134 results about "Scanning transmission electron microscopy" patented technology

The invention relates to a formula and method for immobilizing a tick sample for scanning electron microscopy, which belongs to the technical field of methods for immobilizing samples for scanning electron microscopy. The immobilization formula comprises a PBS buffer solution, polysorbate and glutaraldehyde, and a glutaraldehyde immobilization liquid is prepared from the above-mentioned components. The method comprises the following steps: (1) observing whether host tissue is left in basis capituli of the tick sample and if so, removing the host tissue; (2) cleaning the surface of the tick sample; (3) immobilizing the tick sample at room temperature by using the glutaraldehyde immobilization liquid; (4) carrying out gradient dehydration with ethanol on the immobilized tick sample; (5) putting the tick sample into mixed liquor of absolute ethyl alcohol and acetone for displacement, and then putting the tick sample into acetone for displacement; and (6) drying the tick sample in a vacuum freeze drying instrument for drying and spraying gold on the tick sample. During scanning electron microscopic observation, the phenomenon of fuzzy and foggy images or incapable imaging due to ionization discharging of the sample as water vapor produced after electron beam bombardment of the sample encounters high-energy electron streams is prevented.

The invention discloses a sample stage system for measuring the property of the sodium electronic instrument in original position in a transmission electronic microscope. The system comprises a sample stage front end head, a hollow sample rod, and an insulating channel arranged in the end of the sample rod. The electrode of a semiconductor is electrically connected to the outer-connecting lead wire traversed by the insulating channel via the lead wire of the hollow sample rod, and further connecting to the outer analyzing test meter to research the property of the sodium electronic instrument. The precise size assures the TEM electronic beam can orderly traverse the gap of the semiconductor chips and the through hole of the chip carrying stage, focused on the sodium electronic instrument of the upper surface of thee chap gap, in that way the method directly represents the micro-structure of the sodium electronic instrument. Thereby, the invention achieves the original position research of the property of the sodium electronic instrument and the micro-structure.

The invention provides a method for preparing a scanning electron microscope (SEM) sample or a transmission electron microscope (TEM) sample protection layer by using a focused ion beam (FIB) technology, and is applied to samples of which target surfaces are made of metal. The method comprises the following steps of: selectively scanning a target region by an electronic beam; under the action of the electronic beam, depositing an organic material layer on the target region by gaseous organic impurities in an SEM or a TEM; and depositing a metal protection layer on the organic material layer. By using the method for preparing the SEM sample or the TEM sample protection layer by using the FIB technology, before the sample is prepared by using the FIB technology, the organic material layer is deposited on the target region by using the electronic beam, so that the surface of the target region serves as the sample made of the metal; a deposited organic material and a metal material on the surface of the target region are greatly contrasted, so that the interface definition of the metal surface of the SEM or TEM sample which is required to be precisely positioned is greatly improved; and the analysis quality of the SEM or TEM is improved.

The invention relates to a device and a method for performing in-situ double-tilting single-axis stretching on a nanowire and a two-dimensional laminar thin film in a transmission electron microscope, belonging to the field of in-situ mechanical performance measurement research of transmission electron microscope accessories and a nanomaterial. The device comprises a supporting part, a power part and a carrying network part. The supporting part is a metal ring; the driving part is a thermal double-metal sheet, one end of the double-metal sheet is fixedly arranged on the metal ring, the other end of the double-metal sheet generates driving force through bending and moving caused by heat expansion; the carrying network can carry a nanomaterial and is adhered onto the free end of the double-metal sheet, the heated bent double-metal sheet stretches the carrying network, so that the stretching effect of the nanomaterial can be achieved. According to the device, the axial stretching of a single nanowire, and stretching of single-layer / multilayer two-dimensional thin films can be realized conveniently, the problems that the nanowire and the thin film in the original double-metal sheet technology are difficult to fix and poor in stability can be solved, and the structure evolution of the material during deformation can be observed.

The invention relates to the technical field of semiconductor defect analysis, in particular to a failure analysis method for a gate oxide defect original appearance. The method includes the steps that firstly, a semiconductor structure to be tested is screened out under the preset voltage condition, wherein the semiconductor structure to be tested has a gate oxide defect; secondly, the semiconductor structure to be tested is operated, the semiconductor structure has the gate oxide defect, a metal interconnection layer is ground off, a scanning electron microscope voltage comparison method is used for determining the position of the gate oxide defect, an interconnection line, a dielectric layer and a gate are removed in sequence, a contrast layer having the high contrast ratio with the transmission electron microscope contrast ratio of the gate oxide is deposited on the rest of the gate oxide, a transmission electron microscope sample is manufactured on a defective gate area, and finally analysis is conducted through a transmission electron microscope. According to the failure analysis method for the gate oxide defect original appearance, the gate oxide defect original appearance can be clearly observed, and a forceful basis and a forceful direction can be provided for finding the processing technology defect of the gate oxide.

Provided is a method for preparing a transmission electron microscope thin film sample of a longitudinal section of a filament by the electrolysis double-spray method and belongs to the transmission electron microscope sample preparation field. By utilization of the electrolysis double-spray method and aperture samples with a diameter of 3.0 mm, longitudinal section thin films of filament samples with a diameter of 1.0 mm are prepared successfully, and the structure analysis and second phase analysis are performed by utilization of a transmission electron microscope. The samples are prepared after steps of cutting, grinding, clamping, adjustment of beams, electrolysis double-spray and cleaning. The method is advantaged in that two sides of the longitudinal section of a filament sample are polished and thinned by an electrolysis double-spray instrument at the same time, the polishing and thinning time is only 10 s-2 min, and the structure and secondary phase can be obtained accurately. The method reduces the use of parts of sample preparation devices, reduces the cost, and raises the sample preparation efficiency and success rate.

A method for preparing a specimen for application of microanalysis thereto includes forming an initial conductive layer over a defined area of interest on a semiconductor substrate, the initial conductive layer formed through an electron beam deposition process. A volume of substrate material surrounding the area of interest is removed, thereby forming the specimen, including said area of interest and said initial conductive layer over the area of interest. The specimen is then removed from the bulk substrate material.

A process for preparing the film specimen of transmission electron microscope includes preparing metal or alloy film by magnetically controlled sputter, punching on said film to obtain circular film, and thinning it by dual-spray method or ion method.

The present invention disclosure relates to the use of a silicon substrate with a thin film membrane as a transparent substrate for the imaging of biological- and material-related specimens using a microscope such as a transmission electron microscope (TEM). More specifically, the present invention relates to an improved substrate design that incorporates the fabrication of a circular shape that allows easier insertion into traditional specimen holders used in TEMs. In addition to an improved shape, the present invention incorporates microscopic surface texture on the gripping surface that assists in handling. The invention also encompasses surface modification techniques for enhanced biocompatibility of the thin film membrane for biomedical applications.

The invention discloses a preparing method for a micron-order particle sample for a TEM. The preparing method includes the steps that a groove is formed in a flat plate and then filled with curing adhesive mixed with micron-order particle sample bodies, the mixture is heated, cured, cooled and then taken out, and a sheet-shaped block sample is obtained; the two surfaces of the sheet-shaped block sample are manually grinded and polished on a sample support, and a sample sheet is obtained; then supporting rings are bound through curing and binding agents, heating is carried out, the sample support is removed, and meanwhile the supporting rings are cured and bound to the sample sheet; the sample is finished, ion thinning is finally carried out, and the micron-order particle sample for the TEM is obtained. According to the preparing method, an operation technology is simple, adopted sampling devices and adopted sampling technologies are mature, the sampling success rate is high, practicability is high, and the preparing method is suitable for preparing various micron-order particle samples.

The invention provides a test device of the mechanical and electrical properties of a nano-wire compressed in situ in a transmission electron microscope, which pertains to the field of nano-material property test in situ. The device employs a piezoceramic drawing unit, a micro-cantilever mechanical testing system and an electrical measuring system to achieve compression in situ of a single nano-wire or other one-dimensional nano-materials in the transmission electron microscope, and employs the imaging system of the transmission electron microscope to obtain deformation information on a nano or even atomic scale during the compression process. At the same time, the invention can achieve the quantitative measurements of such mechanical properties as elasticity, plasticity, bending and fracturing, and the electrical properties measurement of one-dimensional nano-materials to allow the study on the transport property of a charge during the compression process. The device of the invention has the advantages of simple structure, easy operation, a wide range of application, intuition and quantitative measurement and is beneficial to the explanation and discovery of the good comprehensive property of nano-materials in respect of mechanics, electricity, etc.

The invention relates to a preparation method of transmission electron microscopy samples for in-situ electrical testing. The method comprises the following steps: cutting a top needle point of a metal probe to be flat so as to form a platform with a flat surface; preparing a two-end semiconductor device on the top platform of the metal probe; depositing a protective layer on the top of the formed two-end semiconductor device; thinning the two-end semiconductor device by using the protective layer as a mask so as to form a thin sheet; cutting the thin sheet of the two-end semiconductor device to form a plurality of independent TEM testing samples. The invention solves the electrical connection problem of TEM samples and an in-situ electrical testing TEM sample rod, avoids the step of sample extraction and transfer to a Cu net in routine TEM sample preparation by FIB, reduces the difficulty for sample preparation, improves the success rate of sample preparation, and greatly reduces the cost of sample preparation.

The invention researches a novel process for Zr-Si-Al ternary inorganic coating for rutile titanium dioxide by using a sol-gel method. Through a uniform test design, the influences of various factors to the ternary inorganic coating performance of the rutile titanium dioxide are researched by a system, and the ternary inorganic coating effect of the rutile titanium dioxide is inspected through testing measures such as Nano-ZS, a Fourier infrared spectrometer (FT-IR), a scanning electron microscope (SEM), a transmission electron microscope (TEM), an energy dispersive spectrometer (EDS) and the like. The process for the ternary inorganic coating for the rutile titanium dioxide has the optimized formula as follows: 0.20% of dispersing agent, 0.6% of zirconium, 3.0% of silicon and 1.6% of aluminum, wherein the rotating speed is 340r / min.

Provided is a method of preparing a sample piece for a transmission electron microscope, the sample piece for a transmission electron microscope including a substantially planar finished surface which can be observed with the transmission electron microscope and a grabbing portion which microtweezers can grab without contacting the finished surface. The method of preparing a sample piece for a transmission electron microscope is characterized by including: a first step of cutting out the sample piece from a sample body Wa with a charged particle beam, the sample piece being coupled to the sample body at a coupling portion; a second step of grabbing with the microtweezers the grabbing portion of the sample piece with the finished surface of the sample piece cut out in the first step being covered with the microtweezers; a third step of detaching the sample piece grabbed with the microtweezers in the second step from the sample body by cutting the coupling portion with the charged particle beam with a grabbed state of the sample piece being maintained; and a fourth step of transferring and fixing with the microtweezers the sample piece detached in the third step onto a sample holder.

The invention discloses a preparation method for a transmission electron microscope (TEM) specimen of a cadmium zinc tellurium (CdZnTe) and metal interface. The preparation method is used for solving the technical problem that the reject rate is high because the specimen is broken very easily when the TEM specimen of the CdZnTe and metal interface is prepared in the prior art. The technical scheme is that the preparation method comprises the following steps of: after a CdZnTe single crystal is linearly cut, washed and polished, conducting chemical corrosion; preparing a metal electrode in a resistive evaporation coating machine; folding and sticking the specimen and drying the specimen on a heating table; and grinding, polishing and thinning the specimen along the normal line direction ofa sticking gap, polishing the two surfaces of the specimen, sticking a copper grid on one surface, using a manual grinder to thin the specimen, and finally using a Gatan 691 ion mill to thin the specimen till the specimen is punctured. Since a multi-piece sticking method and a manual grinder for grinding and polishing through high-grade abrasive paper are adopted, after thinning and polishing arecompleted, the damage caused to an interface area in the thinning process is minimized and the success rate of specimen preparation is improved. The success rate of specimen preparation is improved from 30-40 percent in the background technology to 60-70 percent.

The invention provides a micro / nano-particle sample carrying mesh storage device for a transmission electron microscope. The micro / nano-particle sample carrying mesh storage device comprises a clamping handle, a sample carrying mesh and a bottom tray, wherein the bottom tray is provided with a hollow part; the sample carrying mesh is arranged in the hollow part; a clearance is formed between the sample carrying mesh and the edge of the hollow part; the clearance is a flow guide and observation hole; and the clamping handle is connected with the bottom tray, is used for clamping the bottom tray, and is fixed on a matched base is matched with the bottom tray and the clamping handle in shape. The micro / nano-particle sample carrying mesh storage device for the transmission electron microscope has the advantages that in a sample preparation process, the novel carrying mesh and a storage grid are cooperatively used, and the carrying mesh is suspended in the storage grid; and during the fixation of the carrying mesh, the contact between the carrying mesh and each of other solid media is avoided, and the distribution situation of particle samples on the carrying mesh can be directly observed by using bottom light of an optical microscope. Therefore, three defects of the conventional preparation method are overcome, and the sample preparation efficiency is improved.

The invention relates to a transmission electron microscope in-situ nanomechanical tensile testing sample bonding method, which uses a developed micromechanical unit to transfer a sample under an optical microscope and uses epoxy resin to fix the sample. A counterweight, cantilevers and operating tools are fixedly bonded by using epoxy resin, and a three-coordinate micromotion platform of the optical microscope is adopted as a moving unit; the ultrasonically dispersed sample is transferred into a spray unit, and a spraying method is adopted to uniformly spray the sample onto a copper net; the micromechanical unit is used for transferring a single sample onto a drawing unit of an in-situ nanomechanical testing system under the optical microscope; the second-stage operating tool of the micromechanical unit dips epoxy resin and transfer the epoxy resin to the bonded part of the sample, and the sample bonded by the epoxy resin is kept still under room temperature for 24 hours for solidification. The transmission electron microscope in-situ nanomechanical tensile testing sample bonding method provided by the invention is simple, low-cost and nondestructive, and a transmission electron microscope in-situ nanomechanical tensile testing method for one-dimensional nanomaterials is achieved.

The invention relates to a transmission electron microscope sample table for observing a three-dimensional atom probe test sample. The transmission electron microscope sample table comprises a sample rod main body, a press part, an automatic reset device and guide rails, wherein the guide rails are connected to one end of the sample rod main body, a groove opening is formed in the end of the sample rod main body, an arc bottom groove is formed in the axial center of the groove opening, a rectangular step is arranged at the groove opening of the bottom groove, a stepped through hole is formed in the tail end of the bottom groove, the press part comprises a press block and an eccentric wheel, the eccentric wheel is used for pressing the press block, an arc groove body is formed in the press block, is symmetric to the bottom groove of the sample rod main body and has the same shape as the bottom groove, a guide boss of the press block is arranged in the stepped through hole, the automatic reset device is a spring, and the guide boss passes through the spring. The transmission electron microscope sample table is simple in structure and is convenient to process and maintain, large-angle rotation in an inclination way can be achieved, the three-dimensional atom probe test sample can be directly loaded, the transmission electron microscope sample table can be used as a three-dimensional reconstruction sample rod of a transmission electron microscope, and the acquired transmission electron microscope image can be used for directly correcting a data reconstruction result of a three-dimensional atom probe.

Drift generated at the time of photographing a TEM image is corrected simultaneously with photographing, so that a TEM image free form influence of drift is photographed. While the TEM image is recorded, drift in the place out of the view field subjected to recording is measured from moment to moment by another TV camera or a position sensitive detector. Drift is corrected by the movement of the specimen due to a specimen holder or by the movement of the image due to an image shift coil.

The invention provides a preparation method of a TEM sample. The preparation method comprises the following steps of 1, preparing a sample needing to be detected, wherein the sample is provided with a pattern needing to be detected, 2, cutting the sample to obtain a sample wafer, wherein the sample wafer comprises the pattern needing to be detected, 3, thinning the sample wafer from two opposite cut surfaces, and pasting a fixing ring on one of the thinned cut surfaces, 4, clamping the fixing ring, and through a Ga ion beam, bombarding areas which belong to one sample wafer surface provided with the pattern needing to be detected and are located at two sides of the pattern needing to be detected, so that the two sides of the pattern needing to be detected form pits, 5, clamping the fixing ring, and bombarding the thinned cut surfaces by an Ar ion beam, and 6, sequentially thinning an area comprising the pattern needing to be detected. The preparation method provided by the invention improves efficiency and reduces a cost.

The invention relates to a transmission electron microscope sample holder for three-dimensional reconstruction. The sample holder is connected with a sample clamp, a sample is clamped on the sample clamp, the sample holder comprises a hollow casing and a rotation shaft mounted in the casing, a pair of bearings are arranged between the rotation shaft and the casing, the rotation shaft is provided with a rotation driving mechanism used for driving the rotation shaft for rotation, and the sample clamp is fixed with one end of the rotation shaft. The transmission electron microscope sample holderis advantaged in that changing the structure of a transmission electron microscope in the prior art is not needed, and 360-DEG rotation of the sample can be realized.

An assembly for holding a microscopy sample for storage, observation, manipulation, characterization and / or study of the sample using a microscopy instrument is provided. The assembly includes mating first and second parts having faces between which a microscopy sample, including a TEM grid mounted sample, is secured. A spring is used to provide compression between the faces. A rotatable member such as a threaded screw is operable to draw the parts apart from one another. An annular wall functions to protect microscopy samples held in the assembly from damage.

A method for the growth of diamond on a substrate combines an ECR (Electron cyclotron resonance) MPCVD (Microwave plasma chemical vapor deposition) method with a MPCVD method in one system. A two-step diamond growing method comprises firstly etching and nucleation performed by the ECR method and then diamond grown by the microwave plasma CVD method. Not only are high quality continuous polycrystalline diamond films on silicon wafer obtained but also heteroepitaxial growth has been achieved in the present invention. Auger electron spectroscopy (AES), scanning electron microscopy (SEM) and Raman spectroscopy have been used to characterize the structure and morphology of the synthesized diamond films.

The invention discloses a method for preparing in-situ transmission electron microscope (TEM) sample based on a heated chip. The method comprises a step of fixing an initial sample and a heated chip to adjacent plane and inclined surface on a prefabricated sample table, then transferring the initial sample and the heated chip into a FIB-SEM double-beam system and performing vacuuming, a step of depositing a Pt protective layer on the surface of the initial sample by using an ion beam to obtain the initial sample deposited with the Pt protective layer, a step of cutting the initial sample deposited with the Pt protective layer by an ion beam to obtain a strip sample with a triangular cross section, a step of transferring the strip sample and fixing the strip sample to a sample hole groove of the heated chip by using a mechanical hand, and a step of adjusting the position of the prefabricated sample table and stepwise thinning the strip sample by an ion beam to obtain the in-situ transmission electron microscope sample based on the heated chip. According to the invention, the preparation of the in-situ TEM sample is carried out by using the FIB-SEM double-beam system, only one time of sample introduction is needed, the process flow is greatly simplified, the operation is simple and intuitive, and the improvement of the yield of sample preparation is improved.

The invention relates to a thermally driven deforming transmission electron microscope grid and a one-dimensional nano material deformation method, belonging to the nano device and the transmission electron microscope original position nano material deformation method field. The prior grid can be deformed only through electron beam irradiation and the stress supplied is limited. The grid of the invention is as follows: a metallic film A and a metallic film B are vapor-plated on a supporting film of the prior grid, and the thermal expansion coefficient of the metallic film A is more than that of the metallic film B. The one-dimensional nano material deformation method by adoption of the grid is as follows: after the metallic film A and the metallic film B are cut open, one-dimensional nano materials are dispersed on the metallic film A and the metallic film B which are then placed into a transmission electron microscope for heating; the two cracked films are curled due to difference of the expansion coefficients, thereby the driving force for deformation of the one-dimensional nano materials is provided and deformation of the one-dimensional nano materials is realized. The grid can realize large-angle roll steer in two directions of X and Y and realize the original position deformation operation of the one-dimensional nano materials; moreover, the grid is characterized in reliable performance, convenient assembly and simple structure and expands the function of the transmission electron microscope.

The invention relates to a detection method of high resistance of a tungsten contact plug. The detection method comprises the following steps of grinding a semiconductor sample to a tungsten plug contact layer; forming two location tags used for determining a fail address in an area to be observed of the semiconductor sample, and forming a stop flag on a position, which is close to the fail address; grinding a cross section of the semiconductor sample to the stop flag; digesting the semiconductor sample in boiled hydrogen peroxide until metal tungsten is removed and a cobalt silicide layer is exposed; preparing a planar TEM (Transmission Electron Microscopy) sample; observing the planar TEM sample by adopting STEM (Scan Transmission Electron Microscopy). According to the technical scheme of the invention, the metal tungsten is firstly removed, and then the growth morphology and the quality of the cobalt silicide are observed through a STEM mode, so that the reason for the high resistance of the tungsten contact plug can be quickly found, an improvement direction of a technology is indicated, and the detection method has a very important function of improving formation of the high resistance of the tungsten contact plug.

The invention provides a transmission electron microscope in-situ nano indentation method for micron alloy containing isometric single nano-twin crystal, and belongs to the field of transmission electron microscope in-situ mechanical testing f nano-twin crystal. A macro-micro-nano integrated diamond tool is used, each tip has a curvature radius of 40-90 nm and a height of 100-300 Mu m; the tips are arrayed and are distributed on the surface of the tool. The diamond tool is used to indent the surface of the alloy; the indented surface is processed by chemical mechanical polishing; the polishedalloy has surface roughness Ra of 0.5-0.9 nm. A scanning electron microscope with focusing ion beams is used to perform in-situ cutting, splicing, transporting and ion thinning, and a sample has a length of 5-20 Mu m, a height of 4-10 Mu m and a thickness of 50-100 nm. A displacement control mode is used, maximum displacement is 200-1000 nm, and loading speed is 10-30 nm / s. The transmission electron microscope in-situ nano indentation method for single nano-twin crystal is achieved herein.