CN113218755B - System for biaxial tension test of nanoscale film and manufacturing method thereof - Google Patents
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- CN113218755B CN113218755B CN202110441939.1A CN202110441939A CN113218755B CN 113218755 B CN113218755 B CN 113218755B CN 202110441939 A CN202110441939 A CN 202110441939A CN 113218755 B CN113218755 B CN 113218755B
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
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- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B21/00—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
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- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
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- G01N2203/006—Crack, flaws, fracture or rupture
- G01N2203/0067—Fracture or rupture
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- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
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- G01N2203/0212—Theories, calculations
- G01N2203/0216—Finite elements
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
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- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/0605—Mechanical indicating, recording or sensing means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
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Abstract
The invention provides a system for biaxial tensile test of a nanoscale film and a manufacturing method thereof, belonging to the technical field of microelectronic mechanical system processing, wherein the system combines a uniquely designed on-chip testing machine structure with a probe station for microelectronic process detection and analysis to extract biaxial stress when the nanoscale film is broken, wherein the on-chip testing machine comprises two tensile structures which are vertically arranged; each stretching structure comprises a probe loading structure, a two-wheel loading reversing structure, a movable frame, an elastic beam, a stretching beam, two deformation variable scaleplates, two pointers and two hanging folding beams. The system can be used for exploring the damage rule of the film material under the nanoscale, and can also be used for monitoring the quality of the film preparation process.
Description
Technical Field
The invention belongs to the technical field of micro-electro-mechanical system (MEMS) processing, relates to a system for biaxial tensile test of a nanoscale film and a manufacturing method thereof, and is particularly applied to researching the damage rule of a film material under nanoscale.
Background
Failure behaviour will occur when the structure is subjected to an external load exceeding a critical value. Determining whether a structure will fail under a given external load is an important issue because the structure faces the challenge of possible failure from initial manufacture to final use. To solve this problem, elastomechanics and strength theory is established. The elastic mechanics is responsible for calculating the internal stress of the structure caused by external load, and the strength theory is responsible for judging whether the material fails in a certain stress state, so the strength theory is also called as a material fracture criterion (criterion). The criteria for breaking a material need to be based on a large number of experiments, which typically require biaxial tensile testing of material specimens to extract different internal stress conditions when the material is damaged. The traditional biaxial tensile testing machine is only suitable for testing millimeter and above samples. In the present day that micro-nano processing technology is rapidly developed and MEMS/NEMS devices are continuously emerging, the research of the damage rule of materials under the micro-nano scale becomes the core basic work influencing the development of the industry. For micro-nano-scale samples, corresponding detection means are still lacking at present because of the difficulties in fastening, loading, detection and the like. Therefore, a more reasonable method needs to be provided for biaxial tensile testing of the micro-nano scale sample to extract the biaxial stress when the micro-nano scale sample is broken, so that the damage rule of the material under the micro-nano scale is researched.
Disclosure of Invention
According to the analysis, the biaxial stress of the micro-nano scale film sample at the time of fracture can not be extracted by using the traditional biaxial tensile testing machine, the invention aims to provide a system for extracting the biaxial stress of the nano scale film sample at the time of fracture and a manufacturing method thereof. The method can be used for researching the damage rule of the film material under the nanoscale, and can also be used for monitoring the quality of the film preparation process.
The technical scheme adopted by the invention is as follows:
a system for biaxial tensile test of a nanoscale film comprises an on-chip testing machine and a probe station for applying a load force to the on-chip testing machine, wherein the on-chip testing machine comprises two tensile structures which are vertically arranged; each stretching structure comprises a probe loading structure, a two-wheel loading reversing structure, a movable frame, an elastic beam, a stretching beam, two deformation variable scaleplates, two pointers and two hanging folding beams; the probe loading structure is used for bearing the probe loading of the probe station; the two wheel-shaped loading reversing structures are positioned on two symmetrical sides of the probe loading structure and respectively comprise a wheel-shaped structure and a plurality of spoke beams, two opposite sides of the two wheel-shaped structure are connected to the probe loading structure, the two opposite sides of the two wheel-shaped structure are connected to two front arm beams of the movable frame, and the spoke beams connect the wheel-shaped structure to a first anchor point of a wheel-shaped axis; the movable frame comprises two front arm beams extending towards the direction of the two-wheel-shaped loading reversing structure and two rear arm beams deviating from the direction, the rear ends of the two front arm beams and the front ends of the two rear arm beams are fixed with each other, the two front arm beams and the two rear arm beams are respectively and symmetrically distributed, and the inner sides of the rear ends of the two rear arm beams are provided with the two deformation scaleplates; one end of each of the two hanging folding beams is connected to two sides of the movable frame, and the other end of each of the two hanging folding beams is fixed to the two second anchor points; the elastic beam is vertically connected with the two rear arm beams of the movable frame; the stretching beam comprises a vertical beam and a cross beam, the vertical beam is arranged in the middle of the two rear arm beams of the movable frame in parallel, one end of the vertical beam is connected to the middle of the elastic beam, and the other end of the vertical beam is connected with one edge of a square film sample; the middle part of the cross beam is vertically connected to the vertical beam, and two ends of the cross beam are provided with the two pointers; the two pointers are respectively used for marking the scales of the two deformation variable scaleplates; and two adjacent edges of the film sample which are not connected by the stretching beams of the two stretching structures are respectively and fixedly connected with the two third anchor points.
Furthermore, the probe loading structure is provided with a V-shaped loading port, so that the accuracy of a loading position and the direction of a loading force can be ensured.
Furthermore, the distance between the two rear arm beams of the movable frame is narrower than the distance between the two front arms, the front arm beam and the rear arm beam on each side are connected through a shoulder beam perpendicular to the front arm beams, and one end of the suspension folding beam is specifically connected to the shoulder beam.
Furthermore, the spoke beams of the wheel-shaped loading reversing structure are uniformly distributed around the first anchor point in the circumferential direction.
Furthermore, two adjacent hanging folding beams of the two stretching structures are connected to the same second anchor point.
Furthermore, the first anchor point is a diamond-shaped or round-section anchor point, the second anchor point is a square-section anchor point, and the third anchor point is a rectangular-section anchor point.
Furthermore, four vertexes of the square of the film sample contain the same triangular notch, and the shape design can enable the internal test area to be in a uniform stress state and the stress level to be higher.
Further, the thickness of the film sample is in nanometer level, and the length and width are in micrometer level.
A method of manufacturing a system for biaxial tensile testing of nano-scale thin films, comprising manufacturing an on-chip tester and a probe station, wherein the step of manufacturing the on-chip tester comprises:
(1) forming bonding anchor points on the front surface of the silicon wafer by photoetching and etching, wherein the anchor points comprise a first anchor point, a second anchor point and a third anchor point;
(2) depositing a film material on the front surface of the silicon wafer, and forming a film sample pattern by utilizing photoetching, corrosion or etching according to the plane shape and the size of the film sample;
(3) forming shallow grooves on a glass sheet by photoetching and wet etching, sputtering metal on the glass sheet, and forming a metal electrode for preventing sputtering by using a stripping process;
(4) carrying out anodic bonding on the silicon wafer and the glass sheet which are treated by the steps;
(5) using wet etching to thin the silicon chip to the designed thickness;
(6) the silicon wafer is partially etched through from the back side by photolithography and deep etching to release the movable structures, i.e., all the silicon structures except the anchor points, and the on-chip tester is obtained.
Furthermore, the silicon wafer is an N-type monocrystalline silicon wafer, and the resistivity is 0.001-0.003 omega-cm; and etching the silicon by using an ASE dry method to form bonding anchor points.
Further, a thin film material is deposited on the front side of the silicon wafer by PVD, CVD, ALD or electroplating.
Further, three metals of Ti, Pt and Au were sputtered on the glass sheet.
The invention designs a corresponding on-chip testing machine structure in order to extract the biaxial stress of a nanoscale film sample when the nanoscale film sample is broken, and provides a system for extracting the biaxial stress of the nanoscale film sample when the nanoscale film sample is broken by combining an on-chip testing machine and a probe station for microelectronic process detection and analysis. The spring beam is used to measure the tensile force experienced by the ends of the film sample. The deformation quantity scale is used for recording deformation information of the elastic beam. The suspension folding beam group is used for supporting the whole suspension structure, and the support stability of the on-chip testing machine in the manufacturing and testing processes is guaranteed. The wheel-shaped loading reversing structure is used for converting the pushing force of the probe into the pulling force of the film sample. Applying a load force to the on-chip testing machine by using a probe station until a thin film sample in the on-chip testing machine is broken, and recording the reading of a deformation quantity scale in the on-chip testing machine; and calculating biaxial uniformly-distributed tensile force load borne by the film sample when the film sample is broken according to the reading of the deformation quantity scale, and then obtaining the internal biaxial stress when the film sample is broken by using finite element simulation tools such as ANSYS and the like. The invention also provides a manufacturing method of the system, which is characterized in that one-time film deposition and photoetching are added on the basis of the standard bonding deep etching release process to realize the manufacturing of the structure of the on-chip testing machine, and the manufactured on-chip testing machine is assembled with the probe table manufactured by the prior art for use, so that the system can be obtained. Compared with the existing biaxial tensile test method and system, the method has the following advantages: 1) the biaxial tension test can be carried out on the nanoscale film sample; 2) the method is simple and does not need to use large-scale precise instruments; 3) the process quality monitoring can be carried out on the film preparation process.
Drawings
FIG. 1 is a schematic structural diagram of an on-chip testing machine according to an embodiment of the present invention.
In the figure: 101-probe loading structure, 102-wheel loading reversing structure, 1021-wheel structure, 1022-spoke beam, 103-first anchor point, 104-movable frame, 1041-front arm beam, 1042-rear arm beam, 1043-shoulder beam, 105-suspension folding beam, 106-second anchor point, 107-elastic beam, 108-stretching beam, 1081-vertical beam, 1082-cross beam, 109-deformation variable scale, 110-pointer, 111-third anchor point, 201, 202-probe station probe, 300-thin film sample.
FIG. 2 is a side view of an on-chip testing machine in an embodiment of the present invention.
FIG. 3 is a schematic view showing the displacement of each part of the on-chip testing machine in the embodiment of the present invention when the biaxial tension test of the film is performed.
FIGS. 4A-4F are flow charts of the manufacture of an on-chip tester in an embodiment of the present invention.
In the figure: 1 silicon chip, 2 anchor points, 3 thin film samples, 4 glass chips, 5 anti-footing electrodes and 6 movable structures.
Detailed Description
In order to make the technical solution of the present invention more comprehensible, embodiments accompanied with figures are described in detail below.
The embodiment discloses a system for biaxial tensile testing of a nanoscale film, which comprises an on-chip testing machine and a probe station for applying a load force to the on-chip testing machine, wherein the on-chip testing machine comprises two tensile structures which are vertically arranged, the two tensile structures are identical and only have different directions, and the two tensile structures are shown in fig. 1 and fig. 2. In the following, mainly one of the stretching structures will be described, and only one of the structures is labeled for the same two specific structures in one stretching structure. As shown in fig. 1, each stretching structure includes a probe loading structure 101, two wheel loading reversing structures 102, a movable frame 104, an elastic beam 107, a stretching beam 108, two deformation scales 109, two pointers 110, and two hanging folding beams 105.
The probe loading structure 101 is used for bearing the loading of the probe 201 of the probe station, and the probe loading structure 101 is provided with a V-shaped loading port, so that the accuracy of a loading position and the direction of a loading force can be ensured. The two wheel-shaped loading reversing structures 102 are located on two symmetrical sides of the probe loading structure 101, and each wheel-shaped loading reversing structure 102 includes a wheel-shaped structure 1021 and a plurality of spoke beams 1022, opposite sides of the two wheel-shaped structure 1021 are connected to the probe loading structure 101, opposite sides of the two wheel-shaped structure 1021 are connected to two forearm beams 1041 of the movable frame 104, the spoke beams 1022 connect the wheel-shaped structure 1021 to a first anchor point 103 (diamond-shaped cross-section anchor point) of the wheel-shaped axis, and the spoke beams 1022 are circumferentially and uniformly distributed around the first anchor point 103. The movable frame 104 includes two front arm beams 1041 extending in the direction of the two wheel-shaped loading reversing structure 102 and two rear arm beams 1042 departing from the direction, the distance between the two rear arm beams 1042 is narrower than the distance between the two front arms, the front arm beam 1041 and the rear arm beam 1042 at each side are connected and fixed through a shoulder beam 1043 perpendicular to the front arm beams, the two front arm beams 1041 and the two rear arm beams 1042 are respectively distributed symmetrically, and the two deformation scales 108 are engraved on the inner sides of the rear ends of the two rear arm beams 1042. One end of each of the two hanging folding beams 105 is connected to the shoulder beam 1043, and the other end is fixed to each of the two second anchor points 106 (square cross-section anchor points). The elastic beam 107 vertically connects the two rear arm beams 1042 of the movable frame, and has a certain elasticity. The stretching beam 108 includes a vertical beam 1081 and a cross beam 1082, the vertical beam 1081 is disposed in parallel in the middle of the two rear arm beams 1042 of the movable frame 104, one end of which is connected to the middle of the elastic beam 107, and the other end of which is connected to one side of a square film sample 300; the middle of the cross beam 1082 is connected to the vertical beam 1081, and the two hands 110 are disposed at two ends thereof. The two pointers 110 are used for marking the scales of the two deformation variable scales 109, respectively. Two adjacent sides of the film sample 300, which are not connected by the two stretching beams 108 of the stretching structure, are fixedly connected to two third anchor points 110 (rectangular cross-section anchor points), respectively. The four vertices of the square of the film sample 300 all contain the same triangular notches, which shape design allows the inner test area to be under uniform stress with a higher stress level. The thickness of the film sample 300 is on the order of nanometers and the length and width are on the order of micrometers.
The arrows in FIG. 3 show the directions of displacement of the respective parts of the on-chip tester during the biaxial tensile test of the film, and one of the tensile structures is exemplified. When the probe 201 is applied, the probe loading structure 101 is forced to move upward, the left wheel loading reversing structure 102 rotates counterclockwise, the right wheel loading reversing structure rotates clockwise, the moving direction is changed, so that the movable frame 104 moves downward, and further the elastic beam 107 moves downward, and the stretching beam 108 is driven by the elastic beam 107 to stretch the lower edge of the film sample 300. During the stretching process, the stretching beam 108 and the rear arm beam 1042 displace differently, so that relative displacement is generated, that is, the position indicated by the pointer 110 on the deformation scale 109 changes due to the relative displacement, and the reading of the deformation scale can reflect the magnitude of the stretching force applied to the film sample. The greater the tension, the greater the relative displacement, and the greater the scale indicated by the pointer 110. By applying a load thrust to the biaxial stretching structure, the readings of the two deformation scaleplates at the time of the fracture of the film sample are recorded, and after the test data are processed, the stress data of the film sample 300 at the time of the fracture of the two axes can be measured.
The manufacturing flow of the on-chip tester of the system is shown in fig. 4A-4F, and the adopted process is based on a bonding deep etching release standard process and mainly comprises the following steps:
(1) as shown in fig. 4A, the silicon wafer 1 is an N-type monocrystalline silicon wafer with a thickness of 400 μm and a resistivity of 0.001-0.003 Ω · cm, the silicon wafer 1 is etched by using ASE dry method to form steps, and all anchor points 2 including a first anchor point, a second anchor point and a third anchor point are formed;
(2) as shown in fig. 4B, Al is sputtered,
when Al is deeply etched, the selection ratio of Al to silicon is high enough, Al is corroded by a wet method, and an Al film sample 3 is formed;
(3) as shown in fig. 4C, B33 with a thickness of 500 μm was selected as the glass sheet 4, BHF wet-etched the glass sheet 4,
sputtering Ti/Pt/Au to form a sputtering target,
stripping to form a Footing-preventing electrode 5 which has the function of avoiding the occurrence of a Footing effect during final etching and ensuring the etching quality;
(4) as shown in fig. 4D, the silicon wafer 1 and the glass plate 4 are anodically bonded;
(5) thinning the silicon chip 5 by KOH wet etching, wherein the residual thickness is 60 +/-5 mu m;
(6) as shown in fig. 4F, the silicon wafer 5 was deep etched by ASE dry method, and the movable structure and the thin film sample were released, to obtain the entire on-chip tester structure.
The testing machine on the chip manufactured as above was tested by a probe station. As shown in fig. 1, a probe station probe 201 and a probe 202 are used for applying a load thrust at a V-shaped loading port of a probe loading structure 101 of two stretching structures, a wheel-shaped loading reversing structure is pushed to rotate (see fig. 3), so that the thrust is converted into a stretching force to pull a film sample until the film sample is observed to break through an optical microscope, and the reading d of a deformation variable scale 109 of the two stretching structures is recorded1And d2. Then, carrying out static simulation by using an ANSYS finite element simulation tool to obtain the internal biaxial stress of the film sample when the film sample is broken, wherein two ends of the film sample are connected with the rectangular section anchor points, so that zero displacement constraint is exerted, and biaxial uniformly distributed tensile force loads q borne by the other two ends of the film sample are1And q is2Can be calculated using equations (1) and (2):
wherein E is the Young's modulus of the single crystal silicon, l is the half length of the elastic beam, w is the width of the elastic beam, t is the thickness of the elastic beam, and A is the cross-sectional area of the thin film sample.
The process is repeated for many times, and different load thrust forces are applied to the V-shaped loading ports of the probe loading structures 101 of the two stretching structures, so that the biaxial stress of the film sample when the film sample is broken under different biaxial stretching force combinations can be obtained.
One application of the method of the invention has been described above by way of an example, namely the extraction of a thickness of
The internal biaxial stress of the aluminum thin film prepared by the sputtering method at the time of fracture was utilized. It should be noted that, however,the method is suitable for extracting the biaxial stress when the nano-scale film manufactured by other processing techniques is broken. It will be understood by those skilled in the art that variations and modifications can be made to the structure without departing from the spirit of the invention, and the manufacturing method is not limited to the manufacturing process of the present embodiment, except that the feature of the invention is combined with the probe station for microelectronic process inspection and analysis by using the on-chip tester. The protection scope of the present invention shall be subject to the claims.
Claims (10)
1. A system for biaxial tensile test of a nanoscale film comprises an on-chip testing machine and a probe station for applying a load force to the on-chip testing machine, and is characterized in that the on-chip testing machine comprises two tensile structures which are vertically arranged; each stretching structure comprises a probe loading structure, a two-wheel loading reversing structure, a movable frame, an elastic beam, a stretching beam, two deformation variable scaleplates, two pointers and two hanging folding beams; the probe loading structure is used for bearing the probe loading of the probe station; the two wheel-shaped loading reversing structures are positioned on two symmetrical sides of the probe loading structure and respectively comprise a wheel-shaped structure and a plurality of spoke beams, two opposite sides of the two wheel-shaped structure are connected to the probe loading structure, the two opposite sides of the two wheel-shaped structure are connected to two front arm beams of the movable frame, and the spoke beams connect the wheel-shaped structure to a first anchor point of a wheel-shaped axis; the movable frame comprises two front arm beams extending towards the direction of the two-wheel-shaped loading reversing structure and two rear arm beams deviating from the direction, the rear ends of the two front arm beams and the front ends of the two rear arm beams are fixed with each other, the two front arm beams and the two rear arm beams are respectively and symmetrically distributed, and the inner sides of the rear ends of the two rear arm beams are provided with the two deformation scaleplates; one end of each of the two hanging folding beams is connected to two sides of the movable frame, and the other end of each of the two hanging folding beams is fixed to the two second anchor points; the elastic beam is vertically connected with the two rear arm beams of the movable frame; the stretching beam comprises a vertical beam and a cross beam, the vertical beam is arranged in the middle of the two rear arm beams of the movable frame in parallel, one end of the vertical beam is connected to the middle of the elastic beam, and the other end of the vertical beam is connected with one edge of a square film sample; the middle part of the cross beam is vertically connected to the vertical beam, and two ends of the cross beam are provided with the two pointers; the two pointers are respectively used for marking the scales of the two deformation variable scaleplates; and two adjacent edges of the film sample which are not connected by the stretching beams of the two stretching structures are respectively and fixedly connected with the two third anchor points.
2. The system of claim 1, wherein the probe loading structure has a V-shaped loading port.
3. The system of claim 1, wherein the distance between the rear arm beams of the movable frame is narrower than the distance between the front arms, the front arm beam and the rear arm beam on each side being connected by a shoulder beam perpendicular thereto, the suspension folding beam being connected at one end thereof to the shoulder beam.
4. The system of claim 1, wherein the spoke beams of the wheel load reversing structure are evenly distributed circumferentially about the first anchor point.
5. The system of claim 1, wherein adjacent ones of the hanging folded beams of the two tensile structures are connected to a common second anchor point.
6. The system of claim 1, wherein the first anchor point is a diamond or circular cross-section anchor point, the second anchor point is a square cross-section anchor point, and the third anchor point is a rectangular cross-section anchor point.
7. The system of claim 1, wherein the four vertices of the square of the film sample each comprise the same triangular notch, the shape of the square being designed to provide a uniform stress profile and a higher stress level in the inner test area.
8. A method of manufacturing a system for biaxial tensile testing of nano-scale thin films, comprising manufacturing a probe station and the on-chip testing machine of any of claims 1-7, wherein the step of manufacturing the on-chip testing machine comprises:
(1) forming bonding anchor points on the front surface of the silicon wafer by photoetching and etching, wherein the anchor points comprise a first anchor point, a second anchor point and a third anchor point;
(2) depositing a film material on the front surface of the silicon wafer, and forming a film sample pattern by utilizing photoetching, corrosion or etching according to the plane shape and the size of the film sample;
(3) forming shallow grooves on a glass sheet by photoetching and wet etching, sputtering metal on the glass sheet, and forming a metal electrode for preventing sputtering by using a stripping process;
(4) carrying out anodic bonding on the silicon wafer and the glass sheet which are treated by the steps;
(5) using wet etching to thin the silicon chip to the designed thickness;
(6) the silicon wafer is partially etched through from the back side by photolithography and deep etching to release the movable structures, i.e., all the silicon structures except the anchor points, and the on-chip tester is obtained.
9. The method of claim 8, wherein the silicon wafer is an N-type single crystal silicon wafer having a resistivity of 0.001 to 0.003 Ω -cm; three metals of Ti, Pt and Au are sputtered on the glass sheet.
10. The method of claim 8, wherein the silicon is dry etched using ASE to form bond anchors; and depositing a thin film material on the front side of the silicon wafer by using a PVD, CVD, ALD or electroplating method.
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