Method for detecting of structural heterogeneity of elastomers

FIELD: chemistry.

SUBSTANCE: invention can be used in qualitative and quantitative evaluation of degree of both structural and deformational heterogeneity of such elastomers as oriented polyethylene terephtalate (PETP) or high-pressure polyethylene (HPP), using device for sample heating. As researched polymer sample, preliminary oriented PETP or HPP plate or film is used. Sample is placed on polished substrate, and a sheet of foil made of heat-conducting material is placed on the top of sample surface. Sample is heated through the foil with flat heating element at temperature 1.5-2.5 times higher than upper limit of operating temperature Top., during 2-15 seconds and under pressure of 3-4 g/cm2. Then pressure is reduced to 0.3-0.4 g/cm2, keeping heating element on sample during 1-15 seconds. After that, heating element is removed and sample is air-cooled. Degree of heterogeneity is determined visually both on sample surface and in the volume. After shrinkage change of form of investigated material sample is studied, followed by investigation of tension of compression and stretching in detected sections of higher and delayed deformations respectively in the form of deflection of positive and negative signs, in samples of investigated PETP. Also structure-formation at over-molecular level of different sample sections is studied.

EFFECT: detecting structural heterogeneity at the level of over-molecular organisation, visualisation of heterogeneities, simplification and acceleration of detection and investigation method.

16 dwg


The invention relates to methods for assessing the structural heterogeneity of polymers, in particular to a method of identifying macroinhomogeneity patterns elastomers.

It can be used in assessing the degree of structural and deformation heterogeneity oriented polyethylene terephthalate (PET) or polyethylene (LDPE) using the device for heating the samples.

There is a method of identifying structural heterogeneity [1] elastomer, namely, that the sample of the polyurethane is placed in dioxane in the presence of dimethylformamide at a temperature of 20-25°and incubated in this medium for 3-5 minutes. Solvents cause severe swelling of the disordered parts of elastomer and a slight swelling of the structures themselves. Then the sample is transferred into the water and stand in it for 5 minutes, then removed and dried at a temperature of 20-25°C. the processing precipitator fixation patterns, and in the optical microscope appears clear picture of the supramolecular structure of the elastomer, completely identical to the picture obtained before treatment precipitator.

But the method has limited application. It does not apply to polymers, is not able to swell at room temperature (20-25° (C) the temperature in dioxane in the presence of dimethylformamide. Such polymers relates the I PET. The swelling of the polymer, as is known, leads to the violation of connections between structural elements. Therefore, the amorphous fraction in the solvent can be dissolved and crystalline and intermediate organization of supramolecular structure remains. When exposed precipitator - water - solvent is removed from the polymer, and, indeed, visible structure: that which appeared in the process of swelling.

The part that was dissolved in the plasticizer and solvent, has changed its state and has no boundaries clear organization of the structural elements. The method requires the use of toxic substances. It is not very productive due to the time consuming process of identifying and fixing structure of the elastomer.

There is a method of thermo-mechanical testing samples of plastics with heating it during the test by means of a heating device [2]. The device constituting the heating element, located symmetrically relative to the cross-sectional sample. Heating element made in the form of covering the sample with a metal belt, the profile cross-section which provides a constant temperature along the height of the heated area of the sample and the cavity between the sample and the zone covered by insulating screen. The heating element is made detachable from the guide pins

But the device does not help to identify inhomogeneities in polymers (polyethylene in the form of a film and PET in the form of a film or plate) during mechanical testing. Heating method is designed for a uniform temperature distribution in the sample, the exposure of the sample to the test in the heating element to stabilize the heating mode, which does not contribute to the manifestation of heterogeneity in the studied polymer.

As a prototype of the claimed invention, the selected method of estimating the structural heterogeneity of elastomers [3], which comprises applying to the surface of the sample elastomer organic matter insoluble elastomer, removal of specified substances from the surface of the elastomer and view it in the optical microscope. The study is subjected to a sample of vulcanized film thickness of 1.9-2.1 mm from natural rubber latex or unfilled rubber-based rubber. As an organic substance use polymethylsiloxane, vaseline oil or melt thermoplastic, for example polyethylene terephthalate or polyethylene, is heated to 150-300°s View of the optical microscope is carried out in transmitted light, commonly used to measure the diameter of pores in the sample. The average diameter of pores characterizes the heterogeneity of the structure of the film and shows the presence of unvulcanized zones in the material. The structure considered is tsya optimal and durable rubber for prolonged storage, when the unvulcanized area has certain dimensions identified heat shock (under the drop melt PET).

The method does not allow to identify the heterogeneity of the polymers of the polyolefin and polyester (such as PET)having a high melting point.

At 275°With PET or polyethylene (LDPE) melt. Moreover, the method is difficult to implement, as it requires first obtaining samples with optimal mechanical properties of which make the standards, which assess the degree of heterogeneity of the investigated sample. Because the polymers are heterogeneous material, to determine the optimum average pore size that is required as a reference, can, preparing at least 5-10 samples is not very high-tech. This method is not precise, since shrink linear polymer after hitting a known manner ruining, because it is proposed to carry out a thermal shock at temperatures far above the melting point or degradation as a reference sample and of the investigated polymer. And the shrinking of the investigated polymer under the action proposed prototype temperature should lead to changes in the size, so the method is intended only for surface effect.

Object of the invention is vyyavlennymi inhomogeneities in the film or plate is pre-oriented polymer, mainly PET or LDPE, imaging of discontinuities, simplification and acceleration of the processes of identification and research.

The technical result of the invention is achieved by a method of detecting structural heterogeneity of elastomers, as known, is heat-treated sample of the unfilled polymer in the form of a film thickness up to 2 mm, cooling it in the air, his study on the degree of heterogeneity, according to the invention, and as the study of polymer sample using pre-oriented plate or film of PET or LDPE, studied film or plate, the sample is placed on a flat polished substrate, the top surface of the sample impose a foil sheet of heat conducting material, heat the sample through the foil flat heating element at a temperature at 1.5 to 2.5 times the upper limit of the working temperature Tslave.(i.e. 1.5 to 2.5 Tslave.), for 2 to 15 seconds and under a pressure of 3-4 g/cm2then reduce the pressure to 0.3-0.4 g/cm, while maintaining the heating element in the sample during 1-15, then it is removed, cooling the sample in air, a study on the degree of structural heterogeneity are visually as on the sample surface and in the volume examine the change in the shape of the sample of the study material after Osadchii investigate the compressive stress and strain in the identified areas of increased and delayed deformations, respectively in the form of troughs positive and negative signs in the samples studied PET, study the structure formation at the molecular level, different parts of the sample.

This sequence of actions on the sample allows you to visually detect the oriented film of a thickness of 0.5 mm and a plate thickness of 1 mm poly (ethylene terephthalate) various shapes, sizes and directions of deflections in the direction of the substrate (the negative sign of the deflection and the deflection in the direction of the heating element (positive deflection), by which it is possible to determine structural heterogeneity and local residual stress is also another type known methods [4]. Proposed in the invention procedure identifies the polyethylene material structure and the degree of heterogeneity on the diversity of supramolecular structure and their orientation. The upper and lower surface when the difference in the structural organization can identify different levels of heterogeneity.

Clearly identify structural amorphous component and a crystalline component. The heating element is made with a smooth, flat contact with the sample surface in order to avoid false picture of inhomogeneities (artifact), the resulting unevenness of the load, the educational element. But since the heating element can have different temperatures in areas near and distant from the spiral, and along the edges and in the center of the heating element, the upper surface of the sample placed heat-conducting material in the form of foil, promoting the equalization of temperature around the perimeter of the sample.

The use of heat conducting material in the form of a foil (copper, aluminium etc) unlike analog [2] promotes rapid heat transfer to the sample, due to this, the exposure time of the sample is counted from the moment of contact of the heating element with the sample through the foil. In the device [2] the heating element is a belt of copper considerable thickness that gradually warms up when turning on the power source through the cores, which have a coil resistance heater cores. Thus, the claimed method, as a technical solution has the criterion of "novelty".

A comparison of the proposed solutions to the prototype and analogues was possible to identify the characteristics that distinguish the claimed solution to the prototype and other analogues, which allows to make a conclusion about its compliance with the criterion of "inventive step".

The proposed invention was repeated laboratory tests on materials for electrical purposes and containers for the beverages and showed that it is ready for industrial use. The invention is preparing to implement the enterprise Kamcable" Perm. It is to be used for training purposes (for laboratory works, controlling the quality of products of the investigated materials) in Perm state technical University and the Institute of continuous media mechanics UB RAS (Perm). The invention has the criterion "industrial applicability".

The essence of the claimed method is illustrated using figure 1-16.

Figure 1 shows the structure of a PET in the form of capacity after the blowing of the preform (the middle part of the tank), 2-4 show revealed the heterogeneity of the structure of the plate of the PET from the tank (top, middle and bottom of the tank, respectively, the test was conducted at 140° (C), 5-6 show revealed the heterogeneity of the structure of the plate of the PET from the tank (in the middle and lower parts of the vessel, respectively, the test was conducted at 180°). 7 shows heterogeneity on the film of PET, used for insulation in electrical engineering (the test was conducted at 140°). Fig-11 show the deflections with positive and negative sign on PET-plate detected by the proposed method. On Fig shows the structure of an oriented film of polyethylene, identified after testing to grow the group. Fig-14 exhibit structural heterogeneity of plastic film, Fig - structural heterogeneity identified in the mode of recycling plastic film, and Fig recorded the destruction of the plastic film.

An example of a specific application 1.

Take PET brands PET-O (GOST 24324-80) in the form of containers of carbonated beverages. Capacity cut into segments, taken near the neck, in the middle and under the middle part of the vessel. Prepare plates 50×50 mm Polymer is oriented structure, because of the preform (preform) capacity is obtained by blowing (figure 1).

Since under the action of compressed air procurement from the bottle is blown into the preform from the top down, the degree of orientation in different parts of different capacity. So, closer to the neck of the degree of orientation of the smallest. In the middle the most. From the middle part towards the bottom part orientation is at an angle to the longitudinal axis of the blow. In the orientation of the structural elements in the process of blowing have after blowing forced elastic state of the material (PET). When using tanks on purpose observe that in local areas of the tank after filling carbonated liquid have an increased deformability. As a result, local opening of the wall to the expansion of the tee and the leakage of the beverage from it. Another problem is the recycling of used containers. In connection with forced when blowing elasticity PET in the recycling process behaves unpredictable (due to shrinkage, which controls the mode of processing, because the degree of shrinkage depends on the temperature and pressure used in forming the product).

Samples of such oriented material (PET) is placed on a flat substrate with a smooth polished surface (glass), the sample is placed a thin layer of foil of copper (M1), on the surface of the sample at the temperature of the flat heating element 140-144°C (1,8Tslave.and the pressure of the heating element on a sample of 4 g/cm2withstand 15 seconds, and then at the same temperature of the heating element, the pressure on the sample is reduced sharply to a value of 0.3 g/cm2and again incubated for 15 seconds, the sample in the new position. During this time, the material sample has been shrinking at a certain rate, shrinkage changes shape (Fig.2-5)was conducted deflection at reduced pressure, the deflection is positive. At the same time in some places there are more deformable structures (amorphous) occurred deflections of the material with a negative sign at different depths (figure 2-11). The width of the space deflection (deepening) also RA is Naya, depending on the footprint of this structural component. The view is visually after you clean the heating element with the foil from the surface of the sample and will fully cooled down. Picture of the distribution of the amorphous component or more deformable parts in the sample compared to crystalline (less deformable or deformable with the opposite sign of deflection than the amorphous part) allows to determine the degree of heterogeneity of the material in the investigated temperature processing. In the same way, check the degree of heterogeneity and the forming material (Fig.2-7) at the heating temperature of the sample 160-200°C. it was found that 15 seconds of exposure at a pressure of 3 g/cm2and then 0.3 g/cm2after the next 15 seconds of exposure, allow the deformation of the sample and to stabilize the resulting picture heterogeneity at this temperature. Less than 15 seconds of exposure - the process is not completed and gives a distorted picture, and more than 15 seconds to withstand the sample at a given temperature and pressure, it makes no sense, because the process is complete. Tslave.- the upper limit of the operating temperature of the polyethylene terephthalate in which the material is not prone to shrinkage and structural rearrangements. It is equal to 80°From [6]. To identify the degree of heterogeneity of the material in full when shrinkage aulani the x, complicating the prediction of behavior it can be in the range 140-200°i.e. 1,8-2,5 Tslave.when there is an intensive process of crystallization, followed by shrinkage effect.

Below we propose the temperature range of heating the sample shrinkage occurs due to memory effect. During this period, the heterogeneity is not detected. And above 2.5 Tslave.heating of the sample is undesirable because the restructuring is accompanied by partial or complete destruction of the material.

An example of a specific application 2.

Take a polyethylene film brand 19104-005 a thickness of 1 mm (EDT) TU 6-05-1853-80. The film is cut into segments of size 50×50 mm, the Sample is placed on a flat substrate made of glass with a smooth polished surface, and the sample is placed aluminum foil. Heating a flat element having a temperature of 1.5 Tslave.or 120°With, place under a pressure of 3 g/cm2to the sample and incubated in contact with him for 2 seconds. Then the pressure is reduced to 0.4 g/cm2and maintain the sample in contact with the heating element for about 1 second, then remove the heating element and the pressure on the sample, remove the foil and cool the sample in air. The results reveal the true condition of the structural elements and their interrelation. Watching obtained visually picture, studying stephanoderes systems (Fig) or heterogeneity (Fig-15), which is expressed in the identity or non-identity of structural supramolecular formations on the surface of the sample. For the combined assessment can be done shooting patterns in a given scale of the studied material, repeating the proposed mode of identifying patterns and heterogeneities in samples of larger size, reducing the error in their assessment to a minimum.

To study the behavior of the studied material by processing it at this temperature (1.5 Tslave.where Tslave.=80° (C) requires the sample to stand under the pressure of the heating element 0.3 g/cm2within 8 seconds, during this time, the shrinkage of the film ends and the change in the structural state that is identical to that which corresponds to the secondary processing of the investigated material (Fig).

The method visualizes the structural state of the investigated polyethylene, which allows to determine the degree of heterogeneity him, to draw conclusions depending on the ultimate goal of material used.

When the temperature of the sample is less than 1.5 Tslave.even with increasing time of heating, the material structure is not detected. At high heating temperatures and exposure times (1-2 seconds) the sample begins to melt and be a discrete pieces of film with the rest of the fibrils, is broken off when the material is deformed (Fig).

The proposed method is compared with the prototype has the advantages of:

the method is easily applicable, because it does not require pre-production samples - standards, the study does not require viewing optics picture of an inhomogeneous state of the investigated polymer, because it's clearly seen visually;

the method allows, without breaking the polymer surface by mechanical or chemical means, for detecting a second structural state of the elastomer that is resistant to etching agents, changes its properties under mechanical impact. This applies to polyethylene in the film. The method allows not chemically and mechanically breaking the surface of the sample, to reveal the polyethylene terephthalate is much wider than the task in the invention. In the revealed picture clearly without the use of optics detected deflections of different sign (positive sign of the deflection effect of shrinkage under the influence of temperature, which allows to determine, for example, by the method of moiré patterns [6, str] or by the method of elastic beams [6, str] the residual stress of compression; the negative sign of the deflection of the indicator of the presence of amorphous areas (stress strain) in the studied material, which have a certain size, direction, and density of locations on the surface and which D. who have information on the degree of heterogeneity in percent, expressed in volumetric ratio of amorphous to the crystalline component (deflection with a positive sign), and the difference of the sizes of sections of the trough, height);

the method allows studying the study material for the future, because it detects the "weak" points and allows to quantify the degree of heterogeneity, which affects the physico-mechanical properties of the articles of these materials;

- first discovered the effect of rendering heterogeneities in samples of poly (ethylene terephthalate), carved out of containers for carbonated beverages, due to the fact that was used flat heating element weighing 1.5 kg After keeping the sample under a pressure of 4 g/cm2and a temperature of 140°With (1,8 Tslave.within 15 seconds with the heating element removed the pressure. Remained the pressure of the heating element. Unexpectedly, the sample began to raise the heating element. Waiting for the end of this rise, uncovered, watching through the glass substrate, that the rise occurred due to the elastic forces of the compression of the crystalline part (deflection with a positive sign). During this same time there was deformation of the amorphous parts of the sample down from the heating element (negative deflection). Rapid cooling recorded the resulting picture. Therefore, the method can be simplified if nizatidine in the sample after the initial (3-4 g/cm 2) to 0.3-0.4 g/cm2using a flat heating element that has a weight equal to the lifting force of the subsequent sample period shrinkage.

Sources of information

1. A.S. No. 324561, MKI G01 No. 21/60, from 10.10.69, (similar).

2. A.S. No. 338813, MKI G01 No. 1/28, from 12.05.69, (similar).

3. A.S. No. 1406480, MKI G01 No. 33/44, from 17.12.84, (prototype).

4. The Handbook. Test methods, monitoring and research of engineering materials. M - engineering, V.3, 1973. - P.132.

5. Resisting. Synthetic polymeric membranes. M - Chemistry, 1991. - P.142.

The way to identify the structural heterogeneity of elastomers, including heat treatment of a sample of unfilled polymer in the form of a film thickness up to 2 mm, cooling it in air, the sample on the degree of heterogeneity, characterized in that as the study of polymer sample using pre-oriented film or a sheet made of polyethylene terephthalate or polyethylene high pressure and heat treatment carried out flat heating element, the sample is placed on a flat polished substrate, and on top of the sample surface lay a sheet of heat conducting foil through which carry out heating at a temperature of 1.5-2.5 times the upper limit of the working temperature of the investigated polymer, for 2-15 with under pressure is m, equal to 3-4 g/cm2then the pressure is reduced to 0.3 to 0.4 g/cm2, can withstand the heating element on the sample during 1-15, followed by a heating element with foil removed from the sample after cooling visually lead the study sample by the degree of structural heterogeneity both on the surface and in the volume, by studying the change in the shape of a sample after shrinkage and exploring stresses of compression and tension in the identified areas respectively increased and delayed deformations in the form of troughs positive and negative signs; study the structure formation at the molecular level, different parts of the sample.


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3 cl, 1 dwg

FIELD: investigation of structural changes in materials.

SUBSTANCE: pre-oriented polyethyleneterephthalate is preferably used as a polymeric material under study. Scratches are applied onto the surface of a product under study using a cutting tool made of quenched steel in the form of a rod having a variable cross-section that varies from cylindrical to conical one. The cone point is flanged, polished and the edge of the flanged portion is used as a working, cutting part of the tool. Moreover, the cutting tool is loaded within the limits from 0.5 to 1 kg and in the course of scratching the structure of the polymer is revealed at the supermolecular level of organisation of elements and also layer-by-layer in the area of deformation, i.e. within the scratch. The structure is studied by eye or by means of an optical microscope. The anisotropy of structural organisation is recorded from the difference in revealed structural organisation within the scratches, applied in different directions, as well as from the difference in deformability of the structural elements along the scratch or within different scratches. The structural anisotropy is estimated qualitatively on the surface and by layers from the formula: at Pc-const, where: As - structural anisotropy of polyethyleneterephthalate, in % E1 - elongation along the deformation axis of the structural element within the scratch, applied in the direction of pre-orientation of the polymer or in a predetermined direction of the research, in mkm; E2 - elongation along the deformation axis of the structural element within the scratch, applied in another direction, in mkm; Pc - load to the cutting tool in the moment of scratch applying.

EFFECT: capability of anisotropy of the structural condition of a hardly processable polymer - polyethyleneterephthalate, having antifriction and etch-resistance properties, as well as extending the capabilities of the method of scratching and layer-by-layer study of the structural organisation of the polymer.

1 dwg, 12 ex

FIELD: prospecting.

SUBSTANCE: during geochemical prospecting samples are taken in the area of the assigned network out of the representative formation of loose deposits below the strata enriched with organic material or characterised by intensive desalination of metals or carry-over of superfine fraction of solid particles. Fragments of crystal materials larger than 1- 2 cm and organic remains are removed out of the samples in the place of sampling. The samples are dried under the conditions that exclude dust emission or contacts of the sample material. Next superfine fractions of solid particles under 10 mcm are extracted under laboratory conditions. For this purpose the dried sample is placed into a bin, which is shaken up on a vibrating platform with simultaneous pumping of air out of the bin. The particles carried over by the air flow are captured by air filters, and they are collected from the filters for precision analysis of the content of chemical elements. By the results of the analysis secondary lithochemical haloes and stray fluxes in the superfine fraction of loose deposits are determined by abnormal content of chemical elements determined. Conclusions on availability and characteristics of ore mineralization zones are made by availability and parameters of secondary lithochemical haloes and stray fluxes. These operations increase feasibility and accuracy of selection of the representative stratum for taking samples and the capacity of separation of superfine fraction for determination of the content of chemical elements.

EFFECT: method enables to increase the efficiency of geochemical prospecting of non-ferrous, rare and precious metals in closed and semi-closed areas.

1 dwg

FIELD: analytical chemistry.

SUBSTANCE: method involves selection of samples and conversion of active compounds of calcium, contained in a wire, into calcium hydroxide. Samples of granular filler are put into weighed heat resistant cups. There are more than two cups. The cups are weighed and the net mass of the mixture is determined. The samples are carefully treated with small portions of water until turbulent reaction stops. The obtained mixture is dried in a drying furnace at 105-110°C until constant mass of the filler is attained. It is then cooled, ground and the mass of the obtained powdered filler is determined. The batch of the dried and weighed filler is ground in vibration grinding mills. When determining the mass fraction of calcium the compensation factor is considered. This factor shows the ratio of the mass of the filler with calcium hydroxide to the mass of the filler, containing metallic calcium.

EFFECT: easily accessible method of preparing flux cored wire for carrying out chemical analysis for determining the overall mass fraction of calcium using a complexometric method.

FIELD: instruments.

SUBSTANCE: device consists of an attachment panel, a vertical pneumatic pusher, and a transmitter. Additionally, the following components are introduced into the device: the second vertical pneumatic pusher with a sample ejector secured on its stem, a rotary reversing actuator, on the shaft of which a lever with a cuvette attached to its end is installed, a sample cuvette reception tank, and a discharge bin. Both bins are installed on the attachment panel, in its cut-through windows joined with a cut-through horizontal slot. The drop bottom of the cuvette is supported by a guide designed as a semi-ring. One end of the guide, through the window, is secured to the inclined bottom of the sample cuvette reception bin, the second end of the guide has a chamfer and is located at a distance equal to the cuvette bottom diameter from the sample discharge bin window plane. The middle part of the semi-ring is supported by a support bar.

EFFECT: decrease in integral measurement error in vertically dropping flows of granular medium.

2 dwg

FIELD: blasting operations.

SUBSTANCE: analysis of explosives traces on human hands or documents includes base contact with human hands and/or documents keeping explosives traces, pickup of traces from base by thermal desorption methods, supply of liberated explosive vapours into analiser. Spectrometer of ion fluidity increment is used as vapours analiser. Explosive vapours are supplied to analiser remotely by transferring sample from base surface by directional cooled and swirling air flow.

EFFECT: increase of analysis results reliability.

5 cl, 3 dwg

FIELD: blasting operations.

SUBSTANCE: analysis of explosives traces on human hands or documents includes base contact with human hands and/or documents keeping explosives traces, pickup of traces from base by thermal desorption methods, supply of liberated explosive vapours into analiser. Spectrometer of ion fluidity increment is used as vapours analiser. Explosive vapours are supplied to analiser remotely by transferring sample from base surface by directional cooled and swirling air flow.

EFFECT: increase of analysis results reliability.

5 cl, 3 dwg

FIELD: automatical aids for sampling liquids.

SUBSTANCE: system for sampling and delivering filtrate has filter submerged into tested medium and connected with collecting tank and vacuum pressure source which is connected with top hole of collecting tank by means of pneumatic pipe. System has sample receiving tank connected with collecting tank and control unit which has first output to be connected with vacuum pressure source. Collecting tank has two separated chambers - washing chamber and dispatching chamber. Lower hole of washing chamber has to be lower hole of collecting tank and side hole of dispatching chamber has to be side hole of collecting tank. Floating valve is installed inside washing chamber to shut off lower and top holes. Filter is connected with lower hole of collecting tank through sampling pipe. Side hole of collecting tank is connected with lower hole of tank for receiving samples through sampling pipe. Flow-type sensor and check valve are installed inside transportation pipe. Output of flow-type sensor is connected with input of control unit; second output of control unit is connected with control input of analyzer.

EFFECT: improved precision of measurement of sample ion composition; prolonged service life of filter.

1 cl, 1 dwg