CN217717561U - Transmission electron microscope in-situ gas phase temperature difference chip - Google Patents
Transmission electron microscope in-situ gas phase temperature difference chip Download PDFInfo
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- CN217717561U CN217717561U CN202220334196.8U CN202220334196U CN217717561U CN 217717561 U CN217717561 U CN 217717561U CN 202220334196 U CN202220334196 U CN 202220334196U CN 217717561 U CN217717561 U CN 217717561U
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Abstract
The utility model provides a transmission electron microscope in-situ gas phase temperature difference chip, which comprises an upper chip and a lower chip; the periphery between the upper chip and the lower chip is sealed to form a hollow cavity; in the hollow cavity, the upper surface of the lower chip is provided with a gas outlet, a first heating area, a second heating area, a third heating area and a gas inlet which are sequentially arranged in a straight line shape; an observation window is arranged in any heating zone, an electron beam window penetrating through the lower chip is arranged below the observation window, a lower thin film window is arranged in the electron beam window, and an upper thin film window corresponding to the lower thin film window is arranged in the upper chip. The transmission electron microscope in-situ gas phase temperature difference chip is accurate in heating temperature control, successfully coupled with a high-pressure gas field, capable of realizing loading of accurate temperature gradient by jointly heating a plurality of heating zones, capable of controlling quick response of temperature and capable of carrying out high-resolution measurement of in-situ reaction on a transmission electron microscope sample under gas-heat double loads.
Description
Technical Field
The utility model belongs to the technical field of the material performance normal position test, concretely relates to transmission electron microscope normal position gaseous phase difference in temperature chip.
Background
Conventional transmission electron microscopes can only obtain corresponding structural information within a fixed period of time. The actual reaction conditions are a prerequisite for in situ studies. In-situ transmission electron microscopy provides possibility for simulating industrial conditions of materials under the condition of keeping high resolution, and researchers can obtain important information such as crystal size, morphology, crystal structure, chemical bonds, heat energy change and the like through in-situ transmission electron microscopy introducing an air field and a temperature field for in-situ testing. In the research of catalysis, oxidation and nano-growth, the external environment influences the atomic structure on a micro scale to cause macroscopic performance difference. In-situ Transmission Electron Microscopy (TEM) has been widely accepted in the fields of nanomaterial synthesis, catalysis, metal corrosion, and even energy materials as a powerful tool for direct observation of morphological and structural changes at atomic scale.
At present, methods for carrying out in-situ characterization in a gas-thermal environment mainly include an Environmental Transmission Electron Microscope (ETEM) and a gas chip based on an MEMS chip technology. The environmental transmission electron microscope is additionally provided with a set of differential pumping system by changing the structure of the original electron microscope, and the introduction of gas with proper flow is allowed. In the in-situ chip technology, the high-pressure gas is isolated from the cavity of the electron microscope through the assembly of the upper chip and the lower chip, so that the introduction of a thermal field or a gas field can be realized, and the in-situ chip technology has the advantages of small volume and high integratability.
However, existing ambient transmission electron microscopy allows gas pressures not exceeding 15.0 torr (0.02 atm), about two orders of magnitude lower than atmospheric pressures at which many practical gas phase reactions occur. This "pressure differential" does not facilitate bridging between in situ results and actual application; meanwhile, the differential pumping aperture blocks high-angle scattered electrons, and STEM imaging of the high-angle scattered electrons is influenced.
The existing gas chip can only realize single gas loading, and cannot provide a thermal field for an experiment to reduce the reaction barrier; the existing heating chip is difficult to realize the loading of the temperature gradient, the temperature response rate is slow, although the in-situ temperature difference chip developed by Liaohong and other people can realize the temperature gradient to a certain extent, the chip is not coupled with the air field, and the carried sample is single; the existing gas heating chip, such as a transmission electron microscope in-situ gas heating chip developed by J.Fredrk Creemer and the like, is limited to a uniform temperature field, cannot load a temperature gradient, realizes in-situ temperature difference observation and the like although coupling of gas and a thermal field is realized.
As the most extensive application of the combination of gas and temperature gradient, a material forming mechanism synthesized by CVD or CVT is not clear up till now, the synthesis process is still a black box, but the research on in-situ synthesis of two-dimensional materials under the current atmosphere is few, and although a macroscopic tube furnace can complete the synthesis of related materials, the yield is low, so that the method is not suitable for large-scale preparation; microscopically albeit Christian
The introduction of a low pressure of CVD precursor gas disilane into a conventional planar heated TEM substrate with deposited catalyst in ETEM completes the growth of Si nanowires under a temperature gradient, but is not applicable to other materials.
Meanwhile, the synthesis of the two-dimensional material is accompanied by the formation of byproducts, and because the temperature of the micro-area of the heat treatment furnace is difficult to control, great difficulty is caused for product collection, products and byproducts, products and reactants, and byproducts and reactants are generated and mixed in the same area, great trouble is caused for material preparation, and the problems especially become the technical development bottleneck of the two-dimensional material. For example, in the experiment of the mineralization method of black phosphorus, impurities such as metal phosphide or phosphorus allotrope are easy to generate, so that three temperature zones need to be arranged in the experiment of black phosphorus growth, wherein HT zone, MT zone and LT zone respectively represent a high temperature zone, a medium temperature zone and a low temperature zone, wherein the high temperature zone is a load zone of a precursor, and the temperature is generally set to be 600 ℃ in the experiment so as to promote the volatilization of the precursor; the substrate is placed in a medium-temperature area for growing black phosphorus; and a large amount of phosphorus vapor flows from the high-temperature area to the low-temperature area and is deposited in the low-temperature area due to the driving of the temperature gradient, and byproducts such as red phosphorus, white phosphorus and the like are further formed. Therefore, the existing gas heating chip is needed to be improved, a temperature gradient loading in the atmosphere can be realized in situ, the in-situ growth of the two-dimensional/nano material can be realized, and meanwhile, the high-efficiency separation and collection of the product and the by-product can be realized through the regulation and control of the temperature zone gradient.
SUMMERY OF THE UTILITY MODEL
The utility model provides a transmission electron microscope normal position gas phase difference in temperature chip can carry out the high resolution measurement of normal position reaction to the transmission electron microscope sample under gas heat dual load.
Particularly, the utility model provides a following technical scheme:
a transmission electron microscope in-situ gas phase temperature difference chip comprises an upper chip and a lower chip; the periphery between the upper chip and the lower chip is sealed to form a hollow cavity;
in the hollow cavity, the upper surface of the lower chip is provided with a gas outlet, a first heating area, a second heating area, a third heating area and a gas inlet which are sequentially arranged in a straight line shape;
an observation window is arranged in any heating zone, an electron beam window penetrating through the lower chip is arranged below the observation window, a lower thin film window is arranged in the electron beam window, and an upper thin film window corresponding to the lower thin film window is arranged in the upper chip.
Preferably, in the transmission electron microscope in-situ gas phase temperature difference chip, the heating wire of the first heating zone is spiral ring-shaped or disc-shaped; the heating wires of the second heating area and the third heating area are in a snake shape. In a more preferred embodiment, the first heating zone may be set as a high temperature zone for carrying the raw material, so that the heating wire thereof is set as a spiral ring or a disc for better temperature concentration and control, while the second heating zone (middle temperature zone) and the third heating zone (low temperature zone) are by-product and/or product collecting zones, so as to ensure a larger temperature coverage area, and thus the heating wire is set as a serpentine shape running back and forth to ensure the product collecting efficiency of the middle temperature zone and the low temperature zone.
Preferably, in the in-situ gas phase temperature difference chip for the transmission electron microscope, the outer diameter of the spiral annular or disc-shaped heating wire of the first heating zone is 150 to 220 μm; the shape of the serpentine heating wire of the second heating zone has dimensions of (140-250) μm (axial x transverse); the serpentine heating filament shape of the third heating zone has dimensions of (140-250) μm (axial x lateral). The axial direction is parallel to the gas outlet, the first heating area, the second heating area, the third heating area and the gas inlet which are sequentially arranged in a straight line shape, and the transverse direction is vertical to the axial direction.
Further preferred, the first heating zone size is 180-200 μm in diameter, the second heating zone size is (140-160) μm (180-220) μm (axial x transverse), and the third heating zone size is (170-190) μm (180-220) μm (axial x transverse).
Preferably, in the in-situ gas phase temperature difference chip for the transmission electron microscope, a distance between the first heating region and the second heating region is 140 to 160 μm, and a distance between the second heating region and the third heating region is 140 to 160 μm. In a more preferred embodiment, the adjacent heating zones are all 150 μm apart from each other, which in the temperature field simulation results in a temperature reduction of 100 ℃ for the subsequent temperature requirements.
Preferably, in the above-mentioned tem in-situ gas phase temperature difference chip, the sum of the axial dimensions of the three heating zones is limited within 1mm (the limitation requirement of the field of view of the tem).
Preferably, in the transmission electron microscope in-situ gas phase temperature difference chip, any one of the heating zones is composed of a heating wire with an outer diameter of 2-15 μm. In a more preferred embodiment, the first heating zone is a high temperature zone, the outer diameter of the heater is 6 μm for the inner zone (the inner zone is preferably 1-2 turns from the center outwards), the outer zone is 8 μm, the spacing between adjacent heater zones is 8 μm, the second heating zone is a medium temperature zone, the outer diameter of the heater is 10 μm, the spacing between adjacent heater zones is 12 μm, the third heating zone is a low temperature zone, also the important product collection zone, the outer diameter of the heater zones is 12 μm, and the spacing between adjacent heater zones is 14 μm. (the smaller the outer diameter of the heating wire, the smaller the distance, the higher the heating temperature, the main reason is that the heating wire is more densely distributed and the heat dissipation is smaller)
Preferably, in the transmission electron microscope in-situ gas phase temperature difference chip, the observation window is arranged in the center of the heating area or in the gap of the heating wire.
Preferably, in the in-situ gas-phase temperature difference chip for the transmission electron microscope, any one of the heating zones is respectively connected with one group of pressurizing electrodes and one group of temperature measuring electrodes.
Preferably, in the transmission electron microscope in-situ gas phase temperature difference chip, the height of the hollow cavity is 1-6 μm.
Preferably, in the transmission electron microscope in-situ gas phase temperature difference chip, the upper surface of the lower chip is further provided with concave gas path gaskets, the gas outlet and the gas inlet are respectively arranged in the concave parts of the two concave gas path gaskets, the open ends of the two concave gas path gaskets are oppositely arranged, so that a gas gathering effect can be achieved, and the gas flow rate and the flow rate can be adjusted through adjusting the reaction speed.
Preferably, in the transmission electron microscope in-situ gas phase temperature difference chip, the height of the two concave gas path gaskets is 100-5000nm.
The utility model provides an above-mentioned transmission electron microscope normal position gas phase difference in temperature chip can realize temperature gradient's loading through the coupling in many heating areas, and the temperature value in every temperature field is more even simultaneously to but independent control, each other do not influence. The characterizable sample can be a nanoparticle, a nanowire or a bulk sample carried by a focused ion beam, and a controllable temperature gradient can be provided to realize in-situ growth of the nanowire or the nano-sheet material. Various deposition and synthesis reactions depending on temperature gradient control are carried out, such as film preparation of various depositions and synthesis of two-dimensional materials, the synthesis mechanism in the two-dimensional material synthesis process is explored, and the action behaviors of various factors such as temperature, atmosphere, pressure and the like on the synthesis are explored.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in 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 for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is the utility model discloses transmission electron microscope normal position gaseous phase difference in temperature chip structure sketch map.
Fig. 2 is a top view of the lower chip according to the embodiment of the present invention.
Fig. 3 is a top view of the upper chip according to the embodiment of the present invention.
Fig. 4 is a top view of three heating zones according to an embodiment of the present invention.
Fig. 5 is a schematic structural diagram of a first heating zone according to an embodiment of the present invention.
Fig. 6 is a schematic structural diagram of a second heating zone according to an embodiment of the present invention.
Fig. 7 isbase:Sub>A cross-sectional view ofbase:Sub>A lower chipbase:Sub>A-base:Sub>A according to an embodiment of the present invention.
Fig. 8 is a cross-sectional view of the lower chip B-B according to an embodiment of the present invention.
In the figure: 1. mounting a chip; 2. a chip is put down; 3. a gas pipeline 3-1 and a gas outlet; 3-2, an air inlet; 4. a concave gas path gasket; 5. a heating zone; 5-1, a first heating zone; 5-2, a second heating zone; 5-3, a third heating zone; 6. a lead; 7. a conductive sheet; 8. an isolation layer 9, a heating layer 10 and a support layer; 11. a silicon substrate; 12. a lower silicon nitride film window; 13. a heating wire; 14. an upper silicon nitride film window; 15. sample particles; 16. an observation window; 17. an electron beam window.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
The embodiment of the utility model provides a transmission electron microscope normal position gas phase difference chip need combine transmission electron microscope in order to accomplish the normal position growth and the microscopic structure evolution of normal position observation sample.
Realize room temperature to 1300 ℃ temperature field control in stable atmosphere and controllable pressure in order to realize the sample to obtain normal position atomic resolution image and image, as shown in fig. 1-8, the embodiment of the utility model provides an in situ gas hot difference in temperature chip is formed by lower chip 2 and the combination of last chip 1.
The embodiment of the utility model provides an in, arrange this transmission electron microscope normal position gas phase difference in temperature chip cooperation sample pole in transmission electron microscope, accomplish the alignment of upper and lower chip and with the collocation of sample pole earlier stage in the alignment instrument, adjust temperature and gas flow parameter to stable and guarantee best observation state in the electron microscope. The transmission electron microscope in-situ gas phase temperature difference chip can realize high temperature response rate, high thermal uniformity, adjustable temperature gradient and gas flow rate, can realize atom scale resolution gas-solid reaction experiment under 2atm, and reveals the gas-solid reaction principle.
The embodiment of the utility model provides a transmission electron microscope in-situ gas phase temperature difference chip, as shown in figure 1, which comprises an upper chip 1 and a lower chip 2 which are sequentially connected from top to bottom; the upper chip and the lower chip are divided into a front surface and a back surface, wherein the combination of the upper chip and the lower chip is fixed and sealed through a sealing O ring or filled with a proper amount of sealant, and a small amount of vacuum sealant is coated at the connecting seams of the upper chip 1 and the cover plate and the lower chip 2 and the sample rod substrate for fixing and sealing according to the situation.
The embodiment of the utility model provides a transmission electron microscope normal position gas phase difference in temperature chip, as shown in fig. 2, lower chip 2's surface is equipped with 3-1 gas outlets, the first zone of heating 5-1, the second zone of heating 5-2, the third zone of heating 5-3 and air inlet 3-2 that are the in-line and arrange in proper order, and wherein, the first zone of heating 5-1, the second zone of heating 5-2, the third zone of heating 5-3 constitute zone of heating 5 jointly. Any heating zone adopts a four-electrode method to measure temperature, a pair of pressurizing electrodes and a pair of measuring electrodes are respectively connected through leads 6, the pressurizing electrodes are responsible for providing voltage required by heating, and the measuring electrodes detect the actual temperature generated by the heating zone by measuring real-time voltage in the heating process. The power of the resistance wire 13 in the heating zone 5 is precisely controlled by the application of an external potential to the conducting strip 7 to achieve precise control of the sample temperature. The lead 6 adopts the symmetrical design, has further got rid of the temperature measurement error that lead resistance change brought, improves the temperature measurement precision. The three heating zones are distributed on the same axis and respectively correspond to four electrodes for control, so that not only can a uniform temperature field be realized, but also different voltages can be applied through three sets of systems, different temperatures can be provided at the heating zones, and a macroscopic temperature field required by life of the two-dimensional material/nano material is generated.
As shown in fig. 2, the upper surface of the lower chip 2 is further provided with two concave gas path gaskets 4, the gas outlet 3-1 and the gas inlet 3-2 are respectively arranged in the concave portions of the two concave gas path gaskets 4, the open ends of the two concave gas path gaskets 4 are oppositely arranged, and gas sequentially passes through a flow channel formed by the gas outlet 3-1 and the concave gas path gaskets 4, the gas inlet 3-2 and a communicating gas path inside the sample rod.
The embodiment of the utility model provides a pair of transmission electron microscope normal position gaseous phase difference in temperature chip, as shown in FIG. 4, the first zone of heating 5-1 is the high temperature region, and the shape is the disc type, more does benefit to the concentration and the control of temperature, and the second zone of heating 5-2, the third zone of heating 5-3 are accessory substance, result collecting region respectively, need to guarantee to have bigger temperature coverage area, therefore set up to the snakelike of reciprocating the line of walking to the result collection efficiency of temperature and low temperature district in guaranteeing. The adjacent heating zones are all 150 μm apart from each other along the edge.
As shown in fig. 5, the outer diameter of the disc-shaped heater shape of the first heating zone 5-1 is 200 μm, the outer diameter of the heater is 6 μm for the inner coil (2 coils from the center) and 8 μm for the outer coil, and the interval between the adjacent heaters is 8 μm. The method meets the requirement of temperature uniformity in the region while ensuring higher temperature, the temperature uniformity in the annular range reaches more than 99.5%, and after the Si back bottom matched with the temperature uniformity is etched, the thermal mass of a heating region is reduced, so that the heating power is reduced, the thermal drift is reduced, and the image stability under atomic scale resolution is ensured. The first heating zone 5-1 is centrally provided with a viewing window 16.
As shown in fig. 6, the second heating zone is an intermediate temperature zone, the size of the shape of the serpentine heating wire is 150 μm by 200 μm (axial by lateral), the outer diameter of the heating wire is 10 μm, and the distance between adjacent heating wires is 12 μm. An observation window 16 is arranged in the gap of the heating wire of the second heating area 5-2.
The third heating zone is a low temperature zone and also an important product collecting zone, the shape of the serpentine heating wire has the size of 180 mu m by 200 mu m (axial direction by transverse direction), the outer diameter of the heating wire is 12 mu m, and the distance between adjacent heating wires is 14 mu m. An observation window 16 is arranged in the gap of the heating wires of the third heating area 5-3.
The embodiment of the utility model provides a pair of transmission electron microscope normal position gaseous phase difference in temperature chip, as shown in fig. 7 and fig. 8, lower chip 1 is by supreme silicon substrate 11, supporting layer 10, zone of heating 9 and isolation layer 8 of being in proper order down, zone of heating 9 includes zone of heating 5 and lead wire 6 to connect through conducting strip 7 and external circuit, isolation layer 8 is used for separating zone of heating 9 and sample granule, external atmosphere, avoids the heater strip by oxidation or the short circuit appears. An electron beam window 17 penetrating through the lower chip 2 is arranged below the heating area 5 in the heating layer 9, and a lower silicon nitride film window 12 is arranged in the electron beam window 17. And a gas pipeline 3 penetrating through the lower chip 2 is arranged below the gas outlet 3-1 and the gas inlet 3-2.
As shown in fig. 3, an upper silicon nitride film window 14 corresponding to the lower silicon nitride film window 12 is formed in the upper chip 1.
The embodiment of the utility model provides a pair of transmission electron microscope normal position gas phase difference chip adopts upper and lower double-deck silicon nitride film window, and the last silicon nitride film window 14 of upper chip 1 aligns with the zone of heating 5 of lower chip 2, and the upper surface passes through O type sealing washer after aiming at, and the alignment compresses tightly among the gaseous sample pole of transmission electron microscope, and this greatly reduces electron beam direction gas content, guarantees that the electron beam can not too much scattered by gas, presents higher-quality electron map when seeing through the sample.
The preparation method of the lower chip 1 of the transmission electron microscope in-situ gas phase temperature difference chip provided in this embodiment is explained in detail:
s1, preparing a wafer A which is polished on two sides and is grown with a monocrystalline Si (100) of a silicon nitride or silicon oxide insulating layer, wherein the thickness of the insulating layer is 10nm-1 mu m, and the thickness of a silicon wafer is 100 mu m-1mm;
and S2, transferring the SiNx observation window film pattern to the front surface of the wafer A through low-pressure chemical vapor deposition, photoetching and dry etching processes. Obtaining a wafer A-1;
s3, growing a metal layer on the front surface of the wafer A-1 by utilizing a magnetron sputtering growth technology, transferring a heating resistor pattern from a photoetching mask plate to the front surface of the wafer through photoetching and etching, developing in a positive photoresist developing solution, and cleaning the surface by using deionized water to form a heating resistor and a lead. Obtaining a wafer A-2;
and S4, growing a layer of silicon nitride on the front surface of the wafer A-2 by an LPCVD process to serve as a protective layer. Obtaining a wafer A-3; (SIN protective layer)
S5, depositing a layer of silicon oxide or polycrystalline silicon on the front surface of the wafer A-3 through a PECVD (plasma enhanced chemical vapor deposition) process, transferring a gas circuit pattern from a photoetching mask to the front surface of the wafer by adopting a photoetching process, developing in a positive photoresist developing solution, cleaning the surface by using deionized water, and etching to form a gas channel to obtain the wafer A-4; (deposition of gas channel)
S8, transferring the graph of the area to be etched from the photoetching mask plate to the front side of the wafer A-5 through a photoetching process, developing in positive photoresist developing solution, sequentially cleaning with organic cleaning and deionized water, and removing residual photoresist on the surface by adopting plasma to obtain a wafer A-6; (exposure of detail bonding area)
S9, evaporating a layer of metal film on the front surface of the wafer A-6 by using an electron beam evaporation coating process to form a heating electrode. Placing the wafer with the right side facing upwards into acetone for soaking and stripping, washing with deionized water, removing the photoresist, and leaving a metal electrode to obtain a wafer A-7; (deposition of electrode)
S10, etching silicon nitride or silicon oxide on a region to be etched on the back of the wafer A-7 by using a reactive ion etching process, sequentially putting the wafer with the back facing upwards into acetone for soaking, finally washing with acetone, and removing photoresist to obtain a wafer A-8; (removal of protective back layer)
S11, placing the wafer A-8 with the back face upward into a water bath for wet etching until etching of the substrate silicon of the corresponding window part is completed, taking out the wafer, and cleaning the photoresist to obtain a wafer A-9; (bottom silicon etching)
S12, etching away a silicon nitride or silicon oxide or aluminum oxide protective layer exposed on the front side of the wafer A-9 through a reactive ion etching process, then placing the wafer with the front side facing upwards into acetone for soaking, finally washing with acetone, and removing photoresist to obtain a wafer A-10; (air inlet and outlet port window)
S13, carrying out laser or mechanical scribing on the wafer A-10 to divide the wafer into independent chips.
The embodiment of the utility model provides a transmission electron microscope normal position gas phase difference chip combines concrete experiment "mineralization method normal position preparation black phosphorus", and its assembly and test process can include following step:
wherein, the synthetic raw material for preparing the black phosphorus in situ by the mineralization method is high-purity tin and high-purity red phosphorus I2. The involved reaction equations include:
Sn(s)→Sn(g)+Sn(l)
Sn+I2→SnI4or Sn + I2→SnI2
SnI4→SnI2+I2
RP→P4(g)
s is solid, l is liquid, g is gaseous, wherein the by-products involved include SnI2，SnI4Purple phosphorus and red phosphorus. The experimental principle is that high-purity tin and high-purity red phosphorus are mixed and dispersed at the 5-1 part of the high-temperature area of the chip, the reaction raw material is sublimated by heating, and I is introduced2The gas, carrying sublimed substance by reaction gas, enters a middle temperature region 5-2, and by-product SnI is carried out in the middle temperature region by adjusting and controlling temperature2，SnI4And collecting purple phosphorus and red phosphorus, and observing while synthesizing black phosphorus in the low-temperature region 5-3.
Step S1: red phosphorus (RP, the purity is more than 99.999%) and tin particles (Sn, the purity is more than 99.999%) in the raw materials used for the experiment are uniformly mixed by absolute ethyl alcohol, are dripped into a heating area 5-1 of a lower chip 2, and are dried by a hot table to be stably attached to the surface of the chip;
step S2: placing the lower chip 2 in the groove of the sample rod to enable the length direction of the electron beam window to be parallel to the axial direction of the sample rod;
and step S3: assembling an O-shaped sealing ring on the lower chip 2, and symmetrically assembling the O-shaped sealing ring on the outer edge of the heating area;
and step S4: the surface of a lower chip 2 carrying a sample is horizontally placed under a light mirror, and an upper chip 1 and the lower chip 2 are centered, so that a sample carrying area of the lower chip 2 is aligned with an upper silicon nitride film window 14 of the upper chip;
step S5: checking whether an upper silicon nitride film window 14, a sample and a lower silicon nitride film window 12 of the upper chip 1 are aligned under a light mirror, and carrying out fine adjustment;
step S6: covering the pressing plate and fixing the pressing plate by fastening screws;
step S7: carrying out electrical connection test;
step S8: introducing Ar gas through a gas channel and a gas valve of the sample rod, and performing vacuum leakage detection in a light mirror and an He mass spectrometer leak detector;
step S9: after vacuum leakage detection is carried out, the gas sealing is confirmed to be good, and then the sample rod is inserted into a transmission electron microscope;
step S10: introducing a circulating gas I2Opening the electron beam after confirming that the vacuum of the transmission electron microscope is good, finding a sample on an electron beam window, and adjusting to a proper multiple;
step S11: after an electrical control system is connected, a heating wire 13 on a lower chip 2 is electrified and heated, a first heating zone 5-1 is gradually heated and kept above the sublimation temperature of red phosphorus (650 ℃), the temperature of a second heating zone 5-2 is controlled at 620-500 ℃ (the collection temperature of byproduct purple phosphorus and red phosphorus), and the temperature of a third heating zone 5-3 is controlled at 400-500 ℃, so that the optimal temperature for the growth of black phosphorus is provided, the simultaneous loading of gas and a thermal field is completed, and different voltages can be simultaneously electrified in a plurality of heating zones to meet the loading of temperature gradients between the heating zones;
step S12: the solid red phosphorus particles are sublimated into gas particles in the first heating zone 5-1 by the loading of the temperature gradient, and the reaction gas I2Under the load, the collection of red phosphorus and purple phosphorus byproducts is completed in the second heating area 5-2, the in-situ deposition and growth of black phosphorus are completed in the third heating area 5-3, and real-time observation is carried out to reveal the growth mechanism in the growth process of the black phosphorus.
Although the invention has been described in detail in the foregoing by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that certain modifications and improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of this invention without departing from the spirit thereof.
Claims (10)
1. A transmission electron microscope in-situ gas phase temperature difference chip is characterized by comprising an upper chip and a lower chip; the periphery between the upper chip and the lower chip is sealed to form a hollow cavity;
in the hollow cavity, the upper surface of the lower chip is provided with a gas outlet, a first heating area, a second heating area, a third heating area and a gas inlet which are sequentially arranged in a straight line shape;
an observation window is arranged in any heating area, an electron beam window penetrating through the lower chip is arranged below the observation window, a lower film window is arranged in the electron beam window, and an upper film window corresponding to the lower film window is arranged in the upper chip.
2. The TEM in-situ gas phase temperature difference chip as claimed in claim 1, wherein the heating wire of the first heating zone is in the shape of a spiral ring or a disc; the heating wires of the second heating area and the third heating area are in a snake shape.
3. The TEM in-situ gas phase temperature difference chip as claimed in claim 2, wherein the outer diameter of the spiral ring-shaped or disc-shaped heating wire shape of the first heating zone is 150-220 μm; the shape of the serpentine heating wire of the second heating zone has dimensions of (140-250) μm; the shape of the serpentine heating wire of the third heating zone has a size of (140-250) μm.
4. The TEM in-situ gas-phase thermoelectric chip as claimed in any one of claims 1 to 3, wherein the first and second heating regions are spaced apart from each other by 140-160 μm, and the second and third heating regions are spaced apart from each other by 140-160 μm.
5. The transmission electron microscope in-situ gas phase temperature difference chip according to any one of claims 1 to 3, wherein any one of the heating zones is composed of heating wires with the outer diameter of 2-15 μm, and the distance between every two adjacent heating wires is 5-15 μm.
6. The TEM in-situ gas phase temperature difference chip as claimed in any one of claims 1-3, wherein the observation window is arranged in the center of the heating zone or in the gap of the heating wire.
7. The TEM in-situ gas-phase thermoelectric chip as claimed in any one of claims 1-3, wherein any one of the heating zones is connected to a set of pressurizing electrodes and a set of temperature measuring electrodes, respectively.
8. The TEM in-situ gas-phase thermoelectric chip as claimed in any one of claims 1 to 3, wherein the hollow cavity has a height of 1-6 μm.
9. The TEM in-situ gas phase temperature difference chip as claimed in any one of claims 1-3, wherein the upper surface of the lower chip is further provided with concave gas path gaskets, the gas outlet and the gas inlet are respectively arranged in the concave portions of the two concave gas path gaskets, and the open ends of the two concave gas path gaskets are oppositely arranged.
10. The TEM in-situ gas-phase temperature difference chip as claimed in claim 9, wherein the two concave gas path gaskets have a height of 100-5000nm.
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2022
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