Preparation method of dielectric specimen for investigations on focused-beam electronic microscope

FIELD: electricity.

SUBSTANCE: preparation method of a dielectric specimen for investigation on a focused-beam electronic microscope of its micro- and nanostructure involves application of a current-carrying coating onto the specimen surface and provision of electrical contact of the specimen coating with the current-carrying object table. The current-carrying coating is applied by wetting of the specimen surface with a solution of hydrophilic non-evaporable non-flammable non-toxic current-carrying ionic liquid in the form of tetrachloroferrate of N-decylpyridinium in acetone and further drying of the specimen in the air till complete removal of a volatile component.

EFFECT: prevention of accumulation of electrical charges on the surface of dielectric specimens.

2 dwg


The present invention relates to the field of research of micro - and nanostructure of the dielectric (non-conductive) organic and inorganic objects by scanning electron microscopy (SEM).

One of the problems of non-conductive materials research methods SEM and x-ray microanalysis is the formation of the electric charge, which quickly accumulates on the surface of the samples when they are scanning a beam of electrons with high energy (charging phenomenon). The charging phenomenon leads to image distortion and thermal and radiation damage to the sample. In certain cases, the surface can accumulate a high enough charge and the sample begins to act as an electronic mirror, decelerates the primary electron beam, leading to complete failure of the device.

The most common way of dealing with the effect of charging is to apply on the surface of the sample with a thin conductive coating providing a flow of charge with samples and not on the possibility of changing its microstructure.

The nearest known from the prior art analog (prototype) of the invention is a method of applying a thin conductive layer on the surface of the dielectric non-conductive sample by vacuum sputtering with use of�m resistive, electron beam or laser heating, in which a prepared sample is placed in a vacuum chamber, which creates a residual pressure of not more than 10-3mm Hg. tbsp., in which a sample by vacuum sputtering is applied to the conductive layer of a predetermined thickness is resistant to oxidation of the metal or alloy (gold, platinum, etc.). Then the sample is transferred to a conductive stage coupled with the housing of SEM, and is mounted on it in such a way as to ensure by using conductive glue or adhesive tapes electrical contact of the sample with the subject table (Goldstein J., Newbury, D., Echlin P., joy, D., Fiori C., an Lifshin E. scanning electron microscopy and x-ray microanalysis: In two books. - M: Mir, 1984. - 651 S.).

One of the disadvantages of the prototype is that for depositing thin conductive layer of metal requires additional specialized equipment (vacuum installation for thermal or magnetron sputtering). In addition, the performance of the method relative small due to the large investment of time to start the equipment and training equipment. Other shortcomings should be noted that during the deposition of films on porous objects and unpolished chipped with deep reliefs can be problems with continuity of cover, in St.�u turn leads to the accumulation of charges. In addition, it is necessary to take special measures to exclude the formation of their own microstructure of evaporated metal films, which can mask the microstructure of the investigated objects and complicate the interpretation of the obtained data. In this regard, the choice of the metal used also is somewhat problematic and dependent on the objectives of the study. In the literature there are some recommendations for choosing the composition of the sputtered films. Most commonly used precious metals and their alloys (gold, alloys of gold, palladium, platinum), as well as refractory metals tungsten, molybdenum, however, a single universal approach to date has not been developed.

The object of the invention is the complete or partial exception to these shortcomings of the prototype.

The task and the technical result is achieved in that in the method of preventing the accumulation of electrical charges on the surface of dielectric samples before placing the test sample in the vacuum chamber of the SEM the surface is moistened with a solution of hydrophilic neizprotamas non-flammable non-toxic ionic conductive liquid tetrachloroferrate N-deserpidine in an organic solvent, are in the process of evaporation of the solvent for 30 minutes �ri room temperature and provide the electrical contact of the conductive liquid covering the sample with the housing unit when it is placed on the conductive the sample table.

Fig. 1 shows the microstructure of the chip core of the breed without the conductive layer. Fig. 2 shows the microstructure of the chip core rocks with liquid conductive coating applied according to the proposed method.

On the surface of the dielectric (non-conductive) sample a thin layer is applied to a prepared solution of the hydrophilic neizprotamas non-flammable non-toxic ionic conductive liquid tetrachloroferrate N-deserpidine in an organic solvent acetone in the ratio 1:1. The adjustment of the thickness of the liquid layer is carried out by varying the percentage of organic solvent in the starting solution the ionic liquid. The solvent was dried in air for 30 minutes. Then the sample is fixed to a subject table with a conductive glue or adhesive tape. Thus provide electrical contact conductive liquid covering the sample with the housing unit when it is placed on the conductive the sample table. Next, the sample is examined by known methods of scanning electron microscopy.

Drawing on a sample of the ionic liquid according to the invention takes place by simply wetting the surface without the use of special equipment. Thus, unlike the prototype method yavl�is cost-effective and productive. Another difference of the method in comparison with the prototype is to exclude defects discontinuities, since the conductive liquid easily penetrates into the porous structure and deep reliefs samples. Another difference is the complete lack of its own structure of the liquid coating, which could distort the result of the observation.

The invention is shown in the experimental example photomicrographs of core chips of rock produced without application of conductive coatings (Fig. 1) and with liquid conductive coating deposited according to the invention (Fig. 2). The survey carried out on scanning electron microscope JSM 6610LV firm JEOL. As the ionic liquid used is a solution of tetrachloroferrate N-deserpidine in acetone.

From the presented microphotographs visible image artifacts caused by the surface charging of the sample without conductive coating (Fig. 1), and their elimination when applying the conductive coating according to the invention (Fig. 2).

A method of preparing a dielectric sample for the study on the scanning electron microscope micro - and nanostructures, including the application of a conductive coating on the sample surface and providing electrical contact coating of the sample with a conductive object�th table, characterized in that the conductive coating is applied by wetting the surface of the sample with a solution of hydrophilic neizprotamas non-flammable non-toxic conductive ionic liquid in the form of tetrachloroferrate N-deserpidine in acetone and subsequent drying of the sample in air to remove volatile components.


Same patents:

Sampling device // 2556851

FIELD: oil and gas industry.

SUBSTANCE: sampling device contains a main pipeline, a sampling section joined with the main pipeline with a possibility of sampling with coverage of liquid flow cross section, a sampling tap and a manometer. The sampling tap is designed as housing and bushing which is rigidly joined with a handle, and in a starting position the bushing shuts a drain hole of the housing, and the handle can move together with the bushing, opening the drain hole of the housing in working position. The hollow cylinder with the central channel is installed in the main pipeline, and the hollow cylinder from side of liquid flow movement is fitted with the input cone tapering the flow and the output cone expanding the flow on the other side of the hollow cylinder. The whirler fitted inside with tangential channels is installed in the central channel of the hollow cylinder from the input cone. The bushing of the sampling tap covers hermetically from outside the housing with the drain hole and can move restrictedly in axial direction with reference to the housing. The housing has the first and second external cylindrical grooves and the cutting spring lock ring is located inside. The bushing is fitted with internal ring sampler.

EFFECT: improvement of quality of liquid sampling, improvement of operational reliability of the sampling tap and increase of level of correctness of identified process parameters of wells and layers according to analyses of samplings.

2 dwg

FIELD: biotechnology.

SUBSTANCE: method comprises the steps: collecting from the bile ducts of liver of domestic and/or wild animals infected with fasciolas of only live adult F. hepatica. Placement them into individual tubes with filtered and centrifuged bile diluted with isotonic solution of sodium chloride 1:1. Exposure of tubes at t = 38-39°C if F. hepatica is from cattle, and t = 39-40°C if F. hepatica is from sheep and/or goats, under conditions of thermostat for 5 hours. Subsequent washing eggs in isotonic solution of sodium chloride.

EFFECT: invention enables to obtain up to 100 percent of fertilised eggs of Fasciola of species Fasciola hepatica and can be used for study in the laboratory or field experiments in solving fundamental and applied scientific tasks in the field of epizootiology, treatment and prevention of fascioliasis of domestic or wild animals.

2 ex

FIELD: agriculture.

SUBSTANCE: invention relates to the field of agricultural machinery industry. The device for sampling chopped straw from grain combine harvesters comprises collectors, a retainer, a bracket and a control lever. The collectors are arranged in rows, the number of which in the transverse direction is determined by the header coverage and the selected number of the studied areas, and in the longitudinal - replication of sampling. The collectors are interconnected in longitudinal rows by means of flexible connections equal in magnitude, so that the total length of the row does not exceed the distance to the ground mass descent area on the stubble. The first collectors in each longitudinal row have easily removed connections on the holes in the rod-float leveller which is located perpendicular to the direction of the combine movement and retained by the retainer driven by the control lever.

EFFECT: invention provides a boundary separation of the comparable areas in sampling and reduction of the probability of failure of experimental equipment.

2 cl, 1 dwg

FIELD: instrumentation.

SUBSTANCE: invention relates to the method of analysis of a set of ferromagnetic particles. The method is characterized by that the particles of the named set are levelled in such a way that each of the named particles is oriented practically in the same direction. Then the particles of the named set are fixed in this aligned direction and the internal areas of the named particles levelled in such a way are uncovered. After that the nature of the alloy comprised by each of the named particles is identified, the named particles are grouped by categories depending on their nature and the metallurgical structure and chemical composition of one or more of the named particles in each category are determined.

EFFECT: improvement of accuracy and reliability of the analysis of ferromagnetic particles.

14 cl, 6 dwg

FIELD: instrumentation.

SUBSTANCE: invention relates to forecast of ageing processes of the synthetic polymer materials (SPM) depending on duration of their operation or storage. Analysis of the volatile organic compounds (VOC) migrating from SPM is performed by active sampling for sorbent, with further thermal desorption and gas chromatographic analysis. Forecast of the ageing processes of the material and estimation of toxicity of the gas discharge are performed as per dynamic of the qualitative and quantitative composition of gas discharge components in SPM initial state, and during artificial climatic thermal-humidity ageing. Dynamics analysis of the total gas discharge (ΣT) from each material is performed for all substances migrating from studied SPMs. Change of toxicity is estimated and forecast of the material ageing is performed as per developed indices of total gas discharge (ΣT) and as per hygienic index P=(ΣTinitial/ΣTn)/V, where Tinitial and Tn are indices of toxicity of gas discharge of each substance in initial state and after ageing, respectively, and ΣTinitial and ΣTn are total indices of toxicity of gas discharge of all components of SPM in initial state and after ageing, V is duration of ageing (year, month).

EFFECT: invention ensures high accuracy of the method of VOC qualitative and quantitative composition determination in gas discharge during materials ageing and the analysis results repeatability.

3 tbl

FIELD: physics, acoustics.

SUBSTANCE: group of inventions relates to an apparatus for irradiating a sample with focused acoustic energy, a device which is part of said apparatus, a cartridge for said device and a method of irradiating a sample with focused acoustic energy. The apparatus comprises a device, a cartridge, a completely solid-state connector and a source for generating acoustic energy. The cartridge has a chamber for receiving a sample, and the completely solid-state connector provides a completely dry coupling of acoustic energy between the source and the cartridge. The device and the cartridge are adapted for inserting the cartridge containing a sample into the device and are separable, and the focused acoustic energy is focused high-intensity ultrasound. The device has a source for generating acoustic energy and the cartridge has a chamber for receiving a sample.

EFFECT: improved sample processing.

17 cl, 24 dwg

FIELD: motors and pumps.

SUBSTANCE: simulation device contains an oil batcher, a dispersion chamber and a lubricant oil decomposition chamber (1). At the air outlet downstream the chamber the diffuser (2) is located. On the chamber the heater (3) with the thermocouple (4) and the thermorelay (5) is installed. The device includes the air duct (6) supplying the pumped-over hot air into the lubricant oil decomposition chamber connected through the manometer (7) to the air compressor (8). The device contains the cylinder (13) filled with ultra-pure nitrogen, (23, 24) the sealed gage tank with air cavity with oil and a cover for oil filling, with the oil pipeline connected to it through the gas pipeline with the regulator (12), the adapter (11) and cap nuts. The gage tank (9) is connected through the adapter (11) with cap nuts (20, 21) to the measured capillary (15) in a cooling jacket (16) with circulating water through the thermostat with the pump (18) and radiators, attached to the decomposition chamber by means of the cap nut (22) and the sealing cone (25). Also the device comprises the additional chamber (26) screwed to the main decomposition chamber of (1) coaxially and sealed with a gasket (27), with the rod with a flywheel (17) installed inside, with threaded and non-threaded parts. Meanwhile the threaded part is implemented with a possibility of movement in the internal washer with a thread (28) for adjustment of the decomposition chamber volume and change of conditions of simulation of oil concentration, while the non-threaded part is sealed in a gland with graphite seal (29).

EFFECT: improvement of accuracy of simulation of composition of oil decomposition products in aviation gas-turbine engines.

1 dwg

FIELD: aircraft engineering.

SUBSTANCE: invention relates to aircraft cabin air samplers, gadgets for analysis of admixtures in aircraft cabin air samples for analysis of concentration of contaminants in aircraft air conditioning systems and for determination of the composition of harmful admixtures and dangerous concentrations of gases and vapours in air. This sampler comprises evacuated vessel as air consumption booster, absorption cartridge with sorbent-concentrator composed of sharpened steel tube with plugs of glass wool at tube ends, with side bore in said tube filled with sorbent and glass wool. Evacuated vessel is composed of cylindrical case with inlet and outlet pipes fitted at case ends. Outlet pipe is provided with tube of vacuum rubber and metal plug to be fitted in the tube free end after evacuation. Inlet pipe is welded to the case end and features ID larger than that of the case inlet and internal thread. Aforesaid absorption cartridge with sorbent-concentrator is fitted in said inlet pipe and, partially, in evacuated vessel used also as a sampler of admixtures not absorbed by concentrator. Locking device composed of the tube with air sample passage inlet is screwed via seal ring in evacuated vessel surface neck to tight fit. Cover with stiffness ribs and rubber washer is secured to said locking device and aligned therewith. Lever with triangular cam at the end is articulated with the device on opposite side from the cover attachment side to lift said cover to unseal the system and to bleed air. Said lever and cover are secured to be revolved in one plane relative to axles of rotation and attachment. Springs secured from one side to locking device case and to cover stiffness ribs on opposite sides. This makes said cover opened and cover closed at lowered lever and cover located at lever can outer leg. Lever shifted, cover goes up to unseal the system and to bleed air.

EFFECT: higher sampler sensitivity, accuracy of analysis, accelerated in-flight experiment.

3 dwg

Gas sampling system // 2552267

FIELD: oil and gas industry.

SUBSTANCE: system contains casing-well, cylindrical sampler comprising three main parts, top part is manifold chamber, middle part is connecting coupling with female thread and groove connecting bottom and top parts, bottom part is receiving chamber for accumulation of gas supplied via side holes of the casing-well, receiving chamber and manifold chamber are covered with lids, above the connecting coupling a discharge tube is installed, under it a receiving tube is installed, above it a ball valve is installed, top discharge tube passes through the manifold chamber, lid and goes outside, on it the inlet union valve is installed to inject air in the manifold chamber and safety union valve for overpressure relief, the pneumatic chambers are located one above, and another below the inlet holes in the sampler casing, in top lid of the sampler the outlet valve is installed, casing pipe is made out of n pipes connected by outside thread coupling, with side holes of same diameter uniformly distributed along length of the casing pipe-well.

EFFECT: simplified design.

3 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to a solution for fixing biological cells. The fixing solution is intended for in vitro preservation of a cytological sample containing nucleated cells and erythrocytes. The solution contains 80-95 vol. % of a mixture of 590 ml normal saline, 10 ml polyethylene glycol (Carbowax®), 203 ml isopropyl alcohol, 193 ml pure ethanol, 0.01 vol. % sodium azide, and 5-20 vol. % buffered 4% formalin; pH of the fixing solution is in the range of 6.4 to 7.4.

EFFECT: preserving the integrity of nucleated cells.

2 cl, 2 dwg, 1 ex

FIELD: process engineering.

SUBSTANCE: invention relates to machine building, particularly, to surface hardening of steel parts. Straining force is applied from working tool to spinning article. Said working tool is fed along surface sections that make the part profile. Simultaneously, in rolling tool shift over article surface, said strained surface sections are subjected to effects of variable rotary magnetic field of intensity within 2.5×104-1×105 A/m and frequency of 20-70 Hz. Rolling tool represents steel shots, 0.3-3.0 mm in diameter, placed in aqueous suspension containing 29-31% of said shots as a solid component, lead compounds PbO in amount of 13.9-14.1% and PbO2 in amount of 13.9-14.1%, chromium compounds Cr2O3 in amount of 6.8-7.2%, titanium compounds TiO2 in amount of 9.9-10.2%, black-lead lubrication in amount of 17.8-20.2% and water H2O making the rest. Said aqueous suspension is placed into round circular case to dip the article therein unless all surface sections are completely submerged. Then, article is turned in said suspension relative to its lengthwise mirror axis at the rate of 15-30 rpm for 12-15 minutes. Effects of variable spinning magnetic field are brought about by Φ-like magnetic generators inducing the magnetic field features the clusters of magnetic lines composed by bundles revolving around lengthwise axis extending radially from periphery to the centre of circular round case. Said Φ-like magnetic generators are arranged on round circular case outer side surface in three locating cylindrical helices. Note here that the number of said Φ-like magnetic generators equals three or whatever other quantity multiple thereof. The number of said generators arranged regularly on every said helix makes 9 to 18.

EFFECT: notably longer life, higher resistance to outer aggressive effects.

2 cl, 4 dwg

FIELD: process engineering.

SUBSTANCE: set of inventions relates to production of 3D articles. This process comprises making of flexible film and reiterating the steps that follow. Liquid setting material plies are applied on said film which does not contact with said 3D object. Flexible film is placed to preset position relative to 3D object to apply the ply of liquid setting material on the latter. Said preset area of said ply is solidified. Portions of not solidified ply are removed therefrom to get solid ply of preset shape. Note here that in one of said cycles displacement of said flexible film and said solidification occur simultaneously. Invention covers also the system for implementation of said method.

EFFECT: higher rate of 3D object making.

17 cl, 15 dwg

FIELD: machine building.

SUBSTANCE: device for forming wear-resistant and antifriction coatings of parts surface contains bedplate with table made with possibility of the treated part installation and securing, device for process liquid supply, control panel, drives of rotating and progressive movements of the spindle, power cylinder, tool assembly secured on the spindle and containing casing in which the expanding cone, top support cone and bottom support cone, plungers and shoe with fixed in them rubbings are installed. In the shoes bronze and brass rubbings are installed, the tool assembly contains gear monitoring position of the bronze and brass rubbings, its use ensures possibility of neutral or work positions of the rubbings relatively to the treated surface of the part. Possibility of transition and holding of the bronze and brass rubbings in neutral position is ensured by top and bottom ring springs. In casing of the tool assembly along the longitudinal axis a top cylindrical cavity with cut through radial groove, and bottom cylindrical cavity are made, in its cavity in the casing radial holed are drilled. The expandable casing in top part is connected with rod passing through the top cylindrical cavity and bottom cylindrical cavity. On the rod the top and bottom support cones are secured.

EFFECT: increased level of mechanization and automation of the finish machining processes, increased productivity of the process upon reduced labour intensity, increased accuracy of the machined surface and cleanness of the machined surface.

7 cl, 9 dwg

FIELD: process engineering.

SUBSTANCE: invention relates to protection of steam turbine blades against erosion. Proposed process comprises application of protective coating on the blade. Coating is applied by laser surfacing. Laser head is displaced at the rate of linear interpolation Vi not over 0.05 m/s at laser radiation power making 800-1200 W.

EFFECT: hardened ply of 1/3 length of the blade root at sufficient aerodynamics.

2 dwg

FIELD: process engineering.

SUBSTANCE: invention relates to repair of turbine blades. Proposed process comprises preparation of blade surface. Coating is applied with the help of laser radiation with simultaneous feed of additive powder to melt belt. At hard-facing, radiation power P is varied from 300 to 2500 W, and/or as radiation source feed rate V from 0.1-0.01 m/s, and/or amount of powder fed from 3 to 15 g/min.

EFFECT: accelerated process, higher hard-facing quality.

FIELD: process engineering.

SUBSTANCE: invention relates to oxidation of surfaces of metal parts for processing before application of adhesive plies. Proposed method is used in production of rubber-metal parts and comprises metal part surface processing by oxidation in air oxygen at 220-250°C for 20-30 min.

EFFECT: efficient preparation, higher adhesion between metal part and rubber.

1 tbl

FIELD: machine building.

SUBSTANCE: method is performed by addition to the surface layers of the item the alloying chemical elements and by decreasing of size of the particles forming the surface layer during the item surface treatment by the pulse plasma streams with simultaneous action on the surface of the electric current pulses of the acoustic oscillations and magnetic field. To optimise the treatment process the treated surface is by a controlled method connected with the electric circuit by anode or cathode. Control of the connection polarisation is performed upon the combustion gas mixture addition to the plasma generating medium.

EFFECT: modification of chemical composition and structure of surface layer is performed for its hard facing and for improvement of other operation features.

6 cl, 1 tbl, 7 dwg

FIELD: machine building.

SUBSTANCE: method of bi-metal coatings application on steel part surface includes transfer of the metal sheets from the consumable part of rub to the treated part surface during friction between them under pressure due to radial feed of rubs made with possibility of progressive and rotational motion in the tool assembly. Initial roughness of the treated part surface is brought to level of the true surface by microroughnesses cut off by the cutting edges on the work surfaces of the bronze rubs. Then process liquid is supplied to the treatment zone, and forces are applied for radial movement of the bronze rubs till their contact with the part, at that the bottom bronze monolayer is applied with simultaneous part strengthening using friction of the bronze rubs in the process liquid. The top brass monolayer is applied on surface of the bottom bronze monolayer of the treated part surface, at that the top monolayer is applied by friction of the brass rubs in the process liquid.

EFFECT: assurance of qualitative wear-preventive and antifriction coatings out of plastic metals applied by the selective transfer during precision friction, and assurance of improved energy saving parameters, operation service life and fault-free operation.

8 cl, 5 dwg

FIELD: metallurgy.

SUBSTANCE: invention relates to metallurgy and can be used for application of anti-pickup coating on oxygen lance surface at converter steel casting. Proposed method comprises simultaneous spraying of water-air ply at specific water flow rate of 0.3-0.8 l/m2 by appropriate atomisers to sequential lance section over the entire periphery ay lance downward displacement. Then, loose quick line is fed from slag-forming feed channel onto oxygen lance surface. Note here that said atomisers are fixed relative to said oxygen lance.

EFFECT: accelerated production process.

1 dwg

FIELD: chemistry.

SUBSTANCE: method of applying polyphenylene sulphide-based coating on a metal substrate is characterised by applying onto the surface of the metal substrate 3 vol % of an aqueous solution of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane by immersion, drying at 120°C for 60 minutes and electrostatic spraying a polyphenylene sulphide-based powder coating. The metal substrate used is made of low-carbon steel, carbon steel or cast iron.

EFFECT: high adhesion of the coating to the metal substrate and protection from underfilm corrosion when integrity of the coating is breached, which improves corrosion and chemical resistance of the polyphenylene sulphide-based coating.

2 cl, 2 dwg, 1 ex

FIELD: method for coating of superabrasive, in particular, diamond particles, with metal for manufacture of cutting tools, such as grinding or milling tools, or plated diamond articles.

SUBSTANCE: method involves using coating forming metal powder including compound; providing thermal reduction of metal from compound by placing superabrasive particles and powder adapted for forming of coating together into inert atmosphere; heating superabrasive particles and said powder to temperature of from at least 5000C to temperature below superabrasive destruction temperature during time interval sufficient for effective deposition of metal layer onto at least one portion of surface of each superabrasive particle and providing chemical bonding between said particles and said powder; cooling said particles and said powder to temperature below temperature of reaction between superabrasive particles and powder; separating mixture for obtaining of product fraction in the form of superabrasive particles coated with metal and substantially free from coating forming powder and by-product fraction in the form of coating forming powder substantially free from superabrasive particles coated with metal. Described are superabrasive particles coated with metal by means of said method, method for manufacture of abrasive tool with the use of superabrasive particles coated with metal, abrasive tool comprising said particles, and plated product comprising constructional diamond part and equipped with metal layer chemically bonded with at least one portion of surface of said constructive part.

EFFECT: provision for obtaining of material having superthin coatings of chemically active metal uniformly covering superabrasive over the entire surface of substrate.

27 cl, 2 tbl, 8 ex