CN114264678A - In-situ transmission electron microscope heating chip and preparation method thereof - Google Patents
In-situ transmission electron microscope heating chip and preparation method thereof Download PDFInfo
- Publication number
- CN114264678A CN114264678A CN202111656100.6A CN202111656100A CN114264678A CN 114264678 A CN114264678 A CN 114264678A CN 202111656100 A CN202111656100 A CN 202111656100A CN 114264678 A CN114264678 A CN 114264678A
- Authority
- CN
- China
- Prior art keywords
- heating
- layer
- resistor
- wafer
- electron microscope
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000010438 heat treatment Methods 0.000 title claims abstract description 136
- 230000005540 biological transmission Effects 0.000 title claims abstract description 56
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000010409 thin film Substances 0.000 claims abstract description 32
- 238000009413 insulation Methods 0.000 claims abstract description 31
- 239000000758 substrate Substances 0.000 claims abstract description 22
- 229910052751 metal Inorganic materials 0.000 claims description 50
- 239000002184 metal Substances 0.000 claims description 50
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 13
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical group N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000010408 film Substances 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 6
- 238000004518 low pressure chemical vapour deposition Methods 0.000 claims description 6
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 claims description 4
- 238000001020 plasma etching Methods 0.000 claims description 3
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 238000003384 imaging method Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 238000011109 contamination Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000012613 in situ experiment Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Images
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides an in-situ transmission electron microscope heating chip and a preparation method thereof, wherein the in-situ transmission electron microscope heating chip comprises: the middle part of the substrate is provided with a through hole, and the periphery of the substrate is provided with a plurality of positioning holes; the thin film insulating layer is provided with a heat insulation groove corresponding to the periphery of the through hole; and the heating resistance layer is arranged on the top of the thin film insulation layer and is wound at the edge of the through hole. According to the in-situ transmission electron microscope heating chip and the preparation method thereof, the through holes are formed, so that the heating volume of the heating resistor layer is reduced, the heating power of the in-situ transmission electron microscope heating chip is reduced, the thermal drift generated by the chip in the heating process is reduced, and the transmission electron microscope imaging is more stable and clear; the ultra-large field range is used for experimental observation, and sample preparation is simpler and more convenient; the heat insulation groove effectively restricts the temperature diffusion of the heating resistor layer, so that the temperature is concentrated as much as possible, and the heat influence of the heating resistor layer on external electron microscope accessories in the heating process is reduced.
Description
Technical Field
The invention relates to the technical field of heating chips, in particular to an in-situ transmission electron microscope heating chip and a preparation method thereof.
Background
At present, with the progress of electron microscopy, micro-nano processing and other technologies, the in-situ transmission electron microscope technology is developed more maturely. The in-situ transmission electron microscope analysis technology can apply single or coupled external fields of gas state, liquid state environment, irradiation, force, heat, electricity and the like, research the evolution rule of the microstructure of the material under the external field in real time, and establish the correlation relation between the microstructure and the physical and chemical properties thereof.
The application of a uniform thermal field in the transmission electron microscope is realized, and the microstructure evolution law of the atomic layer in-situ characterization material is still a difficult problem in the technical field of in-situ transmission electron microscopes.
In the prior art, different in-situ experiment platforms have been developed, for example, a model 652 type transmission electron microscope double-inclination in-situ heating sample rod developed by Gatan corporation in usa, and a heating crucible made of different materials is designed at the front end of the sample rod, so that a temperature field of up to 1000 ℃ can be applied to a sample; however, because the crucible heating area is large, when a high heating temperature is applied to the sample, the large heating power of the crucible makes the thermal drift of the sample large, and the resolution of experimental observation is directly influenced. In addition, the Wildfire series transmission electron microscope sample rod developed by Dens Solution of the Netherlands can apply a temperature field of up to 1300 ℃ to a sample by using an MEMS chip at the front end of the sample rod. But the observation area is small and the sample preparation process is complicated.
Disclosure of Invention
The invention provides an in-situ transmission electron microscope heating chip and a preparation method thereof, which are used for overcoming the defects of small observation area and complex sample preparation in the prior art, and the in-situ transmission electron microscope heating chip has a simple structure and is convenient to prepare, can be produced in batch by a micro electro mechanical system processing technology, and realizes in-situ observation of transmission samples with larger sizes in an in-situ transmission electron microscope at different temperatures.
The invention provides an in-situ transmission electron microscope heating chip which is arranged on an installation platform, wherein the installation platform is provided with a plurality of screw holes, and the in-situ transmission electron microscope heating chip comprises:
the middle part of the substrate is provided with a through hole, and the periphery of the substrate is provided with positioning holes which are in one-to-one correspondence with the screw holes;
the thin film insulating layer is arranged on the top of the substrate, and a heat insulation groove is formed in the periphery of the thin film insulating layer, corresponding to the through hole;
and the heating resistance layer is arranged on the top of the thin film insulation layer and is wound at the edge of the through hole.
According to the in-situ transmission electron microscope heating chip provided by the invention, the heat insulation groove and the heating resistance layer are arranged in a circular ring shape, the through hole is arranged in a circular shape, and the heat insulation groove, the heating resistance layer and the through hole are arranged concentrically; and the heating resistor layer is positioned between the heat insulation groove and the through hole.
According to the in-situ transmission electron microscope heating chip provided by the invention, the corners of the heating resistance layer adopt obtuse angle or fillet wiring modes.
According to the in-situ transmission electron microscope heating chip provided by the invention, the heating resistor layer is a snakelike metal resistor which is divided into an upper semi-ring metal resistor and a lower semi-ring metal resistor through two horizontal metal wires; the upper half-ring metal resistor and the lower half-ring metal resistor are connected in parallel to a circuit; the horizontal metal wire is connected with an external power supply through a lead and a pressure welding area.
The in-situ transmission electron microscope heating chip further comprises an electrode protection layer, wherein the electrode protection layer is arranged on the top of the heating resistance layer and completely or partially wraps the thin film insulation layer and the heating resistance layer.
According to the in-situ transmission electron microscope heating chip provided by the invention, the heating resistor layer is an equidistant annular heating resistor, and the distance between the rings is equal; the distance between the rings and the distance between the corners of the joints of the rings can be adjusted, so that the temperature field of the heating battery core is more uniform.
According to the in-situ transmission electron microscope heating chip provided by the invention, the heating resistance layer comprises an inner ring circular metal resistor and an outer ring double helix asymptotic annular resistor, the inner ring circular metal resistor is concentric with the through hole and is positioned at the edge of the through hole, and the outer ring double helix asymptotic annular resistor is connected with the inner ring circular metal resistor and is positioned outside the inner ring circular metal resistor; the temperature field of the heating chip is more uniform by adjusting the width of the inner ring circular metal resistor, the width of the outer ring double-helix asymptotic annular resistor and the distance between the outer ring double-helix asymptotic annular resistors.
According to the in-situ transmission electron microscope heating chip provided by the invention, the thin film insulating layer is a silicon nitride layer and/or a silicon oxide layer.
The invention also provides a preparation method of the in-situ transmission electron microscope heating chip, which comprises the following steps:
providing a monocrystalline silicon wafer A and cleaning;
processing thin film insulating layers on two sides of a monocrystalline silicon wafer A to obtain a wafer A-1;
generating a layer of metal film on the surface of the wafer A-1 to form a heating resistor, and obtaining a wafer A-2;
firstly growing a layer of silicon nitride and silicon oxide layer on the surface of the wafer A-2 by adopting an LPCVD (low pressure chemical vapor deposition) or PECVD (plasma enhanced chemical vapor deposition) process, and etching the silicon nitride or the silicon oxide on the to-be-etched area of the wafer A-2 by utilizing a reactive ion etching process to form a heat insulation groove; obtaining a wafer A-3;
exposing and completely etching the substrate silicon of the wafer A-3 to form a central through hole; obtaining a wafer A-4;
and scribing the wafer A-4 to obtain a single independent chip.
According to the preparation method of the in-situ transmission electron microscope heating chip provided by the invention, the monocrystalline silicon wafer A is processed into the thin film insulating layer to obtain the wafer A-1, wherein the thin film insulating layer is a silicon nitride layer and/or a silicon oxide layer, and the thickness of the thin film insulating layer is 10nm-2 mu m.
According to the in-situ transmission electron microscope heating chip and the preparation method thereof, the through hole is formed in the middle of the substrate, so that the heating volume of the heating resistor layer is reduced, the heating power of the in-situ transmission electron microscope heating chip is reduced, the thermal drift generated by the chip in the heating process is reduced, the transmission electron microscope imaging is more stable and clear, an ultra-large field range is provided for experimental observation, and compared with the traditional heating chip, the sample preparation is simpler and more convenient; the micro electro mechanical system processing technology can be used for batch production, and in-situ observation of transmission samples with larger sizes in a transmission electron microscope at different temperatures is realized; the heat insulation grooves arranged on the thin film insulation layer effectively restrain the temperature diffusion of the heating resistance layer, so that the temperature is concentrated as much as possible, and the heat influence of the heating resistance layer on external electron microscope accessories in the heating process is reduced; meanwhile, the positioning holes and the screw holes are arranged, so that the chip can be more accurately fixed on the mounting table, and the pollution caused by adhesion at high temperature can be avoided.
Drawings
In order to more clearly illustrate the technical solutions of the present invention or the prior art, the drawings needed for the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an in-situ TEM heating chip according to embodiment 1 of the present invention;
FIG. 2 is a schematic structural diagram of an in-situ TEM heating chip according to embodiment 2 of the present invention;
FIG. 3 is a schematic structural diagram of an in-situ TEM heating chip according to embodiment 3 of the present invention;
reference numerals:
1: a substrate; 2: a thin film insulating layer; 3: a heating resistor layer; 4: a heat insulation groove; 5: an upper semi-ring metal resistor; 6: a lower semi-ring metal resistor; 7: a horizontal metal wire; 8: a through hole; 9: positioning holes; 10: an inner ring circular metal resistor; 11: the outer ring double helix asymptotes to the annular resistor.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Embodiment 1 of the present invention is described below with reference to fig. 1, and provides an in-situ tem heating chip, which is disposed on a mounting table, the mounting table being provided with a plurality of screw holes, including a substrate 1, a thin-film insulating layer 2 and a heating resistor layer 3, the substrate 1 being provided with a through hole 8 at the center thereof and positioning holes 9 at the periphery thereof, the through holes corresponding to the screw holes one to one; the arrangement of the positioning holes 9 and the screw holes can not only more accurately fix the chip on the mounting table, but also avoid the pollution caused by adhesion at high temperature. The through hole 8 forms an observation area for microscopic in-situ observation; the thin film insulating layer 2 is arranged on the top of the substrate 1, and the periphery of the thin film insulating layer 2 corresponding to the through hole 8 is provided with a heat insulation groove 4; the heating resistor layer 3 is arranged on top of the thin film insulation layer 2, and the heating resistor layer 3 is coiled at the edge of the through hole 8.
The chip provided by the embodiment 1 of the invention has a simple structure and is convenient to prepare, and can be produced in batch by a Micro Electro Mechanical System (MEMS) process, so that in-situ observation of transmission samples with larger sizes in a transmission electron microscope at different temperatures is realized.
Specifically, the substrate 1 is rectangular, the heat insulation groove 4 and the heating resistor layer 3 are annular, the through hole 8 is a circular hole, and the heat insulation groove 4, the heating resistor layer 3 and the through hole 8 are concentrically arranged; and the heating resistor layer 3 is positioned between the heat insulation groove 4 and the through hole 8; each side of the periphery of the rectangular substrate 1 is provided with a positioning hole 9; the thin film insulating layer 2 adopts a silicon nitride layer and/or a silicon oxide layer; the heating resistor layer 3 is annular and is located between the heat insulation groove 4 and the through hole 8. That is, the heating resistor layer 3 is provided on the periphery of the through hole 8; the heat insulation groove 4 is provided in the periphery of the heating resistor layer 3.
The corners of the heating resistor layer are all wired in an obtuse angle or fillet mode, so that the temperature field of the heating chip is more uniform.
Furthermore, the heating resistor layer 3 is set as a snake-shaped metal resistor, the whole heating resistor layer 3 is centrosymmetric and is wound on the edge of the through hole in a circular ring shape, and the distance between the sections of resistance wires on the inner side of the circular ring is smaller than that between the sections of resistance wires on the outer side of the circular ring. The snakelike metal resistor is divided into an upper semi-ring metal resistor 5 and a lower semi-ring metal resistor 6 through two horizontal metal wires 7; the upper semi-ring metal resistor 5 and the lower semi-ring metal resistor 6 are connected in parallel to a circuit; the horizontal metal wire 7 is connected with an external power supply; meanwhile, the corners of the upper half-ring metal resistor 5 and the lower half-ring metal resistor 6 are all wired in an obtuse angle or a fillet mode.
Moreover, the serpentine metal resistor is thin, and the positions of the far-end lead and the pressure welding area are as wide as possible.
In the embodiment, the heating resistance layer 3 winds the snake-shaped metal resistance wire into a circular ring, and is arranged at the edge of the through hole 8 in the center of the substrate, so that the temperature field on the sample can be uniform and stable as far as possible while the sample with the ultra-large transmission is heated, and the higher temperature uniformity of the heating area is effectively ensured.
The annular heat insulation groove 4 arranged on the thin film insulation layer 2 reduces heat conduction paths and heating volume, reduces heating efficiency, and can effectively restrict temperature diffusion, so that temperature is concentrated as much as possible, heat influence of the heating resistor layer 3 on external electron microscope accessories in the heating process is reduced, and the service life of the heating chip is prolonged.
The through hole 8 in the center of the substrate obviously reduces the heating volume of the heating resistor layer 3, reduces the heating power of the heating chip with the ultra-large temperature area for the transmission electron microscope, reduces the thermal drift generated by the chip in the heating process, and enables the transmission electron microscope to be more stable and clear in imaging. Moreover, the through hole 8 meets the requirement of observing the experimental phenomenon in the heating process of the transmission electron microscope sample in situ within the range of the ultra-large visual field area while ensuring that a uniform temperature field is applied to the large-size transmission sample, and the arrangement of the ultra-large visual field range enables the heating chip disclosed by the invention to be simpler and more convenient to prepare compared with the traditional heating chip.
The use method of the embodiment disclosed by the invention comprises the following steps: and the in-situ transmission electron microscope heating chip is fixed on the mounting table at the front end of the transmission electron microscope double-inclined sample rod by using a mechanical connection structure, so that the positioning holes and the screw holes are ensured to be in one-to-one correspondence. And leading the lead wires to the position of the transmission electron microscope sample rod from the tail end of the heating resistor layer 3 by ultrasonic pressure welding. And inserting the transmission electron microscope sample rod into the transmission electron microscope, and adjusting the transmission electron microscope parameters to the optimal observation state. And when the sample is stable, applying a certain current or a certain voltage to the heating resistor according to the experimental requirement. And precisely controlling the temperature field of the sample, and simultaneously observing the microscopic structure evolution of the material and measuring the physical and chemical properties of the material in situ.
The in-situ transmission electron microscope heating chip disclosed by the embodiment is used for a transmission electron microscope in-situ sample rod, and realizes microstructure observation and physical and chemical property research of material atomic scale in an even thermal field of an ultra-large temperature zone to the maximum extent.
In addition, the mode of resistance heating and sample carrying on the silicon oxide or silicon nitride film is adopted, the heating volume is effectively reduced, the thermal response rate is improved, the thermal balance speed is accelerated, meanwhile, the heating power is reduced, and the thermal drift of the sample is reduced.
Meanwhile, the arrangement of the heating area with the ultra-large area in the embodiment of the invention enables the sample preparation of the transmission electron microscope heating sample to be simpler, and the sample preparation by using the focused ion beam technology and the conventional ion thinning sample and the double-spraying thinning sample can also be directly carried on the heating chip with the ultra-large area for the transmission electron microscope for use.
Finally, the invention adopts the axisymmetric design, which can increase the stability of the chip structure and make the temperature distribution and the stress distribution of the chip more reasonable.
In embodiment 3 of the present invention, the temperature field at the position of the transmission electron microscope sample is made as uniform and stable as possible by adjusting the wire widths of the inner ring annular metal resistor and the outer ring double helix asymptotic annular resistor, and the distance between the outer ring double helix asymptotic annular resistor and the helix asymptotic line.
The embodiment of the other aspect of the invention also discloses a preparation method of the in-situ transmission electron microscope heating chip, which comprises the following steps:
s1, providing a monocrystalline silicon wafer A and cleaning to form a substrate 1;
s2, forming thin film insulating layers 2 on two sides of the monocrystalline silicon wafer to obtain a wafer A-1;
s3, forming a metal film on the surface of the wafer A-1 to form a heating resistor layer 3, and obtaining a wafer A-2;
s4, growing a silicon nitride layer and a silicon oxide layer on the surface of the wafer A-2 by adopting an LPCVD (low pressure chemical vapor deposition) or PECVD (plasma enhanced chemical vapor deposition) process, and etching the silicon nitride or the silicon oxide on the to-be-etched area of the wafer A-2 by utilizing a reactive ion etching process to form a heat insulation groove 4; obtaining a wafer A-3;
s5, exposing and completely etching the substrate silicon of the wafer A-3 to form a through hole 5; obtaining a wafer A-4;
and S6, scribing the wafer A-4 to obtain a single independent chip.
Wherein, in step S1, the thickness of the monocrystalline silicon wafer is 50-500 μm; and RCA cleaning is adopted. The RCA standard clean is one of the typical, most commonly used wet chemical cleans. RCA cleaning is to adopt a proper cleaning agent to remove organic stains on the surface of the silicon wafer firstly, because organic matters cover part of the surface of the silicon wafer, so that an oxidation film and stains related to the oxidation film are difficult to remove; the oxide film is then dissolved, since the oxide layer is a "contamination trap", which also introduces epitaxial defects; finally, the contamination of particles, metals and the like is removed, and the surface of the silicon wafer is passivated. Removal of organic and metal ion contaminants from the wafer prior to high temperature processing is ensured by RCA cleaning.
In step S2, the thin film insulation layer 2 is a silicon nitride layer and/or an oxide layer, and the thickness of the thin film insulation layer 2 is 10nm-2 μm.
In step S3, the thickness of the heating resistor layer 3 is 10nm-2 μm, and the material of the heating resistor layer 3 is one or more of platinum, gold, silver, copper, molybdenum, tungsten, aluminum, and chromium, and the heating material is selected to be compatible with the mems process.
It should be noted that the single crystal silicon wafer can also be replaced by SOI, in which a buried oxide layer is introduced between the top silicon and the back substrate, and a semiconductor thin film is formed on the insulator.
The embodiment adopts the manufacturing technology of the semiconductor micro-electro-mechanical system, can realize mass production, and has the same and controllable quality.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The utility model provides an normal position transmission electron microscope heating chip sets up on the mount table, a plurality of screws have been seted up on the mount table, a serial communication port, include:
the middle part of the substrate is provided with a through hole, and the periphery of the substrate is provided with positioning holes which are in one-to-one correspondence with the screw holes;
the thin film insulating layer is arranged on the top of the substrate, and a heat insulation groove is formed in the periphery of the thin film insulating layer, corresponding to the through hole;
and the heating resistance layer is arranged on the top of the thin film insulation layer and is wound at the edge of the through hole.
2. The in-situ TEM heating chip as claimed in claim 1, wherein the heat insulation groove and the heating resistor layer are arranged in a ring shape, the through hole is arranged in a circle shape, and the heat insulation groove, the heating resistor layer and the through hole are arranged concentrically; and the heating resistor layer is positioned between the heat insulation groove and the through hole.
3. The in-situ TEM heating chip as claimed in claim 2, wherein the corners of the heating resistor layer are all routed in obtuse angle or fillet manner.
4. The in-situ TEM heating chip as claimed in claim 2, wherein the heating resistor layer is a serpentine metal resistor, and the serpentine metal resistor is configured to be divided into an upper half-ring metal resistor and a lower half-ring metal resistor by two horizontal metal wires; the upper half-ring metal resistor and the lower half-ring metal resistor are connected in parallel to a circuit; the horizontal metal wire is connected with an external power supply.
5. The in-situ TEM heating chip as claimed in claim 2, further comprising an electrode protection layer disposed on top of the heating resistor layer, wherein the thin film insulation layer and the heating resistor layer are completely or partially wrapped.
6. The in-situ TEM heating chip as claimed in claim 2, wherein the heating resistor layer is an equidistant annular heating resistor, and the distance between the rings is equal; the distance between the rings and the distance between the corners of the joints of the rings can be adjusted, so that the temperature field of the heating battery core is more uniform.
7. The in-situ TEM heating chip as claimed in claim 2, wherein the heating resistor layer comprises an inner ring circular metal resistor and an outer ring double helix asymptotic annular resistor, the inner ring circular metal resistor is concentric with the through hole and is located at the edge of the through hole, and the outer ring double helix asymptotic annular resistor is connected with the inner ring circular metal resistor and is located outside the inner ring circular metal resistor; the width of the inner ring-shaped metal resistor, the width of the outer ring double-helix asymptotic annular resistor and the distance between the outer ring double-helix asymptotic annular resistors can be adjusted, so that the temperature field of the heating chip is more uniform.
8. The in-situ TEM heating chip according to any one of claims 1-7, wherein the thin-film insulating layer is a silicon nitride layer and/or a silicon oxide layer.
9. A preparation method of an in-situ transmission electron microscope heating chip is characterized by comprising the following steps:
providing a monocrystalline silicon wafer A and cleaning;
processing thin film insulating layers on two sides of a monocrystalline silicon wafer A to obtain a wafer A-1;
generating a layer of metal film on the surface of the wafer A-1 to form a heating resistor, and obtaining a wafer A-2;
firstly growing a layer of silicon nitride and silicon oxide layer on the surface of the wafer A-2 by adopting an LPCVD (low pressure chemical vapor deposition) or PECVD (plasma enhanced chemical vapor deposition) process, and etching the silicon nitride or the silicon oxide on the to-be-etched area of the wafer A-2 by utilizing a reactive ion etching process to obtain a wafer A-3;
exposing and completely etching the substrate silicon of the wafer A-3 to form a central through hole; obtaining a wafer A-4;
and scribing the wafer A-4 to obtain a single independent chip.
10. The method for preparing the in-situ heating chip for the transmission electron microscope according to claim 9, wherein the thin film insulating layers are processed on two sides of the monocrystalline silicon wafer A to obtain the wafer A-1, the thin film insulating layers are silicon nitride layers and/or silicon oxide layers, and the thickness of the thin film insulating layers is 10nm-2 μm.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111656100.6A CN114264678A (en) | 2021-12-30 | 2021-12-30 | In-situ transmission electron microscope heating chip and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111656100.6A CN114264678A (en) | 2021-12-30 | 2021-12-30 | In-situ transmission electron microscope heating chip and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN114264678A true CN114264678A (en) | 2022-04-01 |
Family
ID=80831992
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202111656100.6A Pending CN114264678A (en) | 2021-12-30 | 2021-12-30 | In-situ transmission electron microscope heating chip and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN114264678A (en) |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104319220A (en) * | 2014-10-14 | 2015-01-28 | 西安交通大学 | Quantitative nanometer heating table for electron microscope |
CN105136822A (en) * | 2015-08-06 | 2015-12-09 | 南京大学 | Nanometer material transmission electron microscope in-situ testing chip, preparation method and applications thereof |
CN107765037A (en) * | 2017-09-05 | 2018-03-06 | 浙江大学 | High-temp in-situ specimen holder |
CN111312573A (en) * | 2020-03-12 | 2020-06-19 | 厦门超新芯科技有限公司 | Transmission electron microscope high-resolution in-situ liquid phase heating chip and preparation method thereof |
CN111370280A (en) * | 2020-03-12 | 2020-07-03 | 厦门超新芯科技有限公司 | Transmission electron microscope high-resolution in-situ gas phase heating chip and preparation method thereof |
CN112129786A (en) * | 2020-10-20 | 2020-12-25 | 厦门大学 | Transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip and preparation method thereof |
WO2021179541A1 (en) * | 2020-03-12 | 2021-09-16 | 厦门超新芯科技有限公司 | Transmission electron microscope in-situ chip and preparation method therefor |
CN217688648U (en) * | 2021-12-30 | 2022-10-28 | 北京工业大学 | In-situ transmission electron microscope heating chip |
-
2021
- 2021-12-30 CN CN202111656100.6A patent/CN114264678A/en active Pending
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104319220A (en) * | 2014-10-14 | 2015-01-28 | 西安交通大学 | Quantitative nanometer heating table for electron microscope |
CN105136822A (en) * | 2015-08-06 | 2015-12-09 | 南京大学 | Nanometer material transmission electron microscope in-situ testing chip, preparation method and applications thereof |
CN107765037A (en) * | 2017-09-05 | 2018-03-06 | 浙江大学 | High-temp in-situ specimen holder |
CN111312573A (en) * | 2020-03-12 | 2020-06-19 | 厦门超新芯科技有限公司 | Transmission electron microscope high-resolution in-situ liquid phase heating chip and preparation method thereof |
CN111370280A (en) * | 2020-03-12 | 2020-07-03 | 厦门超新芯科技有限公司 | Transmission electron microscope high-resolution in-situ gas phase heating chip and preparation method thereof |
WO2021179541A1 (en) * | 2020-03-12 | 2021-09-16 | 厦门超新芯科技有限公司 | Transmission electron microscope in-situ chip and preparation method therefor |
CN112129786A (en) * | 2020-10-20 | 2020-12-25 | 厦门大学 | Transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip and preparation method thereof |
CN217688648U (en) * | 2021-12-30 | 2022-10-28 | 北京工业大学 | In-situ transmission electron microscope heating chip |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
TW416117B (en) | Monocrystalline ceramic electrostatic chuck | |
EP3370477B1 (en) | Heater unit | |
JP2015008287A (en) | Temperature controlled substrate support assembly | |
CN110085546B (en) | Electrostatic carrier for thin substrate handling | |
CN217688648U (en) | In-situ transmission electron microscope heating chip | |
US20080277768A1 (en) | Silicon member and method of manufacturing the same | |
CN111879796A (en) | Transmission electron microscope high-resolution in-situ fluid freezing chip and preparation method thereof | |
CN110383432A (en) | Substrate supporting unit and film formation device with substrate supporting unit | |
CN212932446U (en) | Transmission electron microscope high-resolution in-situ fluid freezing chip | |
CN114264678A (en) | In-situ transmission electron microscope heating chip and preparation method thereof | |
TWI659498B (en) | Substrate carrying table for vacuum processing device and manufacturing method thereof | |
CN111812125A (en) | Transmission electron microscope high-resolution in-situ liquid phase temperature change chip and preparation method thereof | |
JP2017520080A (en) | Method and apparatus for plasma processing a substrate | |
CN114112085B (en) | Manufacturing method of high-efficiency MEMS high-temperature film thermocouple sensor | |
CN111474195B (en) | Self-alignment in-situ characterization chip and preparation and use methods thereof | |
US11410869B1 (en) | Electrostatic chuck with differentiated ceramics | |
US20220285140A1 (en) | Apparatus For Fiber Optic Temperature Probe In Processing Chambers | |
WO2023096719A1 (en) | Electrostatic chuck with detachable shaft | |
US20240038483A1 (en) | Charged particle microscopy mems sample support | |
CN103489754B (en) | Preparation method of small-size silver nanoparticles | |
Oliveira et al. | Development of MEMS based microCVD technique for new materials thin films deposition | |
GB2613733A (en) | Transmission electron microscope high-resolution in-situ fluid freezing chip and preparation method therefor | |
US11837492B2 (en) | Electrostatic chuck having a gas flow feature, and related methods | |
CN113394090B (en) | Manufacturing method of n-type 4H-SiC ohmic contact with low resistivity | |
JPH0837173A (en) | Forming apparatus |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |