Method for thermodynamic acoustic-emission standardisation and system for realising said method

FIELD: physics.

SUBSTANCE: signal simulator used is in form of at least micro-weighing chemically pure substances inside sealed cavities of a thermoacoustic waveguide rod (TAWR) with acoustic emission (AE) and temperature sensors, where the mass of said substances is determined with maximum accuracy and said substances have reversible anhysteretic temperature and energy of phase transitions (PT) of the first type (crystallisation/melting, evaporation/condensation), from which, in each cycle for heating and (or) cooling a sample in contact with the TAWR, by receiving AE signals of said PT and by simultaneously measuring contact temperature of the TAWR with the sample at PT points, temperature measurement channels and AE (sensors-amplifiers-converters) as a whole are checked and calibrated from temperature and energy characteristics of the PT of the first type of built-in thermodynamic acoustic-emission (TDAE) standards, by changing amplification coefficients or (and) threshold of sensitivity of measurement channels, or (and) amplitude-frequency characteristics (AFC) of temperature, electric and acoustic signal converters or (and) corresponding corrections when converting digital data to physical parameters. Possibility of TDAE standardisation is provided, which enables metrological support for thermal and (or) acoustic-emission analysis installations through dynamic and static inspection of their temperature and acoustic measurement channels.

EFFECT: increased reliability and accuracy of determining temperature and energy characteristics, stages for destruction of materials.

4 cl, 4 dwg

 

The present invention relates to the field of Metrology in thermal and acoustic emission analysis of substances, materials and products from them, as well as to develop new methods and tools for nano-, micro - and microdiagnostics solid materials.

The development of the modern energy, aviation and rocket-space technology, including nanomaterials and nanotechnology, placing increased demands on ensuring the uniformity of measurements of nano-, micro - and macrocharacteristics materials under operating conditions, determining the accuracy and reliability of the identification of changes in their mechanical, electrical and thermal parameters characterizing their properties and structure, affecting their durability and security.

The fact that cyclical changes in temperature, pressure, humidity and other conditions dramatically activate the processes of aging and degradation of physical-mechanical and chemical properties of a wide class of materials, polymers, composites, semiconductors and other underlying all these degradation processes is accelerated accumulation of structural defects, i.e. nano-, micro - and macrodactyla, ultimately leads to functional failures, and then to the destruction of the material.

So, now all the more urgent becomes the problem of diagnostics and identification of a hundred is the second nano-, micro - and macrodactyly substances, materials and products from them, which cannot be solved without the appropriate metrological support.

Known methods practical assessment stages of destruction of materials and phase transitions in them during heating/cooling change mass or linear dimension, mechanical or dielectric characteristics, as well as some thermodynamic parameters of heat capacity, enthalpy, etc. [Wendland Conventional Thermal methods of analysis, M.: Mir, 1978, 526 S., Bubnova R.S., Filatov S. Kaliev, Fotiev A.A. Thermal analysis and phase equilibria, Perm: Ed. The PSU. 1988, 155 S.], i.e. methods of thermal analysis (TA).

Many leading firms of the world, such as Perkin Elmer, NETZSCH, etc. that produce a variety of settings THAT implement separately the Tg, thermodilatometry (including pressure change), thermo-mechanical analysis, dielectric analysis and other methods THAT [http://www.netzsch-thermal-analysis.com/ru/products/]. At the same time, because of the "destructive nature" methods and metrological challenges in the certification of installations, implementing them, they have large errors and are used mainly for qualitative assessments. However, for the 100 years of its existence, the methods THAT were "captured" negative temperatures, as well as "onasteries" modern "non-destructive" methods: laser back flash. the Ki (LFA), dynamic mechanical analysis (DMA) and others, which expanded the number of defined and calculated parameters (thermal conductivity and thermal diffusivity, modules of elasticity, etc. with precision, allowing to certify some settings as a means of measurement. However, methods and tools for verification and calibration of temperature and energy measurement channels are made the old fashioned way - periodically and individually, as a rule, with the dismantling of the sensors, units and devices to test them on the master devices and reference sources.

In recent years, there has been the development of study materials and products by means of acoustic emission (AE), which is based on the recording and analysis of acoustic radiation resulting from changes in the structure and physico-chemical properties of substances and materials. Method AE allows you to record the temperature and the hysteresis of phase transitions (PT) in substances and materials, identify some of their thermodynamic and kinetic characteristics, including under repeated thermal and mechanical loading in the low and high temperatures. A distinctive feature of the AE method is its non-destructive character," in light of the study of dissipative processes leading to degradation of the materials and their "aging",determinative, including from the point of view of forecasting changes in their structure and properties in real operating conditions [VA Sinners, Drobot SHE Acoustic emission. M.: Publishing house of standards, 1976, 272 S., Triplin A.S., Bolo SR Acoustic emission. Physico-mechanical aspects. Rostov n/D: Publishing house of Rostov University, 1986, 160 S.].

At the same time, in the aspect of reliability of the results obtained by AE method, position, similar to the method of THE: method of AE and install, implement it, and is mostly used for qualitative estimations. Recent methods and means of verification of AE sensors and the simulated AE signals [RF Patent № 2267122 from 27.12.2005 "Multi-channel acoustic emission system for diagnostics of industrial objects and device for the recording and processing of acoustic emission signals"; Arabov VG, Zhukov A.V., Kuzmin, A.N. Practical evaluation of acoustic emission method for technological pipelines - W. "In the WORLD of non-DESTRUCTIVE testing No. 3 (41), September, 2008] do not allow in the process of testing materials sized measuring channels AE-plants as require special imitators and switch to AE sensors [Certificate TSI RU.C.28.036.A No. 15512 from 08.08.2008 "Complex acoustic emission measurement A-Line 32D"] or dismantling and validation of sensors, amplifiers and block education is otci signals separately [PB 03-593-03, decl. the resolution of Gosgortechnadzor of the Russian Federation dated June 9, 2003 N 77]that, firstly, it is not possible to automate these processes, and secondly, and this is important, does not provide the required reliability of measurements with long-term testing of materials, since the characteristics of the measuring channels (sensors, amplifiers, converters, etc.) "float" in the long run.

The proposed method and system, it handles that allow for dynamic and static verification and calibration of measuring channels in plants THAT, and AE-analysis, i.e. without dismantling and perform calibration of sensors, amplifiers, and blocks the processing of their signals separately.

Due to boom in the field of nanotechnology and nanomaterials demand for the proposed method and system, according to the authors, will increase as domestic or the foreign company will launch the installation, interfacing methods of thermal and acoustic emission analysis [Belozerov CENTURIES, Bolo SR, locust J.V. Combined thermogravimetric and acoustic emission method for determining the stages of thermal decomposition of substances and materials and device for its implementation - RF Patent № 2324923 from 20.05.2008; Belozerov CENTURIES, Barefoot SR, Bolo SR, Kryzhanovsky V.M. OCTAHEDRON: Opto-electronic heat acousto-by Electrometry the derivatograph - in Proc.. V Russian-Japanese seminar on "Equipment and analytical systems for materials science, micro - and nanoelectronics" / in 2 volumes, edited by Prof. Korotova L.V. /M: Misa, 2007, Vol.2, s-874].

Closest to the technical nature of the constituent parts of the claimed invention are as follows.

1. The ampoule to reproduce the temperature of the triple point of water ATT-1, intended for the verification and calibration of the reference resistance in accordance with the International temperature scale of 1990 (its-90), which uses a unique water quality - temperature triple point of water is 273.16 degrees Kelvin (0.01 degrees Celsius), which exist in equilibrium all three phases (crystalline, liquid and steam) and is the OP of the first kind - melting/crystallization of ice.

2. Multi-channel acoustic emission system diagnostics of structures (patent RF № 2217741 from 27.11.2003, the authors Stepanova L., Seriesnow A.N., V.M. Kruglov, Ants CENTURIES, wild Boars, S., Lebedev EJ, El'tsov AU), in which the control unit is configured to supply commands to the increase of the threshold, which is using digital to analogue Converter is set at the comparator input, and used the built-in simulator of AE signals, which allows to automatically determine the size of the AOR is localization in the control of complex objects.

3. Acoustic emission detector (RF patent No. 2078338 from 27.04.1997, the authors Thorn CENTURIES, Bigus GA, Dement'ev A.N., Cheburkin SCI), which implements the method of identifying the type of defect and the stage of its development on the spectral components of the AE signal by increasing the signal-to-noise by extracting the maximum spectral density of the analyzed AE signals, the frequency of which is determined by the type of defect.

4. The acoustic-emission method of quality control materials (AU No. 1320739, publ. 30.06.1987 in bull. No. 24, the authors of Bulo SR, Triplin A.S.)in which is recorded the spectral power density of the AE signals and the intensity of AE acts in the same frequency band, then the Poisson approximation of the flow is determined by the power in the entire frequency band, which is divided by the flow rate of AE acts, and obtained values of the energy of a single act AE judged on the quality of the material.

These methods and tools can be taken as prototypes of individual parts of the proposed method and system, it implements.

The objective of the present invention is to develop a method and system, thermodynamic, acoustic emission (TDAE) calibrate to implement the metrological provision of thermal and / or acoustic emission analysis by dynamic and static Prov is key to their thermal and acoustic measurement channels, than to increase the accuracy and precision of determining the temperature and energy characteristics of the stages of decomposition of substances and materials, etc.

This goal is achieved by the fact that in the proposed method as a signal simulator uses the built-in internal sealed cavity thermoacoustic rod-waveguide (TSV) with sensors acoustic emission (AE) and the temperature of the at least two micro weight of chemically pure substances, whose mass is defined as precisely as possible, with reversible temperature and hysteresis-free energy of phase transitions (PT) of the first kind (crystallization/melting, evaporation/condensation), which in each cycle of heating and / or cooling of the sample in contact with TSV, taking the AE signals specified FP and measuring simultaneously the temperature of the contact TSV sample points AF, tested and calibrated at the same time measuring channels of temperature and AE (sensors-amplifiers-converters) on thermal and energy performance of the OP of the first kind of built-in TDAE-standards, through changes of the gain and / or threshold sensitivity of the measuring channels and / or amplitude-frequency characteristics (AFC) converters thermal, electrical and acoustic signals and / or matched with the relevant amendments, when converting digital information into physical parameters.

If this is the determination of the coefficients of the energy dissipation on the ultrasonic radiation through the relationship of the measured spectral densities capacity of the AE signals in the limited actual measurement channels and TSV bands to the calibrated energies OP of the first kind, and relations computed full capacity of AE in the entire frequency band to these energies OP of the first kind, which can be used to estimate energy and identification processes of nano-, micro - and macrodactyly in the sample.

As chemically pure materials for TDAE-standards can be selected from any material featured MPTS-68 or its-90 (GOST 8.157-75). Authors of selected water and mercury, with the following characteristics OP the first kind [Physical encyclopedic dictionary / CH. edit Amerkhanov): Owls. encyclopedia, 1984, s; GOST 8.157-75, Appendix 7, tables 1 and 2]:

H2A: melting/crystallization - TTo=273), 16K (0,01°C) and ETo=334,0 kJ/kg (79,72 kcal/kg), and the evaporation - TAnd=373,15K (+100°C) and EAnd=2269,0 kJ/kg (539,0 kcal/kg);

Hg: melting/crystallization - TTo=234,C (-38,862°C) and ETo=11,9 kJ/kg (2,82 kcal/kg), and the evaporation - TAnd=629,K (+356,66°C) and EAnd=282,0 kJ/kg (E=69.7 kcal/kg).

If you need high caliber of the Cai can be entered third TDAE-reference Sn: melting/crystallization - TTo=505,K (+231,9681°C) and ETo=60,2 kJ/kg (14.4 kcal/kg), and the evaporation - TAnd=2543,15K (+2270,0°C) and EAnd=2520,0 kJ/kg (E=601,53 kcal/kg).

In particular, as mentioned micronano (weight measurement was conducted on the scales WZA-224 company Sartorius) were used:

"drop" of water - 0,501782, with energies of AF in these temperature points ETo=167,595 j and EAnd=1138,543 j, respectively;

the "ball" of mercury - 1,12459 g, with energies of AF in these temperature points ETo=13,383 j and EAnd=317,134 j, respectively.

The application of the above TDAE-standards in this case allowed us to obtain three "reference points" in each thermocycle test sample in thermocrete in operating conditions, i.e. when thermal Cycling in the temperature range from minus 65 to plus 100 degrees Celsius (-38,862°C; +0,01°C, +100,00°C), and two "reference points" when testing it on the heat and fire danger (GOST 12.1.044-90) in the electric furnace, i.e. to a temperature of plus 835 degrees Celsius (+100,00°C and +356,66°C).

The method is based on the following terms and ratios.

1. "The temperature of the shelves" AF stable in a wide range of heating rates of TSV sample or without it until all the substance TDAE-model is not converted from one aggregate state to another (figure 1 and 2), which is logged interval flow AE, fixed the future OP, therefore, in connection with the application as an embedded temperature sensor platinum thermometer-resistance (TC)with standard temperature characteristic, the temperature correction is performed on the output of the measuring channel, by changing the relevant amendments ΔWi converted to electrical parameters in temperature by the following formulas [GOST 8.157-75 PP, 2.5.2, applications 2-7]:

in the temperature range from 13,81 to 903,89 To -

where WTthe relative resistance of the platinum resistance thermometer, RTa platinum resistance thermometer at temperature T, R273,15the resistance of thermometer at a temperature of 273,15 K;

in the temperature range from 13,81 to 273,15 K -

where WCTthe relative resistance of the corresponding standard application functions 3 and table 4, ΔWi(T) - amendments at temperatures specified reference points (N2Oh, and Sn) are obtained from the measured values of WT(T) and corresponding values of WCT(T), is given in Appendix 5, and their differences in reference points are calculated using equations presented in Appendix 6, and the secondary reference point (Hg) - interpolation formula (in accordance with Annex 7, table 2), this correction function is:

on uchastke 90,188 to 273,15 K -

where t=T-273,15 K; And4and C4are constants determined from the values of the amendments (ΔWi=W-WCT), measured at the boiling point of water and mercury;

for the region from 0 to 630,74°C -

where;

a R(t') and R(0°C) resistance thermometer at temperatures t' and 0°C respectively; α and δ are constants determined by measuring the resistance at the triple point of water, the boiling point of water and mercury.

2. Range of AE in the OP of the first kind is a range of random Poisson stream of short acoustic pulses is 1/α. This allows you to appreciate the full power of AE - W across (from 0 to ∞) band on the measured spectral density G*(f) limited from f1to f2the band, which is approximated by the spectrum of a continuous random autoregressive process of first order [AC No. 1320739, publ. 30.06.1987 in bull. No. 24, the authors of Bulo SR, Triplin A.S.]:

and the power of AE is determined by integration:

Power W** approximating process in a limited band of frequencies equal to

Considering that the power of AE obtained from experimental range limited from f1to f2the frequency range equal to the power approximate the corresponding process in the same lane, ie W*=W**, get:

Where it is easy to determine the coefficients of the energy dissipation on the ultrasonic radiation by the formulas:

where Wi - power ultrasonic radiation OP of the first kind corresponding TDAE-model (i=Hg, H2O), EPP- energy OP of the first kind corresponding TDAE-model (i=Hg, H2O).

3. With the quality standards of the energy OP mentioned microlivestock, can be used to identify the stages of decomposition of acoustic emission thermodynamic parameter of damage (AATP)defining the structural-temporal state of the material [Prus J.V. stable acoustic emission characterization of the degree of damage kwasigroch materials - Izv. Higher education institutions. Physics, M., 1994, p.123-129]. The essence AATP is that the relative contribution of the intensity of accumulation of latent internal energy of destruction in the total power dissipation W increases as development of processes of damage and is uniquely determined by the expression:

where ΔE is the energy of a discrete sequence of pulses AE, ΔW is the total dissipation of energy in the time interval Δt.

Figure 1 different channels A-Line 32D reproduced the spectra and the AE pulses from the above TDAE-standards by evaporation of water (2 CH the l - 100°C) and mercury (channel 1 - 356,66°C), which clearly shows that the pulses of water" is shorter and the radiation power is higher than that of mercury, the density of which is higher than that of water. At the same time, the dissipation coefficients evaporation is practically identical and are

ToDfpv=At/EFPV=103,g/1138,j=9.1% and kDfpv=At*/1138,j=51,24/1138,j=4,5%;

ToDfpr=WP/ENRFs=29,g/317,j=9.2% kDfpr=Wp*/317,j=14,59/317,j=4,6%.

Figure 2 also through various channels A-Line 32D reproduced the spectra and the AE pulses from the above TDAE-standards, the formation of ice from water (2 channel - 0,01°C) and the solidification of mercury (channel 1 minus 38,862°C), showing a similar pattern except that in the spectrum of mercury is dominated by high-frequency processes, and the range of water - lower frequency. The coefficients dissipation crystallization is also the same and are

ToDfpv=At/EFPV=103,g/1138,j=9.1% and kDfpv=At*/1138,j=51,24/1138,j=4,5%;

ToDfpr=Wp/ENRFs=29,g/317,j=9.2% kDfpr=Wp*/317,j=14,59/317,j=4,6%.

Figure 3 is given a block diagram of a system implementing the inventive method, and figure 4-scheme of TSV.

Implementation of the described methodology was made possible by the creation of the measuring cell method TDAE calibrate - thermoacoustic rod-waveguide (TSV), representing (figure 4) pamesan the th special ceramic housing (2) molybdenum waveguide (1), in one of the ends of which contact with the test material, built two sealed TDAE-model (5, 6) and temperature resistance (4)connected to the respective conductors are laid in the channels of the ceramic housing, with terminals on it, located on a side near the opposite end of TSV with the AE sensor (3)attached to the other end of the specified waveguide, the ends of which are connected to the terminal block mounted on a ceramic body TSV, near the terminals of thermometer resistance.

This design TSV, as the test showed, allowed to measure the temperature of the sample surface with a precision of 0.01 degrees (because of the losses on thermal conductivity of molybdenum) and to perform heat insulation of the AE sensor from the temperature of the cooling/heating of the sample in the range from minus 65 to plus 835 degrees Celsius.

The implementation of the system TDAE-calibrate in the installation of AE-analysis (figure 3 a) temperature sensor TSV connects to the immittance meter (for example, E7-20), which connects to the computer, and the AE sensor is connected to the "free" channel setup AE-analysis, which also connects to the computer system. In this case (figure 5) for stationary inspection and calibration setup AE-analysis is a universal source of heat/cold (thermokarstic from whom the Lex "OCTAHEDRON" - Belozerov CENTURIES, Barefoot SR, Panchenko E.M., Udovichenko SCI Method synchronously-conjugate thermal analysis of substances and materials and installation for its implementation // Patent RF № 2343467 from 10.01.2009 on the application for invention No. 2006125486 from 17.07.2006), and dynamic calibration is implemented only if the temperature of the test material will reach some of the points the OP TDAE-standards.

The implementation of the system TDAE-calibrate in the installation (figure 3 b) TASW installed instead of the sample holder, and the temperature sensor TSV connects to a "free" channel temperature measurement setup TA, which in turn is connected to the computer system and the AE sensor connects to an 8-channel Board A-Line 32D (PCI-8) installed in your computer. In this case, for stationary and dynamic validation and calibration setup THAT uses the heat/cold of the installation THAT [for example, http://www.netzsch-thermal-analysis.com/ru/products/]. It should be noted that in this case, the set-up is THE "transformed" into a combined AE-TA (for example, AE-TG-DTG, or AE-TD-DTD, or AE-DSC etc).

The implementation of the system TDAE-calibrate in a combined AE-TA analysis (for example, Belozerov CENTURIES, Bolo SR, locust J.V. Combined thermogravimetric and acoustic emission method for determining the stages of destruction is exist and materials and device for its implementation RF patent № 2324923 from 20.05.2008; Belozerov CENTURIES, Barefoot SR, Bolo SR, Kryzhanovsky V.M. OCTAHEDRON: Opto-electronic heat acousto-electrometric derivatograph in Proc.. V Russian-Japanese seminar on "Equipment and analytical systems for materials science, micro - and nanoelectronics" / in 2 volumes, edited by Prof. Korotova L.V. / M: Misa, 2007, Vol.2, s-874), TSV installed instead of the applied TSV under the crucible-thermoelectrochemical and does not require a separate computer, and only install the system TDAE used in the controller and the computer (3"").

The inventive method and system are implemented and work as follows:

the stationary phase verification and calibration is performed each time before testing samples of materials by cooling TASW without the sample from room temperature to a temperature of 1 degree below the solidification of mercury (-38,862°C), and then heating it to a temperature of 1 ° C above the boiling point of mercury (+356,66°C), which results in comparison "passport data" TSV in its manufacture and acceptance testing with actual data paths "TSV measuring channels of temperature and AE used setup THAT or (and) AE and their adjustment to fit set accuracy, after which the calibration is saved and who is next to static checking, this is similar checks coefficients of energy dissipation;

stage dynamic validation and calibration in thermocycle, if the system is used in the combined unit AE and THAT is performed in each cycle of heating/cooling of the sample in contact with TSV by simultaneous registration of threads acts AE (intensity, spectral characteristics, amplitude and time parameters of AE signals) and temperatures not only the material being tested, but also the emerging phase transitions of the first kind in TDAE-standards when the temperature of TSV, the parameters and the corresponding algorithms of the controller corrects or characteristics of the measuring channels AE and temperature control modules, or their resulting values using relevant amendments, or both, and the computer program generates the actual database "nano - and microdistricts" sample, i.e. it tests on aging and operational sustainability;

stage dynamic validation and calibration when termomagnitnye, if the system is used in the combined unit AE and THAT is when termomagnitnye sample in contact with TSV to temperature plus 835 degrees Celsius to characterize thermal stability and fire hazard way of the simultaneous registration of threads acts AE (intensities, spectral characteristics of amplitude and time parameters of AE signals) and temperatures not only the material being tested, but also the emerging phase transitions of the first kind in TDAE-standards when the temperature of TSV, the parameters and the corresponding algorithms of the controller corrects or characteristics of the measuring channels AE and temperature control modules, or their resulting values with appropriate amendments, or both, and the computer program generates the actual database "macrodactyly" sample, i.e. it tests for resistance to heat and fire danger.

The applicant and the unknown thermodynamic methods acoustic emission calibration and technical solutions, which would be conducted static and dynamic calibration of temperature and acoustic measurement channels in General on the parameters of the OP of the first kind of built-in TASW TDAE-standards to improve the reliability and accuracy of measurements of nano-, micro - and macrocharacteristics materials.

Based on the above can be SCITI that the invention has significant differences from the prototype.

The claimed invention meets the condition of patentability "world novelty", as in the prior art is not identified on the basis of the Kie solve the same destination with the declared set of essential features of independent features in the claims.

The claimed invention meets the condition of patentability "inventive step", as in the prior art is not identified technical solutions with signs consistent with the features of independent features in the claims.

The proposed method and installation, his implements, will be used in the fire Test laboratories and Centers Metrology and certification for testing of substances and materials, and hence the goods from them on the subject of their safe use by consumers.

The proposed method and installation, it implements that will be used on objects of increased danger (NPP, TPP and so on), where durability and safety of the substances, materials and products are periodically checked, including state regulatory authority (Gosatomnadzor, legally).

The proposed method and installation, his implements, will find application in material science companies to monitor the stability properties of the produced nano-, micro - and micromaterials.

The proposed method and installation, his implements, will find application in scientific research institutes and design bureaus for scientific research and technological design ensure durability and security products for household, industrial and defense-space the ski application.

The proposed method and installation, his implements, will find application in technical Institutes and universities for research and teaching courses in physics, physical chemistry, mechanics, fire safety, etc.

1. The method of thermodynamic acoustic emission (TDAE) calibrate, characterized by the fact that as a signal simulator uses the built-in internal sealed cavity thermoacoustic rod-waveguide (TSV) with sensors acoustic emission (AE) and the temperature of the at least two micro weight of chemically pure substances, whose mass is defined as precisely as possible, with reversible temperature and hysteresis-free energy of phase transitions (PT) of the first kind (crystallization/melting, evaporation/condensation), which in each cycle of heating and / or cooling of the sample in contact with TSV, taking the AE signals specified AF and simultaneously measuring the temperature of the contact TSV sample points AF, tested and calibrated at the same time measuring channels of temperature and AE (sensors-amplifiers-converters) on thermal and energy performance of the OP of the first kind of built-in TDAE-standards by changes in the gain, or sensitivity thresholds of measuring channels, or (and) am litude-frequency characteristics (AFC) converters temperature, electric and acoustic signals, and / or appropriate corrections when converting digital information into physical parameters.

2. The way TDAE calibrate according to claim 1, characterized in that the determination of the coefficients of the energy dissipation on the ultrasonic radiation through the relationship of the measured spectral densities capacity of the AE signals in the limited actual measurement channels and TSV bands to the calibrated energies OP of the first kind, and relations computed full capacity of AE in the entire frequency band to these energies OP of the first kind, which can be used to estimate energy and identification processes of nano-, micro - and macrodactyly in the sample.

3. thermodynamic system acoustic emission (TDAE) calibrate thermal analysis (TA) and / or acoustic emission (AE) analysis, implementing automated dynamic and static verification and calibration of temperature and acoustic measurement channels installations (TA) and (or) AE, characterized in that it consists of a thermoacoustic rod-waveguide (TASW)contacting the test sample with one end, in which is embedded temperature sensor and at least two TDAE-model, and the other end with the AE sensor connected the units of measure the rhenium temperature and processing of AE signals, respectively, in the installation and (or) AE connected to the controller and the computer on which the software implemented algorithms for the management of these processes and data, and when heating/cooling TSV sample the signal processing unit AE provides synchronous registration characteristics of streams acts AE (intensity, spectral characteristics, amplitude and time parameters of AE signals), and the block temperature measurements - simultaneous registration of the values of the temperatures of the test material, but also in emerging phase transitions of the first kind in TDAE-standards when the temperature of TSV, the parameters and the corresponding algorithms of the controller corrects or characteristics of the measuring channels AE and temperature by using control modules, or their resulting values with appropriate amendments, or both, and the computer program generates the actual database of sample testing.

4. System TDAE calibrate according to claim 3, characterized in that the computer algorithm determines the total capacity of the AE in the entire frequency band, and calculates these rates of energy dissipation on the ultrasonic radiation, which can be used to estimate energy and identification processes of nano-, micro - and macrodactyly in the sample.



 

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SUBSTANCE: two equilateral triangles having side 1 with length shorter than 60 mm are placed on a component. The triangles are placed in a single plane and their bases are on a single line. The analysed space is placed on the extension of the plane of the triangles. Signal receivers AE are placed on vertices of the triangles. Time lag values t1, t2 and t3 for arrival of a signal from the source AE to the receivers are measured. The time lag values t1, t2 and t3 for arrival of the front of the signal from AE at the vertices of triangle vary in accordance with the following expression: t1=(l/υ)·sin(60°+φ), t2=(l/υ)·sinφ, t3=(l/υ)·sin(60°-φ), where φ is an angle measured anticlockwise between the bisector of the angle and direction of the defect, passing through the centre of the triangle. Angles φ1 and <φ1', which characterise the direction of the defect for the first and second triangle are determined using the formula φ11')=arcsin(t2/T), where T=l/υ is time for which sound passes through the component at distance equal to l, and t2 is the least time lag in each triangle. The point of intersection of directions which characterises the position of the defect in the component is determined.

EFFECT: increased accuracy and efficiency of determining position of defects during manufacture and use of components.

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FIELD: physics.

SUBSTANCE: signals from acoustic transducers and dynamic deformation from strain sensors are received and recorded. Parametres of acoustic emission signals are evaluated at the moment of loading the metal bridge structure with a passing train. Acoustic signals are digitised and pre-processed. Noise is filtered off and the arrival time of the acoustic signals is recorded and coordinates of developing defects are calculated from the said arrival time. The bridge structure is divided into N zones, in each of which strain sensors and four acoustic transducers, which form a piezoelectric antenna, are fitted. Recording of acoustic emission signals begins at the moment of detecting change in the deformation derivative sign to a positive sign and its overshooting a threshold value and stops at the moment of detecting change in the deformation derivative sign to a positive sign on another strain sensor in that zone. The location of the defect is determined from the difference in arrival time of signals in the piezoelectric antenna picking up the acoustic signals.

EFFECT: faster operation and improved accuracy characteristics with localisation of acoustic emission signals when diagnosing metal bridge structures.

2 cl, 4 dwg

FIELD: physics.

SUBSTANCE: to solve the aeroplane maintenance problem, the aeroplane is fitted with a constant monitoring device which has piezoelectric sensors. Signals from the sensors are detected in constant mode. Fatigue of critical parts of the aeroplane is determined from the said signals.

EFFECT: improved monitoring of critical parts, lower expenses on maintenance.

11 cl, 8 dwg

FIELD: measurement equipment.

SUBSTANCE: application: for control of items impregnation quality. Control of items impregnation quality is carried out with the help of acoustic emission event, at the same time energy and duration of acoustic signals in ultrasonic range of frequencies in impregnating autoclave, and completion of impregnation and finalisation of impregnating process are detected in case energy and duration of acoustic signals exceed threshold level of impregnation stage.

EFFECT: increased accuracy of impregnation process completion detection.

1 tbl, 5 dwg

FIELD: instrument making.

SUBSTANCE: invention relates to welded seam quality control equipment. Proposed method comprises receiving acoustic signals originating in welding zone with the help of wideband acoustic transducers displaced relative to each other and welded seam K, amplifying received acoustic signals and filtering them according to preset peak amplitude and high-frequency content of acoustic signal spectrum. It comprises also analog-to-digital conversion, recording the time of acoustic emission signal arrival to acoustic transducers and computing acoustic signal source coordinates. Results of acoustic-emission control allow plotting acoustic emission signal localization pattern and selecting active areas that feature increased amount of aforesaid signals. Note here that continuous signals are recorded in control process; their amplitude is averaged for preset time interval for obtained averaged values to be used to adjust the data conversion channel selection threshold for reception of acoustic signals in welding zone. Digital form of acoustic emission signal is used to cluster signal groups for every piezo antenna consisting of three acoustic transducers. Then, groups of clustered signal groups are isolated and localized. If critical number of cluster signals satisfying excess amplitude and frequency selection conditions is exceeded, welded seam should be rejected.

EFFECT: higher validity of flaw detection and accuracy of pinpointing defects in welded seam during welding and cooling.

2 cl, 3 dwg

FIELD: measurement equipment.

SUBSTANCE: application: for flaw detection in pipeline. Detectors are installed at the ends of investigated pipeline, oscillations generated by defect are registered, besides at the ends of investigated section of pipeline they install one piezoelectric detector, at least two own shapes of reference pipeline oscillations are selected, frequencies of own oscillations of reference pipeline are calculated, confident interval is generated by frequency characteristics of reference pipeline, then frequencies of own oscillations of investigated pipeline are registered by each of selected shapes of oscillations, comparison of investigated pipeline signals registered by detectors is carried out with a confident interval of reference pipeline, and whenever confident interval is exceeded, conclusion is made on availability of pipeline flaw, and to detect location of defect, signals registered by detectors are mutually correlated.

EFFECT: simplified process of flaw detection in pipeline and improved accuracy of defect location detection independently on properties of controlled item material.

2 cl, 1 dwg

FIELD: measurement equipment.

SUBSTANCE: application: to detect depth of local corrosion and track its development. One or several converters of acoustic emission are installed onto controlled item, signal oscillogram is registered, differs by the fact that signal oscillogram is used to define share nso of symmetric So Lamb wave in signal and/or share of nA0 of antisymmetric Ao Lamb wave in signal, an share or shares produced as well as their ratio is used to understand depth and development of corrosion.

EFFECT: improved information capacity of the corrosion defect detection process with the help of acoustic emission even by one signal produced at least by one converter of acoustic emission.

7 cl, 3 dwg

FIELD: power industry.

SUBSTANCE: method for determining slagging characteristics of ash for power station coals at flame combustion involves low-temperature ashing of the tested coal, manufacture of test sample from ash for investigation of physical ash properties at heating within temperature of 800°-1300°C with simultaneous fixture of deformation characteristics of the sample by means of measuring tool. Heating of sample in the above temperature interval is performed at constant heating rate of not less than 1.1 deg/sec, during which there determined is dependence of deformation speed of the sample on temperature of its heating; at that, temperature of beginning of ash slagging corresponds to maximum speed of sample deformation, and temperature of load-carrying flue gases at the furnace outlet corresponds to minimum deformation speed. Two to four test samples are subject to tests, and temperatures of the beginning of slagging and load-carrying flue gases at the furnace outlet are determined as arithmetic average of the appropriate values.

EFFECT: improving accuracy of determination of slagging characteristics of ash.

2 cl, 4 dwg

FIELD: nanotechnologies.

SUBSTANCE: nanodiamond is placed into installation for annealing, hydrogen is passed through and maintained at the temperature selected from the range of (900÷1100) °C, cooled down to room temperature. X-ray diffraction pattern is taken. Additionally spectrum of electronic paramagnetic resonance (EPR) is registered at room temperature. Availability of metal phases is identified.

EFFECT: invention makes it possible to increase sensitivity of magnetic admixtures content detection in nanodiamonds of detonation synthesis.

2 cl, 6 ex

FIELD: physics, optics.

SUBSTANCE: invention relates to methods of determining physical conditions at which phase transitions in metals and alloys take place. The method is based on joint analysis of the image of fragments of the surface of analysed material and luminance spectra of visible light reflected from the said surface, taken before and after the external physical action causing the phase transition. The analysis results are processed using special computer software.

EFFECT: invention simplifies diagnosis of phase transitions, increases accuracy and degree of automation of processing experimental results.

11 dwg

FIELD: physics, measurement.

SUBSTANCE: method involves experimental research of substance within temperature range beginning from T=0 K, measurement of heat capacity of substance within this range, and make conclusion on a zone of metastable substance state change by abrupt jump.

EFFECT: possibility to define zone of metastable state in substance.

4 cl, 11 dwg

FIELD: measuring technique.

SUBSTANCE: method can be used for measuring speed of phase transitions in movable structures provided with balance rings of domestic washers provided with dismounted top desk. Weight with mass of 0,5 kg is suspended inside drum of washer at height corresponding to center of gravity of internal movable part. Auto-balancing device is subject to cooling to temperature below 0°C to let solution inside hollow soldered metal balls freeze. Drum during process of cold air to come, inside for making solution freeze, is periodically driven into rotation and then it is stopped. Critical non-balanced mass of mechanical system is measured any time due to suspending additional weights and determining that masses of them, with which the drum touches wall of case. Speed of phase transitions is measured when solution gets frozen inside balls. Then test are conducted to study process of solution melting by using more perforated metal balls, for which purpose the balls are preliminary filled with ice or snow on base on high density solutions. To defrost solution, air compressor is turned on to pump warm air up inside cavity under drum. Drum is periodically driven into rotation and stopped during process of warm air intake. Critical un-balanced mass of mechanical system is measured any time by suspending additional weights to determine that mass of weights, at which mass the drum touches wall of case at rotation. Speed of phase transition in "solid body-liquid" system is measured during defrosting of solution.

EFFECT: improved precision of measurement.

8 dwg, 1 tbl

FIELD: heat-and-power engineering; other industries; installations for the scale formation analysis.

SUBSTANCE: the invention is pertaining to the scale formation analysis in the close to the industrial conditions at the controlled values of such parameters as the pressure and concentration of the salts in the working liquid. The installation for the scale formation analysis made in the form of the evaporation chamber includes: the installed with possibility of replacement heat-exchange system made in the form of the horizontal pipes with the electric heating elements located inside them, on which surfaces formation of the scale silt takes place; the system of feeding of the working liquid into the evaporation chamber and the mean for the steam condensation linked with the evaporation chamber by the steam withdrawal trunk. The installation is additionally supplied with the mean of the pressure control in the evaporation chamber, including the needle-type valve arranged in the steam withdrawal trunk and the system of withdrawal of the working liquid from the evaporation chamber including the needle valve mounted in the working liquid withdrawal trunk. The invention allows to expand the range of the conditions for analysis of the scale formation and to increase reliability of the analysis results.

EFFECT: the invention ensures expansion of the range of the conditions used for analysis of the scale formation and the increased reliability of the analysis results.

1 dwg

FIELD: thermometry.

SUBSTANCE: method provides usage of temperature detectors to transform electric signal, and identification of type of phase transition. Electric Signal from temperature detector is corrected for value of electric signal which is generated by phase transition of material. Correcting electric signal is achieved by means of additional probe.

EFFECT: improved precision of measurement.

4 cl, 9 dwg

FIELD: measuring technique.

SUBSTANCE: while warming sample up, average value of square of voltage of thermal electrical; fluctuations is measured at terminals of measuring converter. Maximal value, which corresponds to glass transition temperature, is measured, at which temperature the value of dielectric permeability is found and value of hardness coefficient is calculated. Method can be used for measurement of equilibrium hardness coefficient of polymer chains for polymers in unit.

EFFECT: improved precision of measurement.

1 dwg, 6 tbl

FIELD: measuring technique.

SUBSTANCE: method comprises testing two samples of the lubricant of the same mass, the first sample being tested without catalyzer and the second sample being tested in the presence of catalyzer, determining transparency coefficient by means of photometric measurements, plotting time dependences of the transparency coefficient, and determining oxidation stability of the lubricant from the equation presented.

EFFECT: enhanced precision.

3 dwg, 1 tbl

FIELD: measurement technology.

SUBSTANCE: method involves carrying out experimental temperature measurements of cooling liquid avalanche dissociation on hot surface under static conditions, without liquid flow being arisen.

EFFECT: simplified cooling liquid quality control process; reduced tested substance quantity in samples under test; personnel safety in carrying out tests.

1 dwg

FIELD: investigating or analyzing materials.

SUBSTANCE: thermograph comprises differential thermocouple and aluminum thermal unit provided with two symmetrically arranged cylindrical holes for crucible with specimen and standard. The crucibles are made of cylinders with caps provided with copper pipes for hot junctions of Chromel-cupel thermocouples. The wires of the thermocouples are housed in the two-channel ceramic rods. The thermoelectric heating of the unit is provided with the use of temperature-sensitive resistor made of nichrome wire. The unit is mounted in the steel sealed housing with a lid and provided with a device for locking it inside the housing during cooling and heating.

EFFECT: simplified design and enhanced accuracy of measuring.

1 dwg

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