CN105136822A - Nanometer material transmission electron microscope in-situ testing chip, preparation method and applications thereof - Google Patents
Nanometer material transmission electron microscope in-situ testing chip, preparation method and applications thereof Download PDFInfo
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Abstract
The present invention discloses a nanometer material transmission electron microscope in-situ testing chip, a preparation method and applications thereof, and belongs to the technical field of nanometer material performance in-situ testing. The chip comprises a silicon substrate, insulating layers and a film window, wherein the insulating layer respectively grows on both surfaces of the silicon substrate, a metal film or device or a semiconductor function film or device grows on the chip front surface insulating layer so as to apply various physical and chemical effects on a sample, the center of the chip is provided with the film window, and the film window region is provided with a electron beam penetrating long hole or electron beam penetrating long groove having a large aspect ratio. According to the present invention, the transmission electron microscope sample can be subjected to in-situ measurement under the atomic scale resolution, the nano-wire samples and the nano-tube samples can be subjected to in-situ characterization, the bulk samples and the heterojunction interface samples can be subjected to in-situ characterization, the placement of the sample through the micro manipulator in the focused ion beam system and the laboratory can be achieved, and the sample transferred and fixed on the chip can be continuously processed by using the ion reduction equipment.
Description
Technical field
The present invention relates to nano ZnO in-situ testing technique field, more particularly, relate to a kind of nano material transmission electron microscope in-situ test chip, chip preparation method and application thereof.
Background technology
In recent years, nano material to obtain the extensive concern of people because of nano-meter characteristics such as its small-size effect, surface effect, quantum size effect and macro quanta tunnel effects at field of scientific study.Transmission electron microscope (TransmissionElectronMicroscope, TEM) is a kind of powerful modern material characterization method, for the fine structure being less than 0.2 μm cannot seen clearly under analyzing optical microscope.Transmission electron microscope of today can reach sub-dust class resolution ratio, is the powerful measure analyzing nano material.Nano material has peculiar effect in fields such as electricity, calorifics, mechanics, along with MEMS (micro electro mechanical system) (MicroElectromechanicalSystem, and the development of nano electromechanical systems (NanoElectromechanicalSystem) MEMS), from nanoscale disclose material structure and above field the relation of various effect, become problem in the urgent need to address.
While obtaining material structure information by transmission electron microscope, detect the character such as electricity corresponding to this structure, calorifics, mechanics, belong to In Situ Tem Study.The instrument realizing In Situ Tem Study at present mainly contains environment transmission electron microscope (ETEM), transmission electron microscope original position specimen holder, original position MEMS chip etc.Have benefited from the development of MEMS technology, can integrated increasing physics, chemical functional in existing original position MEMS chip.And chip small size, energising can the feature of work meet very well with the requirement carrying out transmission electron microscope in-situ test.But existing original position MEMS chip still has its limitation in application, focused ion beam (FIB) system generally can only be used to carry out sample transfer with fixing, limit service condition, and considerably increase use cost.In addition, focused ion beam system cannot be avoided when carrying out sample transfer and fixing producing sample polluting, but existing original position MEMS chip completes the transfer of sample and cannot process sample after fixing again.Above-mentioned limitation greatly limit the application of original position MEMS chip, and does not have solution well at present.
Summary of the invention
1. invent the technical matters that will solve
The object of the invention is to overcome above-mentioned the deficiencies in the prior art, provide a kind of nano material transmission electron microscope in-situ test chip, chip preparation method and application thereof; Adopt in-situ test chip of the present invention, focused ion beam (FIB) system can be used to carry out processing and the transfer of sample, also sample can be placed at FIB external application micro-operation hand (micromanipulator), and the chip being placed with sample can carry out Ion Cleaning or thinning to sample in ion milling equipment, can realize the In Situ Tem Study to the several samples comprising metal, low-dimensional materials, heterojunction boundary and block sample.
2. technical scheme
For achieving the above object, technical scheme provided by the invention is:
A kind of nano material transmission electron microscope in-situ test chip of the present invention, comprise silicon chip, insulation course, film window, described silicon chip two sides is provided with insulation course, and silicon chip front offers the film window be made up of insulation course, have electron beam elongated hole or saturating electron beam elongated slot in film window, the width of described saturating electron beam elongated hole or thoroughly electron beam elongated slot is 5-20 μm; The insulation course in described silicon chip front is provided with all kinds of physics, the metallic film of chemical action or the device needed for can applying sample, or semiconductor function film or device.
Further, the length of described saturating electron beam elongated hole or thoroughly electron beam elongated slot is 100-400 μm.
Further; described insulation course comprises the silicon dioxide layer grown on a silicon substrate and the silicon nitride layer grown on silicon dioxide layer, because silicon dioxide layer crosses thin can impact the protective effect in the stress regulation and control of silicon nitride and supporting capacity and etching process.Silicon nitride layer is crossed thin, affect to the support effect of sample and in etching process the protective effect that rises, therefore the thickness of described silicon dioxide layer is 200-1000nm, and the thickness of silicon nitride layer is 5-200nm.
Further, described metallic film or device, semiconductor function film or device are positioned at the one or both sides distribution along saturating electron beam elongated hole or electron beam elongated slot thoroughly of part on film window.
Further, described silicon chip thickness is 100-400 μm.
The preparation method of a kind of nano material transmission electron microscope in-situ test chip of the present invention, the steps include:
Step one, prepare two sides with the silicon chip of silicon dioxide layer, in silicon chip two sides grown silicon nitride layer;
Step 2, utilize photoetching process, electrode pattern is transferred to step one gained silicon chip front from lithography mask version;
Step 3, utilize micro-electromechanical processing technology, produce metallic film or device in step 2 gained silicon chip front, or semiconductor function film or device;
Step 4, utilize photoetching process and reactive ion etching process, the insulation course at the step 3 gained silicon chip back side etches a square window, and this square window is positioned on the axis of silicon chip;
Step 5, utilize photoetching process and reactive ion etching process, the insulation course in step 4 gained silicon chip front etches electron beam elongated hole or electron beam elongated slot thoroughly;
Step 6, step 5 gained silicon chip is put into potassium hydroxide solution carry out wet etching, until etch into the silicon dioxide layer in silicon chip front thus leave film window, take out silicon chip cleaning;
Step 7, step 6 gained silicon chip is carried out scribing, be divided into individual chips.
The application of a kind of nano material transmission electron microscope in-situ test chip of the present invention, micromanipulator is used to place sample or utilize focused ion beam system to process and place sample on in-situ test chip, make the metallic film on sample and chip or device, or semiconductor function film or device are connected, and be positioned at film window region saturating electron beam elongated hole or thoroughly on electron beam elongated slot; The test chip being loaded with sample is loaded in specimen holder and sends into transmission electron microscope and observe, physics, chemical action receive the signal that sample produces are applied to sample, to sample carry out atomic scale differentiate under home position observation.
Further, the transfer that completes sample of in-situ test chip with fixing after in ion milling equipment, Ion Cleaning and thinning can be carried out to sample.
3. beneficial effect
Adopt technical scheme provided by the invention, compared with existing known technology, there is following remarkable result:
(1) a kind of nano material transmission electron microscope in-situ test chip of the present invention, aspect is have employed than saturating electron beam elongated hole or saturating electron beam elongated slot structure at film window place, give micro-operation hand (micromanipulator) needle point along saturating electron beam elongated hole or thoroughly larger on electron beam elongated slot direction activity space, allow needle point to move up and down through saturating electron beam elongated hole or saturating electron beam elongated slot simultaneously, thus micro-operation hand can be used to coordinate optical microscope to carry out the transfer of sample, reduce service condition and the use cost of chip;
(2) a kind of nano material transmission electron microscope in-situ test chip of the present invention, saturating electron beam elongated hole or thoroughly electron beam elongated slot length breadth ratio are suitable, along saturating electron beam elongated hole or thoroughly electron beam elongated slot direction low-angle incidence ion beam also can well through, therefore conventional ion stripping apparatus can be used to carry out Ion Cleaning or thinning for the sample transferred on chip, effectively can remove the pollution brought in sample transfer and fixation procedure, or continuation processing is carried out to sample, improve electron microscopic observation effect.
(3) a kind of nano material transmission electron microscope in-situ test chip of the present invention, Making programme is simple, is applicable to producing in enormous quantities, and one single chip cost is remarkable reduction compared with existing chip, and has wide range of applications, and result of use is good, is convenient to promote.
Accompanying drawing explanation
Fig. 1 is the Facad structure schematic diagram of situ test chip of the present invention;
Fig. 2 is the partial enlarged drawing at film window position in Fig. 1;
Fig. 3 is the structure schematic diagram of situ test chip of the present invention.
Label declaration in schematic diagram:
1, square window; 2, metal electrode; 3, film window; 4, saturating E-beam area.
Embodiment
For understanding content of the present invention further, the present invention is described in detail in conjunction with the accompanying drawings and embodiments.
Embodiment 1
Referring to Fig. 1, Fig. 2 and Fig. 3, a kind of nano material transmission electron microscope original position electrical testing chip of the present embodiment, comprises silicon chip, insulation course, film window 3 and saturating E-beam area 4.Be specially: described silicon chip is rectangular sheet, thickness is 400 μm, on silicon chip two sides, all length has insulation course, described insulation course comprises the silicon dioxide layer grown on a silicon substrate and the silicon nitride layer grown on silicon dioxide layer, the thickness of silicon dioxide layer is 900nm, and the thickness of silicon nitride layer is 200nm.Silicon chip front insulation course needs to arrange all kinds of physics, the metallic film of chemical action or device needed for can applying sample, or semiconductor function film or device, referring to Fig. 1, the present embodiment is long on the insulation course of silicon chip front metal electrode 2, the thickness of this metal electrode 2 is 150nm, and metal electrode 2 is mainly used in being connected with the lead-in wire on sample for use in transmitted electron microscope bar.In silicon chip front, central authorities offer the film window 3 be made up of insulation course, and this film window 3 obtains by carrying out wet etching to silicon chip overleaf.
The present embodiment is provided with E-beam area 4 in the central authorities of film window 3, offer in this saturating E-beam area 4 can supplied for electronic bundle, ion beam through and the saturating electron beam elongated hole allowing micro-operation hand (micromanipulator) needle point upper and lower and movable or elongated slot.Central authorities specific to the present embodiment film window 3 then have electron beam elongated slot, described metal electrode 2 is positioned at the part on film window 3 and distributes along the both sides of saturating electron beam elongated slot, this saturating electron beam elongated slot extends to film window 3 edge, length is 300 μm, width is 10 μm, for through electron beam and ion beam.
The electrical testing chip of the present embodiment, multiple metal electrode 2 connected for sample is provided, therefore, it is possible to for the original position electrical testing of the several samples such as metal, nano wire, nanotube, two-dimensional material, heterojunction boundary and block sample at saturating electron beam elongated slot areas adjacent.
In addition, the present embodiment have employed the saturating electron beam elongated slot structure of aspect ratio at film window 3 place, make chip both can complete sample processing in the FIB being equipped with micro-operation hand, again with the micro-operation hand in FIB by sample across the saturating electron beam elongated slot being placed on chip is connected and fixed with the metal electrode 2 contacted by the certain thickness platinum of deposition, taking-up chip puts into transmission electron microscope then.Also the micro-operation hand by experiment in room environmental can be transferred in desired location by sample, then carry out processing or directly entering transmission electron microscope observing in FIB, more economical compared with shifting with the intrasystem micro-operation hand of the FIB of routine.
Inventor points out, the effect of saturating electron beam elongated slot be allow electron beam through, its wide meeting causes comparatively small sample cannot ride on electron beam elongated slot, narrow, and the permeable region of electron beam is diminished affects observing effect.Too short, the scope of activities needed for micro-operation hand (micromanipulator) needle point cannot be given, long, affect the intensity of film window.Tradition in-situ test chip uses the round tube hole of micron order diameter, elliptical hole or thickness lower than the silicon nitride film of 50nm through electron beam in film window region, if use micro-operation hand (micromanipulator) to shift sample, the space that it moves up and down cannot be provided, so focused ion beam system can only be used to carry out the transfer of sample, limit service condition, and considerably increase use cost.Simultaneously, aperture or film can stop the ion beam of oblique incidence, conventional films window structure cannot through the ion beam of low-angle incidence, so complete sample transfer with fixing after in ion milling equipment, Ion Cleaning and thinning cannot be carried out to sample, and focused ion beam system cannot be avoided when carrying out sample transfer and fixing producing sample polluting, this directly affects observing effect.
The problems referred to above all make original position MEMS chip be very restricted in application, and it is 300 μm that the present embodiment designs electron beam elongated slot length, and width is 10 μm, makes length breadth ratio be 30.Use aspect than saturating electron beam elongated slot through electron beam, give micro-operation hand (micromanipulator) needle point along activity space larger on saturating electron beam elongated slot direction, allow needle point to move up and down through saturating electron beam elongated slot simultaneously, thus micro-operation hand can be used to coordinate optical microscope to carry out the transfer of sample, reduce service condition and the use cost of chip.And due to saturating electron beam elongated slot length breadth ratio suitable, along saturating electron beam elongated slot direction low-angle incidence ion beam also can well through, therefore conventional ion stripping apparatus can be used to carry out Ion Cleaning or thinning for the sample transferred on chip, effectively can remove the pollution brought in sample transfer and fixation procedure, or continuation processing is carried out to sample, improve electron microscopic observation effect.
And for output in film window aspect than saturating electron beam elongated slot compare aperture can stress concentrate, easily cause the problem that film breaks along saturating electron beam elongated slot direction, the present embodiment adopts the composite bed of silica coating and silicon nitride film layer to form film window, the intensity utilizing the silica coating good and stress regulation and control effect of silicon nitride is effectively improved to the intensity of film window, thus solve film easily along the problem broken in saturating electron beam elongated slot direction.
The process that the present embodiment prepares nano material transmission electron microscope original position electrical testing chip is:
(1) Si (100) wafer (i.e. silicon chip) of two sides with silicon dioxide layer is prepared, wafer size 2 cun, thickness 400um, silicon dioxide layer thickness 900nm.Plasma enhanced chemical vapor deposition method (PECVD) is utilized to be the silicon nitride layer of 200nm at wafer two sides growth thickness, growth temperature 300 DEG C, N
2flow 900sccm, SiH
4flow 25sccm;
(2) wafer that step (1) is produced is put into muffle furnace 500 DEG C annealing 1h, cool with stove;
(3) photoetching process is utilized, 7s is exposed under the hardcontact pattern of ultraviolet photolithographic machine, electrode pattern is transferred to from lithography mask version the wafer frontside that step (2) produces, and then develop 45s in 3038 developer solutions, is AZ5214 with photoresist;
(4) electron beam evaporation is utilized, the wafer frontside evaporation a layer thickness produced in step (3) is the Cr of 5nm, evaporation a layer thickness is the Au of 100nm again, then wafer frontside is successively put into acetone upward, aqueous isopropanol carries out ultrasonic cleaning, finally use washed with de-ionized water, remove photoresist, leave metal electrode;
(5) photoetching process is utilized, 7s is exposed under the hardcontact pattern of ultraviolet photolithographic machine, square window pattern is transferred to from lithography mask version the wafer rear that step (4) produces, and then develop 45s in 3038 developer solutions, is AZ5214 with photoresist;
(6) reactive ion etching process (RIE) is utilized, the silicon nitride layer of the wafer rear produced in step (5) and silicon dioxide layer etch square window, then wafer rear is successively put into acetone upward, aqueous isopropanol carries out ultrasonic cleaning, finally use washed with de-ionized water, remove photoresist; The square window 5 of the present embodiment is positioned on the axis of wafer, specifically determines according to the sample for use in transmitted electron microscope bar that chip is supporting.Because silicon wet etching exists etching angle, square window is too small, and etch into certain depth and namely form pyramid-shaped pit and cannot etch into front, window is excessive, the film window in front can be caused excessive thus affect the strength and stability of film window.According to substrates of different thickness, square window size is can etch into substrate front and to make front film window be not more than 2mm*2mm to determine;
(7) photoetching process is utilized, 7s is exposed under the hardcontact pattern of ultraviolet photolithographic machine, turned by saturating electron beam elongated slot pattern and move on to from lithography mask version the wafer frontside that step (6) produces, then develop 45s in 3038 developer solutions, is AZ5214 with photoresist;
(8) reactive ion etching process (RIE) is utilized, the silicon nitride layer of the wafer frontside produced in step (7) and silicon dioxide layer etch electron beam elongated slot, then wafer frontside is successively put into acetone upward, aqueous isopropanol carries out ultrasonic cleaning, finally use washed with de-ionized water, remove photoresist;
(9) wafer rear that step (8) is produced being put into mass percent concentration is upward that 20% potassium hydroxide solution carries out wet etching, etching temperature is 80 DEG C, etch about 4.5h until front only leaves film window, take out wafer cleaning.
(10) wafer that step (9) is produced is carried out scribing, be divided into individual chips.
The flow process that the present embodiment makes nano material transmission electron microscope original position electrical testing chip is simple, and be applicable to producing in enormous quantities, one single chip cost is remarkable reduction compared with existing chip, and has wide range of applications.Micro-operation hand can be utilized in laboratory environments to place sample, focused ion beam system also can be utilized to process and place sample, sample is connected with the electrode on chip, and be positioned at the film window region of electron beam.The chip being loaded with sample is fit into can provide and sends into transmission electron microscope in the specimen holder of multichannel electricity passage and observe, by electric signal sample being applied to electricity effect or receive sample realize atomic scale differentiate under electricity home position observation to sample.Simultaneously this chip the transfer completing sample with fixing after in ion milling equipment, Ion Cleaning and thinning can be carried out to sample, effectively can reduce to the pollution that sample produces in process, improve electron microscopic observation effect.
Introduce below and utilize focused ion beam system (FIB) to prepare and shift heterojunction boundary sample and use ion milling equipment to carry out the detailed process of processing further to sample:
(1) chip prepared by the substrate with heterostructure grown, half load sharing net and the present embodiment is put into focused ion beam system cavity, on substrate, cut out with the ion beam focused on the heterojunction boundary sample blank that a size is approximately 20 μm × 10 μm × 3 μm.
(2) the micro-operation hand needle point in FIB is utilized to be connected by depositing certain thickness platinum with sample blank, mention sample blank and to be transferred to half load sharing online, by depositing certain thickness platinum, sample blank being connected with half load sharing net, re-using focused ion beam and sealing-off is carried out to micro-operation hand needle point and sample blank.Focused ion beam carried out to sample blank on the net at half load sharing thinning, obtain the heterojunction boundary sample with thin district.
(3) by micro-operation hand needle point with complete thinning sample and be connected by depositing certain thickness platinum, re-use focused ion beam by sample from the online sealing-off of half load sharing, sample transferred to the saturating electron beam elongated slot position of chip by micro-operation hand and contact with the electrode needed, by focused ion beam, sealing-off being carried out to sample and micro-operation hand needle point.Deposit certain thickness platinum at sample and electrode contact locations to weld, can fixed sample, can ensure again have good electricity to be connected between sample with electrode.
(4) from FIB system, the chip being loaded with sample is taken out, put into ion milling equipment (as PIPS), adjustment chip and top ion gun relative angle to ion beam incidence direction and saturating electron beam elongated slot direction consistent, ion beam can bombard sample from top with low-angle.Due to ion beam along smaller angle (1 to 5 °) from top incident sample position, therefore the ion beam spot reality of sample plane is elongated, to electron beam elongated slot place be dropped on thus the ion making not to be irradiated to sample can pass from saturating electron beam elongated slot, avoid the damage to chip thin films window.Fixed chip position, closes bottom ion gun, selects suitable line size, open top ion gun and carry out Ion Cleaning to sample.
(5) from ion milling equipment, take out chip after completing Ion Cleaning, load sample for use in transmitted electron microscope bar, be connected with electrical measurement equipment, transmission electron microscope can be entered and carry out home position observation and test.
Embodiment 2
A kind of nano material transmission electron microscope original position electrical testing chip of the present embodiment and preparation method thereof, basic with embodiment 1, its difference is: in the present embodiment, silicon chip thickness is 300 μm, metal electrode is positioned at the part on film window and distributes along the side of saturating electron beam elongated slot, the length of saturating electron beam elongated slot is 300 μm, and width is 10 μm.The thickness of metal electrode is 50nm, and in insulation course, the thickness of silicon dioxide layer is 200nm, and the thickness of silicon nitride layer is 5nm.
It is as follows that the present embodiment application original position electrical testing chip uses micro-operation hand (micromanipulator) to shift the process of nano wire sample in the lab:
(1) provoke with micro-operation hand needle point the nano wire sample that length is about 20 microns under an optical microscope.Because micro-operation hand is glass material, after provoking sample, by making with the Van der Waals force of sample room, sample is stable to be attached on micro-operation hand needle point.Micromanipulator only needs optical microscope and manual micro-operation hand system to get final product work, compare focused ion beam system have easy to operate, be suitable for outfit, feature that use cost is low.
(2) above mobile micro-operation hand needle point to the saturating electron beam elongated slot of chip, make micro-operation hand needle point concordant with saturating electron beam elongated slot, the angle between micro-operation hand and chip upper surface is 10 to 45 ° (works fine angles of micro-operation hand).
(3) position that there is electrode in micro-operation hand needle point to saturating electron beam elongated slot both sides branch is moved along saturating electron beam elongated slot direction, because micro-operation hand needle point place diameter is only several microns, be less than the width of electron beam elongated slot 10 μm, so the height that can reduce micro-operation hand needle point makes needle point pass from saturating electron beam elongated slot.Traditional die only has circle or ellipse hole due to film window region or does not offer through hole and uses the silicon nitride film of below 50nm through electron beam, micro-operation hand needle point therefore cannot be allowed to pass through, so micro-operation hand cannot be used to complete the transfer of sample.
(4) be attached to nano wire sample on micro-operation hand needle point due to length be greater than electron beam elongated slot width will stop by saturating electron beam elongated slot, thus stay on the electrode of chip, be connected with chip by Van der Waals force.
(5) sample is loaded specimen holder, transmission electron microscope can be entered and carry out home position observation and test.
Embodiment 3
A kind of nano material transmission electron microscope original position electrical testing chip of the present embodiment and preparation method thereof, basic with embodiment 1, its difference is: in the present embodiment, silicon chip thickness is 200 μm, metal electrode is positioned at the part on film window and distributes along the both sides of saturating electron beam elongated slot, the length of saturating electron beam elongated slot is 320 μm, and width is 8 μm.The thickness of metal electrode is 200nm, and in insulation course, the thickness of silicon dioxide layer is 1000nm, and the thickness of silicon nitride layer is 150nm.
Embodiment 4
A kind of nano material transmission electron microscope original position electrical testing chip of the present embodiment and preparation method thereof, basic with embodiment 1, its difference is: in the present embodiment, silicon chip thickness is 300 μm, electron beam elongated hole is had in film window, metal electrode is positioned at the part on film window and distributes along the side of saturating electron beam elongated hole, the length of saturating electron beam elongated hole is 400 μm, and width is 20 μm.The thickness of metal electrode is 150nm, and in insulation course, the thickness of silicon dioxide layer is 800nm, and the thickness of silicon nitride layer is 120nm.
Embodiment 5
A kind of nano material transmission electron microscope original position electrical testing chip of the present embodiment and preparation method thereof, basic with embodiment 1, its difference is: have electron beam elongated hole in film window in the present embodiment, the length of saturating electron beam elongated hole is 100 μm, width is 5 μm, in insulation course, the thickness of silicon dioxide layer is 900nm, and the thickness of silicon nitride layer is 160nm.
Embodiment 6
A kind of nano material transmission electron microscope original position calorifics test chip of the present embodiment and preparation method thereof, basic with embodiment 1, its difference is: in the present embodiment, silicon chip thickness is 200 μm, on film window, growth has silit (SiC) layer that one deck 50nm is thick, the present embodiment (is specially on film window) growth one deck silit (SiC) film on the insulating layer, because silit (SiC) is semiconductor, it is made to generate heat by providing electric current, so can heat the superincumbent sample of placement, and change heating-up temperature by adjusting the size of current inputing to carborundum films, for heating sample.
Schematically above be described the present invention and embodiment thereof, this description does not have restricted, and also just one of the embodiments of the present invention shown in accompanying drawing, actual structure is not limited thereto.So, if those of ordinary skill in the art enlightens by it, when not departing from the invention aim, designing the frame mode similar to this technical scheme and embodiment without creationary, all should protection scope of the present invention be belonged to.
Claims (8)
1. a nano material transmission electron microscope in-situ test chip, comprise silicon chip and insulation course, it is characterized in that: also comprise film window (3), described silicon chip two sides is provided with insulation course, and silicon chip front offers the film window (3) be made up of insulation course, have electron beam elongated hole or saturating electron beam elongated slot in film window (3), the width of described saturating electron beam elongated hole or thoroughly electron beam elongated slot is 5-20 μm; The insulation course in described silicon chip front is provided with metallic film or device, or semiconductor function film or device.
2. a kind of nano material transmission electron microscope in-situ test chip according to claim 1, is characterized in that: the length of described saturating electron beam elongated hole or thoroughly electron beam elongated slot is 100-400 μm.
3. a kind of nano material transmission electron microscope in-situ test chip according to claim 2, it is characterized in that: described insulation course comprises the silicon dioxide layer grown on a silicon substrate and the silicon nitride layer grown on silicon dioxide layer, the thickness of silicon dioxide layer is 200-1000nm, and the thickness of silicon nitride layer is 5-200nm.
4. a kind of nano material transmission electron microscope in-situ test chip according to claim 3, is characterized in that: described metallic film or device, semiconductor function film or device are positioned at the one or both sides distribution along saturating electron beam elongated hole or electron beam elongated slot thoroughly of part on film window (3).
5. a kind of nano material transmission electron microscope in-situ test chip according to claim 4, is characterized in that: described silicon chip thickness is 100-400 μm.
6. a preparation method for the nano material transmission electron microscope in-situ test chip as described in any one of Claims 1 to 5, the steps include:
Step one, prepare two sides with the silicon chip of silicon dioxide layer, in silicon chip two sides grown silicon nitride layer;
Step 2, utilize photoetching process, electrode pattern is transferred to step one gained silicon chip front from lithography mask version;
Step 3, utilize micro-electromechanical processing technology, produce metallic film or device in step 2 gained silicon chip front, or semiconductor function film or device;
Step 4, utilize photoetching process and reactive ion etching process, the insulation course at the step 3 gained silicon chip back side etches a square window (1), and this square window (1) is positioned on the axis of silicon chip;
Step 5, utilize photoetching process and reactive ion etching process, the insulation course in step 4 gained silicon chip front etches electron beam elongated hole or electron beam elongated slot thoroughly;
Step 6, step 5 gained silicon chip is put into potassium hydroxide solution carry out wet etching, until etch into the silicon dioxide layer in silicon chip front thus leave film window (3), take out silicon chip cleaning;
Step 7, step 6 gained silicon chip is carried out scribing, be divided into individual chips.
7. the application of a nano material transmission electron microscope in-situ test chip, it is characterized in that: use micromanipulator place sample or utilize focused ion beam system to process and place sample on test chip, make the metallic film on sample and chip or device, or semiconductor function film or device are connected, and be positioned at film window (3) region saturating electron beam elongated hole or thoroughly on electron beam elongated slot; The test chip being loaded with sample is loaded in specimen holder and sends into transmission electron microscope and observe, physics, chemical action receive the signal that sample produces are applied to sample, to sample carry out atomic scale differentiate under home position observation.
8. the application of a kind of nano material transmission electron microscope in-situ test chip according to claim 7, is characterized in that: the transfer that in-situ test chip completes sample with fixing after in ion milling equipment, Ion Cleaning and thinning can be carried out to sample.
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