CN109665485B - MEMS heating chip for microscopic in-situ observation and manufacturing method thereof - Google Patents
MEMS heating chip for microscopic in-situ observation and manufacturing method thereof Download PDFInfo
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 160
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 47
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- 229910052581 Si3N4 Inorganic materials 0.000 claims description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 5
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910002601 GaN Inorganic materials 0.000 claims description 4
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims description 4
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 claims description 4
- 239000004642 Polyimide Substances 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 229910001080 W alloy Inorganic materials 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 239000011651 chromium Substances 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
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- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B7/00—Microstructural systems; Auxiliary parts of microstructural devices or systems
- B81B7/02—Microstructural systems; Auxiliary parts of microstructural devices or systems containing distinct electrical or optical devices of particular relevance for their function, e.g. microelectro-mechanical systems [MEMS]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00206—Processes for functionalising a surface, e.g. provide the surface with specific mechanical, chemical or biological properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00349—Creating layers of material on a substrate
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Computer Hardware Design (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Micromachines (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
The invention provides an MEMS heating chip for microscopic in-situ observation and a preparation method thereof, comprising the following steps: the silicon-based substrate is sequentially provided with a supporting layer and a passivation layer on the silicon-based substrate; the heating electrode and the measuring electrode are arranged on the upper surface of the passivation layer, are arranged in an insulating manner in the same layer and are both positioned on the passivation layer, and surround an observation area for microscopic in-situ observation; the upper surface of the heat insulation cavity corresponds to the observation area in the direction perpendicular to the silicon substrate. According to the heating chip, the heating electrode and the measuring electrode are protected by the passivation layer, so that the resistance in the heating process is more stable, the temperature can be heated to be more than 1000 ℃, gas and liquid are effectively isolated, the electrode is prevented from volatilizing and polluting a sample to be tested in the heating process, the heating temperature of the heating chip is high, the heating is stable, the pollution is small, and then the detection requirement of microscopic in-situ observation by SEM or TEM is met.
Description
Technical Field
The invention relates to the field of heating chips, in particular to an MEMS heating chip for microscopic in-situ observation and a manufacturing method thereof.
Background
The heating chip is a high-tech electronic mechanical device manufactured by combining micro-machining, precision machining and other technologies based on micro-electronic technology (semiconductor manufacturing technology). At present, the MEMS-based chip is widely applied to the fields of industrial control, automobile electronics, medical instruments, analytical instruments, air quality detection and the like. Compared with the traditional mechanical flowmeter, the heating chip has the characteristics of small volume, light weight, low power consumption and high reliability. The heating chip based on the silicon micromachining technology is formed by micromachining a silicon-based semiconductor material using a microelectromechanical system (MEMS).
Microelectromechanical systems (Micro-Electro-MECHANICAL SYSTEM, MEMS) are an advanced manufacturing technology platform. MEMS technology includes two major parts, microelectronics and micromachining. The main contents of microelectronic technology include oxide layer growth, photoetching mask manufacture, photoetching selective doping (shielding diffusion and ion implantation), film (layer) growth, wire manufacture and the like. The main contents of the micro-processing technology are silicon surface micro-processing and silicon body micro-processing (anisotropic etching and sacrificial layer) technology, wafer bonding technology, deep structure exposure and electroforming technology (LIGA) for manufacturing high aspect ratio structures, and the like. Integrated circuits and many sensors can be fabricated using microelectronics technologies. The silicon-based processing technology is a micro-processing technology developed on the basis of the micro-electronic processing technology and mainly depends on the process technologies of photoetching, diffusion, oxidation, film growth, dry etching, wet etching, evaporation sputtering and the like.
Because the heating chip relates to multidisciplinary field, the technical difficulty is big, and processing requirement is high, reaches the heating of about a thousand two hundred degrees on millimeter size chip, has very big challenge. In particular, scanning electron microscopes (scanning electronmicroscope, SEM) and transmission electron microscopes (Transmission electron microscope, TEM) require a heating function of about one thousand two hundred degrees for heating the chip when observing the sample.
However, in the prior art, a heating chip generally uses silicon nitride, silicon oxide and the like as a supporting film, an electrode is added as a heating layer, and the heating temperature is regulated by changing the current, so that the heating chip has the problems that the heating temperature is low and is mostly lower than 600 ℃; in the heating process, the metal electrode is evaporated, so that the heating temperature drift is serious, the heating effect is unstable, and the evaporating metal ash pollutes the observation cavity, so that the microcosmic in-situ heating observation effect of the object to be detected is affected.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the MEMS heating chip for microscopic in-situ observation and the manufacturing method thereof, and the passivation layer is adopted to protect the heating electrode and the measuring electrode, so that the heating chip has high heating temperature, stable heating, small pollution and wide application range, and further meets the detection requirement of SEM or TEM for microscopic in-situ observation. The heating chip has high heating temperature, stable heating, small pollution and wide application range, and further meets the detection requirement of microscopic in-situ observation by SEM or TEM.
In order to achieve the above object, on the one hand, the embodiment of the present invention adopts the following technical scheme:
A MEMS heater chip for microscopic in situ observation, the heater chip comprising: the silicon-based substrate is sequentially provided with a supporting layer and a passivation layer on the silicon-based substrate; the heating electrode and the measuring electrode are arranged on the upper surface of the passivation layer, are arranged in an insulating manner in the same layer and are both positioned on the passivation layer, and surround an observation area for microscopic in-situ observation; the upper surface of the heat insulation cavity corresponds to the observation area in the direction perpendicular to the silicon substrate.
Further, a plurality of spiral hollow heating channels positioned in the passivation layer are arranged in the observation area, and a plurality of observation windows for microscopic in-situ observation are arranged in the heating channels.
Further, the measuring electrodes are symmetrically arranged at two sides of the observation area, and the heating electrodes are symmetrically arranged at two sides of the measuring electrodes.
Further, the passivation layer is made of any one or more of silicon dioxide, silicon nitride and silicon carbide, and the thickness of the passivation layer is 0.01-100 mu m.
Further, the material of the supporting layer is any one or more of silicon, gallium nitride, polyimide or polyethylene terephthalate, gallium arsenide and quartz glass, and the thickness of the supporting layer is 50-2000 mu m.
Further, the heating electrode and the measuring electrode are made of any one or more of nickel, platinum, gold, aluminum, copper and polysilicon.
Further, the upper surface and/or the lower surface of the heating electrode and the measuring electrode are/is provided with a metal adhesion layer.
Further, the material of the metal adhesion layer comprises titanium, chromium, nickel, titanium oxide or titanium tungsten alloy.
On the other hand, the embodiment of the invention also adopts the following technical scheme:
A method of fabricating a MEMS heating chip for microscopic in-situ observation, comprising:
A silicon-based substrate is provided and,
Sequentially forming a supporting layer and a passivation layer on a silicon-based substrate;
forming a heating electrode and a measuring electrode on the upper surface of the passivation layer, wherein the heating electrode and the measuring electrode are arranged in an insulating manner on the passivation layer, and are arranged on the passivation layer, and the heating electrode and the measuring electrode surround an observation area for microscopic in-situ observation;
And forming a heat insulation cavity penetrating the silicon substrate and the supporting layer on the lower surface of the silicon substrate, wherein the upper surface of the heat insulation cavity corresponds to the observation area in the direction perpendicular to the silicon substrate.
Further, the method also comprises the step of arranging a metal adhesion layer on the upper surface and/or the lower surface of the heating electrode and the measuring electrode.
Compared with the prior art, the invention has the following technical effects:
The invention provides an MEMS heating chip for microscopic in-situ observation and a manufacturing method thereof, comprising the following steps: the silicon-based substrate is sequentially provided with a supporting layer and a passivation layer on the silicon-based substrate; the heating electrode and the measuring electrode are arranged on the upper surface of the passivation layer, are arranged in an insulating manner in the same layer and are both positioned on the passivation layer, and surround an observation area for microscopic in-situ observation; the upper surface of the heat insulation cavity corresponds to the observation area in the direction perpendicular to the silicon substrate. According to the heating chip, the heating electrode and the measuring electrode are protected by the passivation layer, so that the resistance is more stable in the heating process, the temperature can be heated to a temperature above 1000 ℃, the gas and the liquid can be effectively isolated to protect the internal electrode element, the electrode is prevented from volatilizing and polluting a sample to be tested in the heating process, the heating temperature of the heating chip is high, the heating is stable, the pollution is small, the application range is wide, and then the detection requirement of microscopic in-situ observation by SEM or TEM is met.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a MEMS heating chip for microscopic in-situ observation according to an embodiment of the present invention;
FIG. 2 is a top view of a MEMS heating chip for microscopic in situ observation provided by an embodiment of the present invention;
FIG. 3 is a partial enlarged view of an observation area of a MEMS heating chip for microscopic in-situ observation provided by an embodiment of the present invention;
FIG. 4 is a schematic illustration of a method for fabricating a MEMS heating chip for microscopic in-situ observation according to an embodiment of the present invention;
Wherein: 1. a silicon-based substrate; 2. a support layer; 3. a passivation layer; 4. heating the electrode; 5. a measuring electrode; 6. an observation area; 61. a heating channel; 62. an observation window; 7. and (5) insulating the cavity.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In addition, the term "and/or" herein is merely an association relationship describing an association object, and means that three relationships may exist, for example, a and/or B may mean: a exists alone, A and B exist together, and B exists alone. In addition, the character "/" herein generally indicates that the front and rear associated objects are an "or" relationship.
As shown in fig. 1, an embodiment of the present invention provides a MEMS heating chip for microscopic in-situ observation, the heating chip comprising: a silicon-based substrate 1, a supporting layer 2 and a passivation layer 3 which are sequentially arranged on the silicon-based substrate 1; the heating electrode 4 and the measuring electrode 5 are arranged on the upper surface of the passivation layer 3, the heating electrode 4 and the measuring electrode 5 are arranged in an insulating manner in the same layer and are both positioned on the passivation layer 3, and the heating electrode 4 and the measuring electrode 5 surround an observation area 6 for microscopic in-situ observation; the upper surface of the insulating cavity corresponds to the observation area 6 in the direction perpendicular to the silicon-based substrate, through the insulating cavity 7 provided in the silicon-based substrate 1 and the support layer 2.
The silicon-based substrate 1 is monocrystalline silicon, and the crystal orientation, size and thickness thereof need to be selected according to the application scenario, manufacturing process and performance requirements of the product, and are not particularly limited herein. In the present embodiment, only one of the heater chips is described as a structure in which a plurality of heater chips are fabricated on the silicon substrate 1.
The support layer 2 is used for supporting the whole heating chip. Preferably, the material of the supporting layer 2 is any one or more of silicon, gallium nitride, polyimide or polyethylene terephthalate, gallium arsenide and quartz glass, and the thickness of the supporting layer 2 is 50-2000 μm.
The passivation layer 3 is used for supporting the heating electrode and the measuring electrode and has an insulating effect, so that the stability of the electrode can be effectively improved. Preferably, the passivation layer 3 is made of any one or more of silicon carbide (SiC), aluminum oxide (Al 2O 3), silicon nitride (Si 3N 4), silicon dioxide (SiO 2), and the like, and has a thickness of 0.01 to 100 μm. In addition, the passivation layer 3 is made of materials with higher mechanical properties such as hardness and wear resistance, so that gas and liquid can be effectively isolated to protect internal electrode elements, volatilization of electrodes in a heating process can be avoided, and pollution to a test sample is avoided.
The heating electrode 4 and the measuring electrode 5 are both of an electrically conductive material, i.e. the resistance thereof has a positive correlation with temperature. The heating electrode 4 and the measuring electrode 5 are arranged in an insulating way, and the manufacturing of the heating electrode 4 and the measuring electrode 5 can be completed only by depositing a metal electrode layer and adopting a one-time metal patterning process, so that the electrode manufacturing yield is improved.
Preferably, the heating electrode 4 and the measuring electrode 5 are made of any one or more of nickel, platinum, gold, aluminum, copper and polysilicon. The thickness of the heating electrode 4 and the measuring electrode 5 are both 100 nm-400 nm, the thickness of the electrode is inversely proportional to the resistance, the thicker the electrode thickness is, the smaller the resistance is, and the thinner the electrode thickness is, the larger the resistance is.
It can be understood by those skilled in the art that, according to the working temperature of the heating chip, the related practitioner can reasonably select the measuring electrode of the heating chip and the composition materials of the heating electrode, not only metallic nickel, platinum, gold, aluminum, copper, etc.; and according to the type of the application device of the heating chip, the related practitioner can reasonably select the thickness of the measuring electrode and the heating electrode of the heating chip, and the thickness is not limited to the limitation.
The observation region 6 is used for microscopic in-situ observation of the object to be detected, is formed around by the heating electrode 4 and the measuring electrode 5, and is located on the passivation layer 3.
The heat insulation cavity 7 is positioned at the bottom of the supporting layer 2 and penetrates through the silicon-based substrate 1 and the supporting layer 2, and the upper surface of the heat insulation cavity 7 corresponds to the observation area 6 in the direction perpendicular to the silicon-based substrate 1. The structure of the insulating cavity 7 can avoid the diffusion of temperature, realize the rise of temperature in a shorter time and reach the temperature exceeding 1000 ℃.
Preferably, the inside of the heat insulation cavity 7 is of a vacuum structure, or is provided with gas or liquid with extremely low heat conductivity coefficient, so that heat diffusion is reduced, heat is ensured to be concentrated on the upper surface of the chip, and the sensitivity and the precision of the chip are improved.
According to the heating chip, the heating electrode and the measuring electrode are protected by the passivation layer, so that the resistance is more stable in the heating process, the temperature can be heated to a temperature above 1000 ℃, the gas and the liquid can be effectively isolated to protect the internal electrode element, the electrode is prevented from volatilizing and polluting a sample to be tested in the heating process, the heating temperature of the heating chip is high, the heating is stable, the pollution is small, the application range is wide, and then the detection requirement of microscopic in-situ observation by SEM or TEM is met.
Preferably, as shown in fig. 2, the measuring electrodes 5 are symmetrically disposed on both sides of the observation area 6, and the heating electrodes 4 are symmetrically disposed on both sides of the measuring electrodes 5.
The heating chip is connected with the outside through the heating electrode 4 to supply power, and the heating temperature is regulated by regulating the current; the temperature measuring electrode 5 is connected with the outside, and the temperature change is fed back by measuring the resistance change; the sample observation area 6 is used for placing a sample to be observed, so that the observation of the sample is realized while heating.
By adopting a heating and temperature measuring structure integrated mode, the heating temperature can be adjusted at any time and can be monitored and fed back at any time, so that the heating parameters are more reliable and stable, and the heating device is further used for in-situ heating observation of SEM or TEM micro particles.
Further, it is also necessary to form an external connection pad, a heating electrode lead, and a measuring electrode lead, which are provided in the same layer as the heating electrode 4 and the measuring electrode 5.
Preferably, as shown in fig. 3, a plurality of spiral hollow heating channels 61 are provided in the passivation layer 3 in the observation region 6, and a plurality of observation windows 62 for microscopic in-situ observation are provided in the heating channels 61.
Preferably, the heating channel 61 is a spiral hollow structure with one end located at the edge of the observation area 6 and the other end located at the middle of the observation area 6, and is spirally arranged from one end to the other end from large to small.
Preferably, the heating channel 61 comprises a plurality of helical hollow structures, for example comprising 2. The two spiral hollow structures are arranged in opposite ways, namely one end of the two spiral hollow structures is positioned at the edge of the observation area 6, the other end of the two spiral hollow structures is positioned at the middle position of the observation area 6, and the other end of the two spiral hollow structures is positioned at the edge symmetrical to the structure, and the other end of the other spiral hollow structures is also positioned at the middle position of the observation area 6 and symmetrical to the structure.
Preferably, the observation windows 62 are arranged at intervals at the upper end of the hollow heating channel 61 for in-situ observation of the tiny particle objects, and the number of the observation windows 62 is plural.
Preferably, the observation windows 62 are sequentially arranged at intervals along the spiral hollow structure, and at least four observation windows are arranged in each circle so as to meet the observation requirements of articles in different shapes.
Preferably, to accommodate the stress variations generated by the extreme temperatures, the upper and/or lower surfaces of the heating electrode 4 and the measuring electrode 5 are provided with a metal adhesion layer.
Preferably, the material of the metal adhesion layer comprises titanium, chromium, nickel, titanium oxide or titanium tungsten alloy.
Preferably, as shown in fig. 4, another embodiment of the present invention provides a method for manufacturing a MEMS heating chip for microscopic in-situ observation, which is applicable to any one of the heating chips described above and any one of the heating chips in the prior art. The manufacturing method of the heating chip provided in the embodiment specifically includes the following steps:
providing a silicon-based substrate 1;
Specifically, the silicon-based substrate 1 is monocrystalline silicon, and the crystal orientation, size and thickness thereof need to be selected according to the application scenario, manufacturing process and performance requirements of the product, which are not particularly limited herein. In the present embodiment, only one of the heater chips is described as a structure in which a plurality of heater chips are fabricated on the silicon substrate 1.
Sequentially forming a support layer 2 and a passivation layer 3 on a silicon-based substrate 1;
Specifically, a Low Pressure Chemical Vapor Deposition (LPCVD) method is used to sequentially deposit a support layer 2 and a passivation layer 3 on the upper surface of the silicon-based substrate. Wherein the supporting layer 2 is used for supporting the whole heating chip, and is made of any one or more of silicon, gallium nitride, polyimide or polyethylene terephthalate, gallium arsenide and quartz glass, and has a thickness of 50-2000 μm. The passivation layer 3 is used for supporting the heating electrode and the measuring electrode and has an insulating effect, so that the stability of the electrode can be effectively improved, and the passivation layer is made of any one or more of silicon carbide (SiC), aluminum oxide (Al 2O 3), silicon nitride (Si 3N 4), silicon dioxide (SiO 2) and other film structures, and has a thickness of 0.01-100 mu m. The passivation layer 3 is made of materials with higher mechanical properties such as hardness and wear resistance, can effectively isolate gas and liquid so as to protect internal electrode elements, and can also prevent the electrodes from volatilizing in the heating process and prevent the test sample from being polluted.
In addition, in other embodiments, the relevant practitioner can select the support layer 2 and the passivation layer 3 with reasonable parameters such as process, material, stress and thickness according to factors such as manufacturing process, production condition, product, etc.
Forming a heating electrode 4 and a measuring electrode 5 on the upper surface of the passivation layer 3, wherein the heating electrode 4 and the measuring electrode 5 are arranged in an insulating manner in the same layer and are both positioned on the passivation layer 3, and the heating electrode 4 and the measuring electrode 5 surround an observation area 6 for microscopic in-situ observation;
Specifically, a magnetron sputtering method or an electron beam evaporation method is adopted to deposit a metal electrode layer, photoresist is adopted to carry out photoetching patterning, and then the photoresist is stripped to pattern the metal electrode layer so as to form a heating electrode and a measuring electrode.
The heating electrode 4 and the measuring electrode 5 are arranged in the same layer, namely in a coplanar design, and the manufacturing of the heating electrode and the measuring electrode can be completed only by depositing a metal electrode layer and adopting a one-time metal patterning process. Compared with the prior art, the method reduces the complexity of the processing technology, reduces the manufacturing process and reduces the manufacturing cost, and meanwhile, the manufacturing yield of the electrode can be improved by adopting the coplanar design for the heating electrode and the measuring electrode, so that the manufacturing yield of the heating chip is improved.
A heat-insulating cavity 7 penetrating the silicon substrate 1 and the support layer 2 is formed on the lower surface of the silicon substrate 1, and the upper surface of the heat-insulating cavity 7 corresponds to the observation area 6 in the direction perpendicular to the silicon substrate 1.
Specifically, a wet etching process is used to pattern the lower surface of the silicon-based substrate and etch to form the insulating cavity. In other embodiments, an optional dry etching process forms an insulating cavity in the lower surface of the silicon-based substrate.
Preferably, the manufacturing method of the MEMS heating chip for microscopic in-situ observation further comprises the step of arranging metal adhesion layers on the upper surfaces and/or the lower surfaces of the heating electrode and the measuring electrode.
Wherein, the material of the metal adhesion layer comprises titanium, chromium, nickel, titanium oxide or titanium tungsten alloy.
The heating chip prepared by the method protects the heating electrode and the measuring electrode by adopting the passivation layer, so that the resistance is more stable in the heating process, the temperature can be heated to a temperature above 1000 ℃, the gas and the liquid can be effectively isolated to protect the internal electrode element, the electrode is prevented from volatilizing and polluting the sample to be tested in the heating process, the heating temperature of the heating chip is high, the heating is stable, the pollution is small, the application range is wide, and the detection requirement of microscopic in-situ observation by SEM or TEM is further met.
In summary, the present invention provides a MEMS heating chip for microscopic in-situ observation and a method for manufacturing the same, wherein the heating chip comprises: the silicon-based substrate is sequentially provided with a supporting layer and a passivation layer on the silicon-based substrate; the heating electrode and the measuring electrode are arranged on the upper surface of the passivation layer, are arranged in an insulating manner in the same layer and are both positioned on the passivation layer, and surround an observation area for microscopic in-situ observation; the upper surface of the heat insulation cavity corresponds to the observation area in the direction perpendicular to the silicon substrate. According to the heating chip, the heating electrode and the measuring electrode are protected by the passivation layer, so that the resistance is more stable in the heating process, the temperature can be heated to a temperature above 1000 ℃, the gas and the liquid can be effectively isolated to protect the internal electrode element, the electrode is prevented from volatilizing and polluting a sample to be tested in the heating process, the heating temperature of the heating chip is high, the heating is stable, the pollution is small, the application range is wide, and then the detection requirement of microscopic in-situ observation by SEM or TEM is met.
From the foregoing description of the embodiments, it will be apparent to those skilled in the art that, for convenience and brevity of description, only the above-described division of functional units is illustrated, and in practical application, the above-described functional allocation may be performed by different functional units, that is, the internal structure of the apparatus is divided into different functional units, so as to perform all or part of the functions described above. The specific working processes of the above-described systems, devices and units may refer to the corresponding processes in the foregoing method embodiments, which are not described herein.
In the several embodiments provided in the present application, it should be understood that the disclosed method and apparatus may be implemented in other manners. For example, the apparatus embodiments described above are merely illustrative, e.g., the division of the units or units is merely a logical functional division, and there may be additional divisions when actually implemented, e.g., multiple units or components may be combined or integrated into another system, or some features may be omitted or not performed. Alternatively, the coupling or direct coupling or communication connection shown or discussed with each other may be an indirect coupling or communication connection via some interfaces, devices or units, which may be in electrical, mechanical, or other forms.
The units described as separate units may or may not be physically separate, and units shown as units may or may not be physical units, may be located in one place, or may be distributed on a plurality of network units. Some or all of the units may be selected according to actual needs to achieve the purpose of the solution of this embodiment.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (9)
1. A MEMS heating chip for microscopic in-situ observation, comprising: a silicon-based substrate, a supporting layer and a passivation layer which are sequentially arranged on the silicon-based substrate; the heating electrode and the measuring electrode are arranged on the upper surface of the passivation layer, are arranged in an insulating mode in the same layer and are both positioned on the passivation layer, and surround an observation area for microscopic in-situ observation; the upper surface of the heat insulation cavity corresponds to the observation area in the direction perpendicular to the silicon-based substrate; the heating electrode and the measuring electrode are made of one or more of nickel, platinum, gold, aluminum, copper and polysilicon.
2. The MEMS heating chip for microscopic in-situ observation according to claim 1, wherein a plurality of helical hollow heating channels in the passivation layer are disposed within the observation region, and a plurality of observation windows for microscopic in-situ observation are disposed within the heating channels.
3. The MEMS heating chip for microscopic in-situ observation according to claim 1, wherein the measurement electrodes are symmetrically disposed on both sides of the observation region, and the heating electrodes are symmetrically disposed on both sides of the measurement electrodes.
4. The MEMS heating chip for microscopic in-situ observation according to claim 1, wherein the passivation layer is made of any one or more of silicon dioxide, silicon nitride and silicon carbide, and the passivation layer has a thickness of 0.01-100 μm.
5. The MEMS heating chip for microscopic in-situ observation according to claim 1, wherein the material of the supporting layer is any one or more of silicon, gallium nitride, polyimide or polyethylene terephthalate, gallium arsenide and quartz glass, and the thickness of the supporting layer is 50-2000 μm.
6. The MEMS heating chip for microscopic in-situ observation according to claim 1, wherein the upper and/or lower surfaces of the heating electrode and the measuring electrode are provided with a metal adhesion layer.
7. The MEMS heating chip for microscopic in-situ observation according to claim 6, wherein the material of the metal adhesion layer comprises titanium, chromium, nickel, titanium oxide, or titanium tungsten alloy.
8. A method for fabricating a MEMS heating chip for microscopic in-situ observation, comprising: providing a silicon-based substrate, and sequentially forming a supporting layer and a passivation layer on the silicon-based substrate; forming a heating electrode and a measuring electrode on the upper surface of the passivation layer, wherein the heating electrode and the measuring electrode are arranged in an insulating manner in the same layer and are both positioned on the passivation layer, and the heating electrode and the measuring electrode surround an observation area for microscopic in-situ observation; and forming a heat insulation cavity penetrating through the silicon substrate and the supporting layer on the lower surface of the silicon substrate, wherein the upper surface of the heat insulation cavity corresponds to the observation area in the direction perpendicular to the silicon substrate.
9. The method of claim 8, further comprising providing a metal adhesion layer on the upper and/or lower surfaces of the heating electrode and the measuring electrode.
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| CN110702717B (en) * | 2019-10-15 | 2022-05-10 | 重庆大学 | Preparation method for transmission electron microscope slicing sample and slicing transfer device |
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| CN111272781A (en) * | 2020-02-14 | 2020-06-12 | 东南大学 | CVD chip for in-situ characterization of transmission electron microscope and use method thereof |
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| WO2022040967A1 (en) * | 2020-08-26 | 2022-03-03 | 厦门超新芯科技有限公司 | High-resolution in-situ temperature difference chip for transmission electron microscope and manufacturing 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 |
| CN112837984B (en) * | 2021-01-06 | 2023-07-04 | 东南大学 | Double-temperature-zone sealed cavity chip suitable for transmission electron microscope characterization and manufacturing method thereof |
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