CN113189123B - Observation micro-area positioning method based on internal standard substance microarray - Google Patents
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Abstract
The invention discloses an observation micro-area positioning method based on an internal standard substance microarray, which comprises the following steps: dispersing a powdery sample to be observed in a solvent to prepare a solution, and dripping the solution on a heating chip special for a transmission electron microscope; placing a chip carrying a sample to be observed on a metal table, fixing the edge of the chip on the metal table, fixing the metal table carrying the chip in an FIB-SEM dual-beam system, and determining the position of the sample to be observed on the chip under an electron beam window; directionally depositing metal tungsten I at the contact position of the sample and the chip under an ion beam window, and fixing the sample; depositing metal tungsten II directionally along the periphery of the sample under a chip observable window, and forming an internal standard substance microarray at the periphery of the sample; loading the marked chip to a transmission electron microscope in-situ heating sample rod, selecting an observation micro-area, and recording the structure and component information of the sample by image acquisition and energy spectrum technology; taking out the chip, putting the chip into a reactor, and starting a specific reaction; and after the reaction is finished, taking out the chip, reloading the chip to a transmission electron microscope in-situ heating sample rod, positioning and navigating the chip to the selected observation micro-area through an internal standard substance microarray, and observing the structure and component changes of the sample after the reaction in the observation micro-area through image acquisition and energy spectrum technology.
Description
Technical Field
The invention relates to an observation micro-area positioning method based on an internal standard substance microarray.
Background
The rapid development of transmission electron microscope and its peripheral technology, especially the spherical aberration electron microscope and in-situ electron microscope technology, provides possibility for observing the fine structure and dynamic change process of nanometer material at molecular/atomic layer. Researchers can track and observe the structure evolution process of a series of nano catalytic materials in the high-temperature heating process on a transmission electron microscope in-situ heating sample rod, more direct image information is provided for the thermal diffusion mechanism of metal particles in the catalyst sintering process, and the method has great significance for guiding the synthesis of novel thermal stable catalytic materials. In fact, tracking the high resolution and dynamic change process of materials under the action of preparation, reaction or other external field factors is a direct evidence and important way to analyze key scientific problems such as formation mechanism and reaction mechanism of related materials. However, due to the environmental and parameter requirements of the tem chamber and the sample rod, it is impossible to simulate all physical and chemical environments during the testing process, especially the coexistence of multiple and multi-phase reactants. Thus, many important material inactivation mechanisms and reaction mechanisms are not well defined. In order to more truly study the dynamic process of the nano material under the actual chemical reaction-oriented service condition, a researcher loads gold nanoparticles on the surface of a transmission electron microscope carrier net, directly places the gold nanoparticles into a CO oxidation reactor, and counts the direct information of the sizes of the nanoparticles before and after the actual reaction, thereby tracking the thermal diffusion process. However, after the grid-carrying is transferred, the accurate resetting of the original observation position is difficult, and especially for nano materials (such as fiber materials) with highly symmetrical overall shapes, the original observation micro-area cannot be traced back by the shape characteristics of the sample per se, and the important structure and component change information of the specific micro-area can be traced, so that the application of the transmission electron microscope technology in deep analysis of related micro-mechanism research at the atom/molecule level is hindered.
Disclosure of Invention
The purpose of the invention is as follows: the invention provides an observation micro-area positioning method based on an internal standard substance micro-array, aiming at the problems that in the prior art, when the direct information of the sizes of nano particles on the atom/molecule layer before and after reaction is researched by utilizing a transmission electron microscope technology, the accurate resetting of an original observation position is difficult after a carrier net is transferred, and the nano materials with highly symmetrical overall shapes cannot backtrack the original observation micro-area by the shape characteristics of the sample, and the method can effectively prevent the displacement of the sample loaded on the carrier net surface under the action of an external field on one hand, and can realize the accurate resetting of the original observation position after the carrier net is transferred on the other hand, and the problem that the nano materials with highly symmetrical overall shapes cannot backtrack the original observation micro-area by the shape characteristics of the sample on the other hand.
The technical scheme is as follows: the invention relates to an observation micro-area positioning method based on an internal standard substance microarray, which comprises the following steps:
(1) Dispersing a powdery sample to be observed in a solvent to prepare a uniform solution, and dripping the solution on a special heatable chip for a transmission electron microscope;
(2) Placing a chip carrying a sample to be observed on a metal table, fixing the edge of the chip on the metal table, fixing the metal table carrying the chip in an FIB-SEM dual-beam system, and determining the position of the sample to be observed on the chip under an electron beam window;
(3) Under an ion beam window, at least two points are selected to directionally deposit metal tungsten I at the contact position of a sample and a chip, and the position of the sample on a grid is fixed; preventing the sample from shifting on the carrier net in subsequent observation or reaction;
(4) Depositing metal tungsten II directionally along the periphery of the sample under a chip observable window, and forming an internal standard substance microarray at the periphery of the sample;
(5) Loading the marked chip to a transmission electron microscope in-situ heating sample rod, selecting a plurality of observation micro-areas, and recording the structure and component information of the corresponding observation micro-area samples by image acquisition and energy spectrum technology;
(6) Taking out the chip, putting the chip into a reactor, and starting a specific reaction;
(7) And (3) after the reaction is finished, taking out the chip, reloading the chip to a transmission electron microscope in-situ heating sample rod, positioning and navigating the chip to the observation micro-area selected in the step (5) through an internal standard substance microarray, and observing the structure and component changes of the sample corresponding to the observation micro-area after the reaction through image acquisition and energy spectrum technology.
In the step (1), a powdery sample to be observed is dispersed in ethanol to prepare a uniform solution, and the concentration of the sample is not more than 0.1mg/mL.
Wherein in the step (1), the chip is Si 3 N 4 The TEM grid chip can be heated.
In the step (2), the edge of the chip is fixed on the metal platform through the conductive adhesive.
In the step (3), when the nano material is fibrous, the upper end point and the lower end point of the fiber are selected to deposit metal tungsten I, and the diameter of the deposited metal tungsten I is larger than that of the fibrous nano material; when the nano material is in a sheet shape, at least two vertexes are selected to deposit the metal tungsten I.
In the step (4), the particle size of the deposited metal tungsten II is not larger than the diameter of the target nano-particles in the micro-area to be observed, and the distance between adjacent metal tungsten II particles is not larger than D + D, wherein D is the diameter of the target nano-particles, and D is the adjacent distance of the target nano-particles.
Wherein, in the step (5), the number of the observation micro-regions is 2-5.
Has the beneficial effects that: according to the positioning method, on one hand, a metal tungsten fixed sample is deposited through a Focused Ion Beam (FIB), on the other hand, an internal standard substance array is constructed on the periphery of a grid-carrying observable window sample through the Focused Ion Beam (FIB), and the position relation between a selected micro area to be detected and a corresponding monomer in the array is determined by limiting the relation between the size of a single internal standard substance in the internal standard substance array and the grain size of the sample and the distance between adjacent internal standard substances, so that the grid can be accurately positioned to the corresponding micro area to be detected after necessary transfer, namely, the grid can still be conveniently and accurately positioned to an initial observation micro area after necessary transfer, the change conditions of the structure and the component of the nano material after the action of a specific external field are tracked, a relevant reaction mechanism is guided and analyzed, and the efficient and stable nano material is synthesized.
Drawings
FIG. 1 is a diagram of Aduro mirror stem mating Si of Protochips 3 N 4 A schematic structural diagram of a heating chip;
FIG. 2 is a schematic diagram showing the operation flow of the transmission electron microscope grid internal standard substance microarray accurate positioning method;
FIG. 3 is a schematic diagram showing a procedure for constructing an internal standard microarray near a fiber sample by FIB deposition in example 1;
FIG. 4 is a schematic flow chart of construction of an internal standard microarray near a fiber sample by FIB deposition-etching;
FIG. 5 is a schematic flow chart of constructing an internal standard microarray near a nanosheet sample by FIB deposition.
Detailed Description
The technical solution of the present invention is further described with reference to the following specific embodiments.
Example 1
The invention relates to an observation micro-area positioning method based on an internal standard substance microarray, which specifically comprises the following steps:
(1) A small amount of Al is added 2 O 3 /TiO 2 Dispersing composite nano fiber (the diameter of the nano fiber is about 300 nm) in ethanol to prepare a uniform solution with the concentration of 0.1mg/mL, and dripping the solution on Si matched with Aduro electric mirror rods of high-temperature resistant Protocochips 3 N 4 Heating the chip;
(2) After a sample is dried, placing the chip on a clean metal table, fixing the edge of the chip by using a conductive adhesive, fixing the metal table carrying the chip in an FIB-SEM dual-beam system, and determining the position of the sample to be detected on the chip by using secondary electrons under an electron beam window;
(3) Under the ion beam window, towards Al 2 O 3 /TiO 2 Directionally depositing metal tungsten I at two ends of the composite nanofiber, which are in contact with the chip carrier net, processing the composite nanofiber for 60s under the conditions that the voltage is 30kV and the current is 40pA to obtain the metal tungsten I with the diameter of 400nm, and fixing a sample on the chip to prevent the sample from shifting in subsequent observation or reaction;
(4) To observe Al 2 O 3 /TiO 2 The migration motion of oxide crystal grain interface (the crystal grain size is 30 nm) in the composite nano fiber is towards Al in the observation window of the chip under an ion beam window 2 O 3 /TiO 2 Directionally depositing a metal tungsten II nano lattice around the composite nano fiber, and processing for 1-10 s under the conditions that the voltage is 10kV and the current is 7pA to obtain metal tungsten II particles with the diameter of 5-30 nm, wherein the distance between adjacent metal tungsten II particles and an internal standard substance is not more than 50nm (shown in figure 3);
(5) Loading the marked chip to an Aduro electric mirror rod of the Protochips, selecting 2-5 typical observation micro-areas, and recording the structure and component information of corresponding crystal grains in the observation micro-areas by image acquisition, energy spectrum and other spectroscopy technologies;
(6) Taking out the chip, putting the chip into a carbon black oxidation reactor, and starting reaction;
(7) And (3) after the reaction is finished, taking out the chip, reloading the chip to an Aduro electron microscope rod of the protocols, positioning the chip to the micro area to be tested selected in the step (5) through the internal standard substance microarray, and observing the structure and component change of the corresponding crystal grains in the micro area to be tested after the reaction.
Example 2
The invention relates to an observation micro-area positioning method based on an internal standard substance microarray, which specifically comprises the following steps:
(1) A small amount of TiO loaded with Pt nanoparticles (the diameter of the Pt nanoparticles is 3 nm) 2 Dispersing nanometer fiber material (diameter of fiber material is 100 nm) in ethanol to obtain uniform solution with concentration of 0.1mg/mL, and dripping the solution on Si matched with Aduro electric mirror rod of high temperature resistant Protocochips 3 N 4 Heating the chip;
(2) After a sample is dried, placing the chip on a clean metal table, fixing the edge of the chip by using a conductive adhesive, fixing the metal table carrying the chip in an FIB-SEM dual-beam system, and determining the position of the sample to be detected on the chip by using secondary electrons under an electron beam window;
(3) Under the ion beam window towards the TiO 2 Directionally depositing metal tungsten I at two ends of the nanofiber, which are in contact with the chip carrier net, processing for 30s under the conditions that the voltage is 30kV and the current is 40pA to obtain the metal tungsten I with the diameter of 150nm, and fixing a sample on the chip to prevent the sample from shifting in subsequent observation or reaction;
(4) To observe Pt nanoparticles and TiO 2 The surface interface micro-area of (2) is under the high-magnification ion beam window, and the TiO in the observation window of the chip net is carried 2 Directionally depositing a metal tungsten II nano lattice around the nano fiber, processing for 1-5 s under the conditions that the voltage is 10kV and the current is 7pA to obtain metal tungsten II particles with the diameter of 1-3 nm, and combining with etching operation (etching solid metal tungsten particles into hollow metal tungsten particles), on one hand, the using amount of metal tungsten can be reduced, on the other hand, a nano lattice with more identification degree (as shown in figure 4) can be constructed, and adjacent inner parts are adjacentThe distance between the targets is not more than 5nm;
(5) Loading the marked chip to an Aduro electric mirror rod of the Protochips, selecting 2-5 typical observation micro-areas, and recording corresponding structure and component information in the observation micro-areas through image acquisition, energy spectrum and other spectroscopy technologies;
(6) Taking out the chip, putting the chip into a CO oxidation reactor, and starting reaction;
(7) And (3) after the reaction is finished, taking out the chip, reloading the chip to an Aduro electron microscope rod of the protocols, positioning the chip to the micro area to be detected selected in the step (5) through the internal standard substance microarray, and observing the structure and component change of the sample in the micro area to be detected after the reaction.
Example 3
The invention relates to an observation micro-area positioning method based on an internal standard substance microarray, which specifically comprises the following steps:
(1) A small amount of Al loaded with Pt nanoparticles (the diameter of Pt nanoparticles is 3 nm) 2 O 3 Nanosheet material (the area of the nanosheet material is 100 x 100nm) 2 ) Dispersing in ethanol to obtain a uniform solution with a concentration of 0.1mg/mL, and dripping the solution on Si matched with Aduro electron microscope rods of high-temperature resistant protocols 3 N 4 Heating the chip;
(2) After a sample is dried, placing the chip on a clean metal table, fixing the edge of the chip by using a conductive adhesive, fixing the metal table carrying the chip in an FIB-SEM dual-beam system, and determining the position of the sample to be detected on the chip by using secondary electrons under an electron beam window;
(3) Under the ion beam window, towards Al 2 O 3 Directionally depositing metal tungsten I at two ends of the nanosheet, which are in contact with the chip carrier net, processing the nanosheet for 10s under the conditions of voltage of 10kV and current of 7pA to obtain the metal tungsten I with the diameter of 20nm, and fixing a sample on the chip to prevent the sample from shifting in subsequent observation or reaction;
(4) To observe Pt nanoparticles and Al 2 O 3 The surface interface micro-area of (1) is arranged in the observation window of the chip grid under the high-magnification ion beam window 2 O 3 Directionally depositing a metal tungsten II nano lattice around the nano sheet, and processing the nano sheet 1 under the conditions that the voltage is 10kV and the current is 7pAAbout 5s, obtaining metal tungsten II particles with the diameter of 1-3 nm, wherein the distance between adjacent internal standards does not exceed 5nm (shown in figure 5);
(5) Loading the marked chip to an Aduro electric mirror rod of the Protochips, selecting 2-5 typical observation micro-areas, and recording the structure and component information corresponding to the sample in the observation micro-areas by the image acquisition and energy spectrum and other spectroscopy technologies;
(6) Taking out the chip, putting the chip into a CO oxidation reactor, and starting reaction;
(7) And (3) after the reaction is finished, taking out the chip, reloading the chip to an Aduro electron microscope rod of the protocols, positioning the chip to the micro area to be detected selected in the step (5) through the internal standard substance microarray, and observing the structure and component change of the sample in the micro area to be detected after the reaction.
The method can realize accurate positioning of the nano material on the grid surface of the transmission electron microscope, solves the key problem that the micro area to be detected cannot be accurately tracked in the using process of the transmission electron microscope, solves the difficulty that various real reaction processes cannot be simulated in the using process of an in-situ transmission electron microscope, enables tracking of fine structure change of the material in the reaction process to be possible, provides a new idea for the application of the transmission electron microscope in analyzing the interface structure evolution mechanism of the material surface with high spatial and temporal resolution, and can restore the fine structure evolution process of the material in complex chemical and physical environments under real working conditions; the positioning method can be expanded to be applied to similar microscopic observation technology, and helps to realize positioning and resetting observation of the nano-sized micro-area.
Claims (7)
1. An observation micro-area positioning method based on an internal standard substance microarray is characterized in that: the method comprises the following steps:
(1) Dispersing a powdery sample to be observed in a solvent to prepare a uniform solution, and dripping the solution on a special heating chip of a transmission electron microscope;
(2) Placing a chip carrying a sample to be observed on a metal table, fixing the edge of the chip on the metal table, fixing the metal table carrying the chip in an FIB-SEM dual-beam system, and determining the position of the sample to be observed on the chip under an electron beam window;
(3) Under an ion beam window, at least two points are selected to directionally deposit metal tungsten I at the contact position of a sample and a chip, and the position of the sample on a grid is fixed;
(4) Depositing metal tungsten II directionally along the periphery of the sample under a chip observable window, and forming an internal standard substance microarray at the periphery of the sample;
(5) Loading the marked chip to a transmission electron microscope in-situ heating sample rod, selecting a plurality of observation micro-areas, and recording the structure and component information of the corresponding observation micro-area samples by image acquisition and energy spectrum technology;
(6) Taking out the chip, putting the chip into a reactor, and starting a specific reaction;
(7) And (4) after the reaction is finished, taking out the chip, reloading the chip to the transmission electron microscope in-situ heating sample rod, positioning and navigating to the observation micro-area selected in the step (5) through the internal standard substance micro-array, and observing the structure and component change of the sample corresponding to the observation micro-area after the reaction through image acquisition and energy spectrum technology.
2. The method of claim 1, wherein the internal standard microarray-based observation micro-area localization method comprises: in the step (1), a powdery sample to be observed is dispersed in ethanol to prepare a uniform solution, and the concentration of the sample is not more than 0.1mg/mL.
3. The method of claim 1, wherein the method comprises: in the step (1), the chip is Si 3 N 4 Heatable TEM grid chip.
4. The method of claim 1, wherein the method comprises: in the step (2), the edge of the chip is fixed on the metal platform through conductive adhesive.
5. The method of claim 1, wherein the method comprises: in the step (3), when the nano material is fibrous, selecting upper and lower end points of the fiber to deposit metal tungsten I, wherein the diameter of the deposited metal tungsten I is larger than that of the fibrous nano material; when the nano material is in a sheet shape, at least two vertexes are selected to deposit the metal tungsten I.
6. The method of claim 1, wherein the method comprises: in the step (4), the particle size of the deposited metal tungsten II is not larger than the diameter of the target nano-particles of the micro-area to be observed, and the distance between adjacent metal tungsten II particles is not larger than D + D, wherein D is the diameter of the target nano-particles, and D is the adjacent distance between the target nano-particles.
7. The method of claim 1, wherein the internal standard microarray-based observation micro-area localization method comprises: in the step (5), the number of observation micro-regions is 2-5.
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