Pending CN113984469A (en)

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