CN210534032U - Chip for testing in-situ mechanical property of electron microscope - Google Patents
Chip for testing in-situ mechanical property of electron microscope Download PDFInfo
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- CN210534032U CN210534032U CN201920925743.8U CN201920925743U CN210534032U CN 210534032 U CN210534032 U CN 210534032U CN 201920925743 U CN201920925743 U CN 201920925743U CN 210534032 U CN210534032 U CN 210534032U
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Abstract
The utility model relates to an electron microscope normal position mechanical properties test field especially relates to an electron microscope normal position mechanical properties test chip. The chip is formed on a monocrystalline silicon wafer in two parts: one part is a fixed end and is fixed on the electron microscope sample rod or the bracket through a fixing piece mounting hole; the other part is a moving end which is connected with a component for applying force through a connecting piece of the force applying end; the fixed end and the moving end are buckled together through the concave/convex parts which are matched with each other, so that the sample load is applied. Depositing silicon nitride on two sides of the double-polished monocrystalline silicon wafer, depositing a platinum electrode on one side by using an ultraviolet lithography technology, and then performing deep silicon etching; and performing plasma etching on the other side, etching the silicon nitride to form a required pattern, etching the silicon by using wet etching, depositing a passivation layer, obtaining an electron microscope in-situ mechanical property testing chip for applying load and heating, and performing microstructure evolution analysis on the sample.
Description
Technical Field
The utility model relates to an electron microscope normal position mechanical properties test field especially relates to an electron microscope normal position mechanical properties test chip that can realize applying load and heating.
Background
The mechanical property of the material is always one of the most important properties of the traditional structural material, the traditional method for representing the mechanical property of the material can only provide the criterion of the good and bad mechanical property of the material and cannot provide the deformation mechanism of the material, and the study on the deformation mechanism of the material needs to carry out detailed analysis on the microstructure of the material before and after deformation. However, the method only depends on the comparison of the microstructures before and after the material deformation, that is, only the microstructures in the initial state and the deformation state are known, and the deformation process is not known, so that the obtained deformation mechanism is inaccurate, and the in-situ observation of the deformation process of the material is very important.
In recent years, electron microscope in-situ application based on MEMS technology has attracted wide attention of researchers. The development of the in-situ technology realizes real-time and dynamic recording of the change process of the sample under different environments and conditions under an electron microscope, and expands the research of experiments in the fields of battery, catalysis, irradiation, corrosion, mechanical property test and the like.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing an electron microscope normal position mechanical properties test chip capable of realizing load application and heating, which adopts a monocrystalline silicon piece as a raw material, can realize load application and heating on a sample simultaneously, and can observe the microstructure evolution of the sample under the conditions of stress and heating simultaneously; and the load and displacement of the sample in the stretching process can be obtained, and the strain is calculated to obtain the yield strength of the sample.
In order to achieve the above purpose, the technical solution of the present invention is as follows:
an electron microscope in-situ mechanical property test chip, which forms two parts on a monocrystalline silicon piece: one part is a fixed end and is fixed on the electron microscope sample rod or the bracket through a fixing piece mounting hole; the other part is a moving end which is connected with a component for applying force through a connecting piece of the force applying end; the fixed end and the moving end are buckled together through the concave/convex parts which are matched with each other, so that the sample load is applied.
Electron microscope normal position mechanical properties test chip, the stiff end includes: the device comprises a platinum electrode for heating a sample by utilizing a joule heat effect, a supporting beam for ensuring uniaxial tension of the sample, a force sensor beam for reading a mark of sample displacement and calculating stress strain, a sample table and an electrode block, and has the following specific structures: the single crystal silicon wafer is oppositely provided with sample tables, each sample table is provided with a platinum electrode, each platinum electrode is connected with an electrode block through a circuit, the two oppositely arranged platinum electrodes are provided with samples, the side surfaces of the two ends of each sample are respectively and correspondingly provided with a first displacement mark and a second displacement mark, and the outer side of each supporting beam is provided with a moving end connecting piece.
The electron microscope in-situ mechanical property testing chip is characterized in that 2-8 groups of supporting beams are arranged at the fixed end in order to guarantee uniaxial stress of a sample during testing.
In the electron microscope in-situ mechanical property testing chip, the fixed end is provided with the force sensor beam, the chip can deform after a load is applied to a sample, and the sample is transmitted to the force sensor beam to deform the force sensor beam; the force F acting on the sample is equal to the spring constant of the force sensor beam multiplied by its deflection d, which is observed by a low power electron microscope.
The chip for testing the in-situ mechanical property of the electron microscope is characterized in that a first displacement mark and a second displacement mark are arranged at two ends of a sample, the displacements at two ends of the sample are read, the difference between the first displacement mark and the second displacement mark is the deformation of the sample, and the displacements at two ends of the sample are obtained by observing through a low-power electron microscope.
After the fixed end and the moving end of the electron microscope in-situ mechanical property testing chip are buckled, a gap exists between the fixed end and the moving end.
The utility model relates to a thinking as follows:
aiming at analyzing a chip for testing the in-situ mechanical properties of an electron microscope on a sample, which is provided by the existing literature, the existing chip can only apply load or heat, and the composition of the chip which can apply the load and heat is too complex, so that the success rate of the experiment is difficult to ensure. Therefore, the utility model discloses hope to design and make a preparation simple process and can realize exerting the electronic speculum normal position mechanical properties test chip of load and heating to the sample simultaneously. The utility model discloses a methods such as dark silicon etching, reactive ion etching, wet etching utilize ultraviolet lithography technique, chemical vapor deposition technique and physics vapor deposition technique etc. to realize applying the normal position electron microscope mechanical properties test chip of load and heating to can obtain the load and the displacement of sample in tensile process, calculate and meet an emergency, obtain the yield strength of sample. The chip can be matched with focused ion beams and femtosecond laser cutting processing technologies to realize the transfer of a sample to be detected.
The utility model has the advantages and beneficial effects as follows:
1. the utility model discloses utilize ultraviolet lithography technique and physical vapor deposition technique deposit one deck thickness at 50 ~ 200 nm's platinum electrode on the chip, utilize joule heating effect to heat up for the sample to realize normal position electron microscope observation under the heating condition.
2. The utility model discloses on double-sided polishing monocrystalline silicon piece, utilize low pressure chemical vapor deposition technique (LPCVD) or plasma enhanced chemical vapor deposition technique (PECVD) deposit one deck thickness 500nm ~ 2 mu m's silicon nitride film, silicon nitride is a heat capacity little, and the material that the thermal resistance is big can reduce the heat and scatter and disappear, guarantees the sample temperature rise.
3. The utility model discloses the stiff end sets up the force sensor roof beam, exerts the load back to the sample, and the chip can take place to warp, transmits the force sensor roof beam through sample itself on, makes the force sensor roof beam take place to warp. The force (F) acting on the sample is equal to the spring constant of the beam multiplied by its deflection (d). The displacement marks at the two ends of the sample are used for reading the displacement at the two ends of the sample, and the difference between the two displacement marks is the elongation of the sample. And the deformation of the force sensor beam and the displacement of the two ends of the sample are obtained by observing through a low-power electron microscope, and further the strain and the yield strength of the sample are calculated.
4. The utility model discloses utilize physical vapor deposition technique deposit one deck thickness 50 ~ 300 nm's passivation layer film on platinum electrode, prevent sample and platinum electrode direct contact and cause the short circuit.
5. The utility model discloses the chip can cooperate focus ion beam, femto second laser cutting processing technique, realizes the transfer of the sample that awaits measuring.
6. The utility model discloses the preparation process of chip is ripe simple, mainly includes ultraviolet lithography technique, vacuum coating technique, dark silicon etching technique, reaction ion etching technique and wet etching technique etc..
Drawings
Fig. 1 is a flow chart of the manufacturing process of the in-situ stretching chip of the present invention.
Fig. 2a is a perspective view of the fixed end of the in-situ stretching chip manufactured by the present invention.
FIG. 2b is an enlarged view of the support beam portion L of FIG. 2 a.
Fig. 2c is an enlarged view of the platinum electrode portion of fig. 2a at M.
Fig. 2d is an enlarged view of the beam portion of the force sensor of fig. 2a at N.
Fig. 3 is a perspective view of the motion end of the in-situ stretching chip manufactured by the present invention.
In the figure, 1 a support beam; 101, supporting a beam I; 102 a second support beam; 103, supporting a beam III; 104 supporting the beam IV; 105 supporting the beam five; 106 supporting beams six; 2, marking a first displacement; 3 a platinum electrode; 4 a force sensor beam; 5, a second displacement mark; 6, a sample stage; 7, a monocrystalline silicon wafer; 8, fixing the end; 9 and a moving end connecting piece; 10 electrode blocks; 11 a fixing piece mounting hole; 12 a motion end; 13 connecting piece with fixed end; 14 to the force application end.
Detailed Description
In the specific implementation process, the utility model provides a pair of can realize applying load and the electron microscope normal position mechanical properties test chip of heating and manufacturing method thereof, mainly to the design of chip and the manufacturing method of chip. Depositing silicon nitride on two sides of the double-polished silicon wafer, depositing a platinum electrode on one side by utilizing an ultraviolet lithography technology and a physical vapor deposition technology, and then carrying out deep silicon etching; and performing plasma etching on the other side, etching the silicon nitride into a required pattern, etching the silicon by using wet etching until the silicon wafers subjected to wet etching and deep silicon etching on the two sides are contacted, and depositing a passivation layer by using a metal mask plate to prevent a platinum electrode from being contacted with the metal, thereby realizing heating and stress application and performing microstructure evolution analysis on a sample to be detected. The uniaxial stress of the sample to be measured is ensured in the stretching process, and the strain and the yield strength of the sample in the deformation process can be calculated. The chip can be matched with focused ion beams and femtosecond laser cutting processing technologies to realize the transfer of the to-be-detected product.
In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the drawings in the embodiments of the present invention are combined below to clearly and completely describe the technical solution in the embodiments of the present invention. It is to be understood that the embodiments described are only some of the embodiments of the present invention, and not all of them. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work all belong to the protection scope of the present invention.
Example 1
Referring to fig. 2a to 2d and fig. 3, in this embodiment, the chip for testing the in-situ mechanical properties of the electron microscope is divided into two parts formed on the monocrystalline silicon wafer 7: one part is a fixed end 8 (fig. 2 a-2 d), which is fixed on the electron microscope sample rod or the bracket through a fixing piece mounting hole 11 by a screw, a positioning pin and the like; the other part is a moving end 12 (figure 3), the moving end 12 is connected with a component for applying force through a force applying end connecting piece 14; the fixed end 8 and the moving end 12 are buckled together through the concave/convex parts (the moving end connecting piece 9 and the fixed end connecting piece 13) which are matched with each other, so that the sample load is applied.
Wherein, the fixed end 8 includes: the device comprises a platinum electrode 3 for heating a sample by utilizing a joule heat effect, a supporting beam 1 for ensuring uniaxial tension of the sample, marks (a displacement mark I2 and a displacement mark II 5) for reading displacement of the sample, a force sensor beam 4 for calculating stress strain, a sample table 6, an electrode block 10 and the like, and has the following specific structures:
the testing device comprises a monocrystalline silicon wafer 7, sample tables 6 are oppositely arranged on the monocrystalline silicon wafer 7, a platinum electrode 3 is arranged on each sample table 6, each platinum electrode 3 is connected with an electrode block 10 through a circuit, samples are arranged on two platinum electrodes 3 which are oppositely arranged, a first displacement mark 2 and a second displacement mark 5 are correspondingly arranged on the side faces of the two ends of each sample respectively, a connecting piece 9 is arranged on the outer side of a supporting beam 1 and is used for ensuring the uniaxial stress of the samples during testing, the platinum electrodes 3 are used for heating the samples through the joule heat effect, and the electrode blocks 10 are used for electrifying the platinum electrodes. The heating range of the electron microscope in-situ tensile chip is from room temperature to 800 ℃, and the range of the applied load is from 0 to 1 Newton.
Referring to fig. 1, fig. 2a to fig. 2d, the chip for testing in-situ mechanical properties of an electron microscope capable of applying a load and heating can be realized, and the steps of manufacturing the fixing section are as follows:
(S1) selecting a double-sided polished monocrystalline silicon wafer 7 with the thickness of 300 microns, and depositing a silicon nitride film with the thickness of about 1 micron on two sides of the monocrystalline silicon wafer 7 by using a Plasma Enhanced Chemical Vapor Deposition (PECVD) method;
(S2) spin-coating a photoresist on one side of the monocrystalline silicon wafer 7, and performing ultraviolet exposure and development by using a mask plate; then, a 100nm thick platinum electrode is deposited by electron beam evaporation, and then the photoresist is removed (see fig. 2 b);
(S3) spin-coating a layer of photoresist on one side of the deposited platinum electrode, and carrying out ultraviolet exposure and development to obtain an etched pattern of the support beam, the force sensor beam, the displacement mark and the sample stage;
(S4) performing deep silicon etching to the side of the single crystal silicon wafer 7 having the photoresist to an etching depth of 50 μm, and then removing the photoresist. Thus, the required supporting beam, the force sensor beam, the displacement mark and the etched pattern of the sample stage are repeatedly etched to one side of the monocrystalline silicon wafer 7;
(S5) spin-coating photoresist on the other side of the monocrystalline silicon piece 7, carrying out ultraviolet exposure and development by using a required pattern, etching a certain pattern on the silicon nitride on the side with the photoresist by using reactive ion etching, and then removing the photoresist;
(S6) adopting a mixed aqueous solution of 30 mass percent of KOH and 8 mass percent of isopropanol as an erosion liquid, wherein the etching temperature is 80 ℃; and etching the monocrystalline silicon wafer 7 by using wet etching until the support beam, the force sensor beam, the displacement mark and the sample platform of the deep silicon etching are exposed.
(S7) depositing a passivation layer of 150nm, which may be silicon nitride, aluminum oxide, etc., on the platinum electrode side by a magnetron sputtering technique using a metal mask.
When the device is used, a platinum electrode 3 with the thickness of 100nm is deposited on a chip by utilizing an ultraviolet lithography technology, and the temperature of a sample is raised by utilizing the joule heat effect, so that the in-situ transmission electron microscope observation of the sample under the heating condition is realized. In order to ensure the uniaxial stress of the sample during the test, 6 groups of supporting beams 1 are arranged at the fixed end of the chip (6 groups of supporting beams 1 are a supporting beam I101, a supporting beam II 102, a supporting beam III 103, a supporting beam IV 104, a supporting beam V105 and a supporting beam VI 106 which are sequentially arranged in parallel). And, set up force sensor roof beam 4 at stiff end 8, exert load to the sample after, the chip can take place to warp, and load is transmitted to force sensor roof beam 4 through the sample itself, causes the deformation of force sensor roof beam 4. The force F acting on the sample is equal to the spring constant of the beam multiplied by its deformation d, which can be observed by a low power electron microscope. The marks (the first displacement mark 2 and the second displacement mark 5) at the two ends of the sample are used for reading the displacement of the two ends of the sample, the difference between the two displacement marks is the deformation of the sample, and the deflection of the force sensor beam 4 and the displacement of the two ends of the sample can be obtained by observing through a low power electron microscope. After the fixed end 8 is snapped into place with the moving end 12, a gap is created that prevents any pre-stressing of the sample during any handling prior to loading or testing, and avoids additional strain. The utility model discloses the micro-structure evolution that can realize the tensile chip of electronic speculum normal position of loading and heating at the deformation process of research material to the film sample simultaneously of preparation has wide application prospect.
The embodiment result shows that the utility model discloses a method can obtain the electron microscope normal position mechanical properties test chip that can realize exerting load and heating.
It is right above that the utility model provides a can realize that an electron microscope normal position mechanical properties tests chip and manufacturing method do the detailed introduction. The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the methods and core concepts of the present invention. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, the present invention can be further modified and modified, and such modifications and modifications also fall within the protection scope of the appended claims.
Claims (6)
1. The in-situ mechanical performance testing chip of the electron microscope is characterized in that the chip forms two parts on a monocrystalline silicon piece: one part is a fixed end and is fixed on the electron microscope sample rod or the bracket through a fixing piece mounting hole; the other part is a moving end which is connected with a component for applying force through a connecting piece of the force applying end; the fixed end and the moving end are buckled together through the concave/convex parts which are matched with each other, so that the sample load is applied.
2. The electron microscope in-situ mechanical property testing chip of claim 1, wherein the fixing end comprises: the device comprises a platinum electrode for heating a sample by utilizing a joule heat effect, a supporting beam for ensuring uniaxial tension of the sample, a force sensor beam for reading a mark of sample displacement and calculating stress strain, a sample table and an electrode block, and has the following specific structures: the single crystal silicon wafer is oppositely provided with sample tables, each sample table is provided with a platinum electrode, each platinum electrode is connected with an electrode block through a circuit, the two oppositely arranged platinum electrodes are provided with samples, the side surfaces of the two ends of each sample are respectively and correspondingly provided with a first displacement mark and a second displacement mark, and the outer side of each supporting beam is provided with a moving end connecting piece.
3. The electron microscope in-situ mechanical property test chip as claimed in claim 2, wherein 2-8 groups of support beams are arranged at the fixed end in order to ensure the uniaxial stress of the sample during the test.
4. The electron microscope in-situ mechanical property test chip as claimed in claim 2, wherein the fixed end is provided with a force sensor beam, and after a load is applied to a sample, the chip is deformed and is transmitted to the force sensor beam through the sample to deform the force sensor beam; the force F acting on the sample is equal to the spring constant of the force sensor beam multiplied by its deflection d, which is observed by a low power electron microscope.
5. The electron microscope in-situ mechanical property test chip as claimed in claim 2, wherein the displacement marks one and two ends of the sample are respectively the displacement of the two ends of the sample, the difference between the two displacement marks is the deformation of the sample, and the displacement of the two ends of the sample is obtained by low power electron microscope observation.
6. The electron microscope in-situ mechanical property testing chip of claim 1, wherein a gap exists between the fixed end and the moving end after the fixed end and the moving end are buckled.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112834539A (en) * | 2020-12-31 | 2021-05-25 | 厦门超新芯科技有限公司 | Transmission electron microscope power electric heating in-situ sample rod |
| CN113237734A (en) * | 2021-05-14 | 2021-08-10 | 东南大学 | High-precision in-situ mechanical test chip and preparation method thereof |
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2019
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112834539A (en) * | 2020-12-31 | 2021-05-25 | 厦门超新芯科技有限公司 | Transmission electron microscope power electric heating in-situ sample rod |
| CN113237734A (en) * | 2021-05-14 | 2021-08-10 | 东南大学 | High-precision in-situ mechanical test chip and preparation method thereof |
| CN113237734B (en) * | 2021-05-14 | 2022-03-01 | 东南大学 | High-precision in-situ mechanical test chip and preparation method thereof |
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