Non-destructive testing methods and apparatus
11275036 · 2022-03-15
Assignee
Inventors
Cpc classification
International classification
Abstract
A non-destructive testing method of analyzing a sample comprising a composite material is disclosed. The method comprises: emitting an electromagnetic signal onto the sample, the electromagnetic signal having a range of frequencies; detecting a response signal transmitted and/or reflected by the sample in response to the electromagnetic signal; processing the response signal to determine variation with frequency of a dielectric permittivity of the sample over the range of frequencies; and determining an indication of a structural characteristic of the sample from a measure of the variation with frequency of the dielectric permittivity of the sample.
Claims
1. A non-destructive testing method of analyzing a sample comprising a composite material, the method comprising: emitting an electromagnetic signal onto the sample, the electromagnetic signal having a range of frequencies; detecting a response signal transmitted and/or reflected by the sample in response to the electromagnetic signal; processing the response signal to determine variation with frequency of a dielectric permittivity of the sample over the range of frequencies; and determining an indication of a structural characteristic of the sample from a measure of the variation with frequency of the dielectric permittivity of the sample, wherein the sample comprises a continuous conductive filler and/or a non-continuous conductive filler.
2. A non-destructive testing method according to claim 1, wherein the structural characteristic of the sample comprises a defect level, a conductive filler concentration and/or a conductive filler dispersion level.
3. A non-destructive testing method according to claim 1, wherein the range of frequencies is within the range 0.1 KHz to 300 GHz.
4. A non-destructive testing method according to claim 3, wherein the range of frequencies is within the range 1 GHz to 300 GHz.
5. A non-destructive testing method according to claim 4, wherein the range of frequencies is within the range 8 GHz to 13 GHz.
6. A non-destructive testing method according to claim 1, wherein the measure variation with frequency of the dielectric permittivity of the sample is a standard deviation.
7. A non-destructive testing method according to claim 1, further comprising comparing the measure of the variation with frequency of the dielectric permittivity of the sample with a threshold criterion or a plurality of threshold criteria and evaluating the structural characteristic of the sample as a result of the comparison.
8. A non-destructive testing apparatus for analyzing a sample comprising a composite material, the apparatus comprising: an emitter configured to emit an electromagnetic signal onto the sample, the electromagnetic signal having a range of frequencies; a detector configured to detect a response signal transmitted and/or reflected by the sample in response to the electromagnetic signal; a network analyzer configured to process the response signal to determine variation with frequency of a dielectric permittivity of the sample over the range of frequencies; and a computing device configured to determine an indication of a structural characteristic of the sample from a measure of the variation with frequency of the dielectric permittivity of the sample, wherein the sample comprises a continuous conductive filler and/or a non-continuous conductive filler.
9. A non-destructive testing apparatus according to claim 8, wherein the emitter and the detector are integrated in a probe.
10. A non-destructive testing apparatus according to claim 8, wherein the structural characteristic of the sample comprises a defect level, a conductive filler concentration and/or a conductive filler dispersion level.
11. A non-destructive testing apparatus according to claim 8, wherein the range of frequencies is within the range 0.1 KHZ to 300 GHz.
12. A non-destructive testing apparatus according to claim 11, wherein the range of frequencies is within the range 1 GHz to 300 GHz.
13. A non-destructive testing apparatus according to claim 12, wherein the range of frequencies is within the range 8 GHz to 13 GHz.
14. A non-destructive testing apparatus according to claim 8, wherein the computing device is configured to calculate the measure of variation with frequency of the dielectric permittivity of the sample as a standard deviation of the dielectric permittivity.
15. A non-destructive testing apparatus according to claim 8, wherein the computing device is further configured to compare the measure of the variation with frequency of the dielectric permittivity of the sample with a threshold criterion or a plurality of threshold criteria and evaluating the structural characteristic of the sample as a result of the comparison.
16. A non-destructive testing method of analyzing a sample comprising a composite material, the method comprising: emitting an electromagnetic signal onto the sample, the electromagnetic signal having a range of frequencies; detecting a response signal transmitted and/or reflected by the sample in response to the electromagnetic signal; processing the response signal to determine variation with frequency of a dielectric permittivity of the sample over the range of frequencies, wherein the measure variation with frequency of the dielectric permittivity of the sample is a standard deviation; and determining an indication of a structural characteristic of the sample from a measure of the variation with frequency of the dielectric permittivity of the sample.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
(1) In the following, embodiments of the present invention will be described as non-limiting examples with reference to the accompanying drawings in which:
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DETAILED DESCRIPTION
(27) Embodiments of the present disclosure relate to the dispersion evaluation and/or defects detection of composites containing conductive fillers or reinforcements. The present disclosure is based on a completely new mechanism and working principle in comparison to other existing or previously reported non-destructive measurement methods.
(28) The working principle can be related to two generic theories proposed by John Pendry concerning the change of the number and effective mass of free electrons on individual conductive particles (wires) when they approach in close proximity. This change, which is also related to the plasmonic effect of electrons, becomes discontinuous when the inter-particle distance is below certain value. On the other hand, the number and effective mass of free electrons also affects the particles interaction with the electromagnetic wave, according to Lorentz-Drude theory. Therefore, the electromagnetic wave signal from a conducting particle dispersed material system, e.g., permittivity, carries information or signature of interaction or dispersion state of the particles. This is shown schematically in
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(30) A close analogy of using information form ‘noise’ level was reported in a study on corrosion of a metallic material. In the study, noise analysis of electrochemical noise (ECN) was conducted. ECN is an electrochemical technique in which the potential and/or current signals that arise directly from the electrochemical reactions (corrosion) taking place on an electrode surface are measured and interpreted. In this work the equipment (an electrochemical workstation) tracks extremely small current and voltage fluctuations or noise among three electrodes made from the material of interest in a corrosion medium. Current is measured between two electrically coupled electrodes (a working electrode and a counter electrode), while the third electrode is connected between the working electrode and a pseudo reference electrode to measure the voltage. The measured stochastic pulses or oscillation of current/potential are related to different corrosion events such as rupture, cracking, discrete events involving metal dissolution (e.g., pitting) etc.
(31) However, the stochastic ECN signal is used to detect corrosion, while in the methods described herein the oscillation of permittivity level is used to evaluate dispersion or distribution state of the discontinuous conductive fillers in the composites or defects in the continuous conductive fillers reinforced composites. In addition, the permittivity oscillation is not necessarily stochastic in the tests because most of the tests are done in static condition when the dispersion or defect states are fixed in a given composite or different regions of a composite material.
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(33) The probe is a structure that guides electromagnetic waves with minimal loss of energy by restricting expansion to one dimension or two. Without the physical constraint of a probe, electromagnetic wave amplitudes decrease as they expand into three dimensional space. In this method, a probe transfers electromagnetic wave energy to and from the network analyser. The probe can be changed based on the testing requirement/environment.
(34) The sample 140 is a composite material comprising a conductive filler. The conductive filler may be based on carbon, metal and others, and distributed in a non-conducting matrix, e.g, polymer, hybrid, glass or ceramics. The composite material comprises a discontinuous or continuous filler. The dimensions of filler can be 0D, 1D and 2D, in which the size of filler can be nano-scale, micro-scale and millimeter-scale.
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(36) In step 302, the probe 110 emits an electromagnetic signal onto the sample 140. The network analyzer 120 generates the electromagnetic signals which are varied in frequency. In some embodiments the frequency is varied in the x-band, that is between 8 GHz and 13 GHz. However, embodiments of the present invention are not limited to the x band. The present invention is also applicable for non-ionizing frequency range of 0.1 KHz to 300 GHz and preferably in the range of 1 GHz to 300 GHz for practical applications.
(37) In step 304, the probe 110 receives and detects a response signal transmitted and/or reflected by the sample 140. In step 306, the network analyzer 120, processes the receive signal to determine the dielectric permittivity of the sample 140 for different frequencies. The network analyzer 120 generates data representing the variation of the dielectric permittivity of the sample with frequency. This data is received by the computer 130.
(38) In step 308, the computer 130 determines an indication of a structural characteristic of the sample. The structural characteristic of the sample may be fiber woven/braiding structure, orientation, defects and impurities introduced during manufacturing, fiber breaking, delamination, debonding, matrix damages and other defects due to fatigue, aging, or other damage. The structural characteristic may be to detect stochastic defects, including dynamic defects and static defects formed during manufacturing, assembling or service. The structural characteristic may be a measure of the concentration of the filler.
(39) In step 308, the computer determines a measure of the oscillation of the dielectric permittivity of the sample with frequency. This measure may be the standard deviation of the dielectric permittivity of the sample over the frequency range.
(40) The standard deviation (SD) may be calculated using the following formula:
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where (x.sub.1, x.sub.2, . . . , x.sub.n) are the data point values of the sample,
(42) In step 308, the computer may compare the calculated standard deviation with a calibration curve to determine the dispersion behavior of the conductive filler in the sample.
(43) As described above, for discontinuous fillers, the SD could be used to determine the dispersion behaviour of the filler. For continuous filler, the SD could be used to determine the structural defects in the sample by comparing with the sample curve without structural defects.
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(46) The probes may be connected to a section of rectangular waveguide 412a or coaxial airline 412b. One end of the probe is connected to the signal source (Port 1) of the network analyzer and the other end of the probe is terminated at the measurement port (Port 2) of the network analyzer. The signal source at Port 1 generates a uniform transverse electromagnetic (TEM) wave propagating along the transmission line test jig and the wave will be detected at Port 2 as a voltage signal.
(47) The sample thickness I has effects on the parameters like permittivity (E), permeability (μ), reflected signal (S11) and transmitted signal (S21). The theory is based on the equations below.
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z: impedance; n: refractive index; K.sub.0: the wave number of the incident wave; I: sample thickness
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(50) As shows in
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C.sub.0: air capacitance; ω: Angular frequency
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t: sample thickness; ε.sub.0: permittivity of free space,
ε.sub.0=8.854×10.sup.−12 F.Math.m.sup.−1
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Example 1
(55) Several surfactants (i.e., Span 80, Triton X-100 and polyvinyl pyrrolidone) were employed to facilitate dispersion of CNTs in a polymer matrix. The matrix was thermoplastic polyurethane (TPU), which was supplied in the form of pellets. 200 mg Raw-CNTs were added into 400 g acetone and ultrasonically dispersed for 1 h. Then, 200 mg surfactant was incorporated into CNTs suspension followed by the addition of 36 g 10% TPU in cyclohexanone solution. The TPU/surfactant-CNTs solution was further ultrasonically mixed in ultrasonic bath at room temperature. The solution was poured into a PTFE mold and dried in 80° C. oven to obtain a solid film.
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(57) As can be seen from
(58) The dielectric permittivity of the four samples shown in
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(60) The standard deviation was calculated using the formula given above for 201 values of the dielectric permittivity in the range 8.2-12.4 GHz.
(61) As can be seen from
Example 2
(62) In order to evaluate the sensitivity of this methodology, thermoset PU was employed. The thermoset PU was fabricated by mixing Part A (hardener) and Part B (polyol), which have different molecular structures. Raw CNTs were incorporated into PU at the concentration of 5 wt % and 10 wt %.
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(64) As shown in
(65) As shown in
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Example 3
(68) It is inevitable that CNTs aggregate when CNTs loading increases. Thus, a series of PU/CNTs composites were prepared by varying the CNTs concentration from 1 wt % to 8 wt %. CNTs were dispersed in acetone for 1 h, followed by addition of Part A (hardener) and continuous 3 h ultrasonication. After a formation of homogeneous CNTs suspension, the mixture was concentrated by rotary evaporation, and further added into a three-neck flask containing stoichiometric Part B (polyols). The composites were obtained by casting the solution into a PTFE mould and subsequently removed the solvent at 60° C. for 24 h.
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(70) As indicated in
Example 4
(71) Examples 1-3 demonstrate that the new method is accurate, sensitive and reliable for 1D CNTs. 0D carbon black and 2D graphene were studied as well. Here, we investigated the relationship of oscillation of dielectric permittivity of 0D and 2D filler filled composites with the filler concentration. As mentioned above in Example 3, it is inevitable that fillers aggregate when increased filler loading.
(72) Various amount of 0D carbon black (2D graphene) were dispersed in acetone for 1 h, followed by addition of Part A (hardener) and continuous 3 h ultrasonication. After a formation of homogeneous suspension, the mixture was concentrated by rotary evaporation, and further added into a three-neck flask containing stoichiometric Part B (polyols). The composites were obtained by casting the solution into a PTFE mold and subsequently removed the solvent at 60° C. for 24 h.
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(77) From
Example 5
(78) The present disclosure is based on the quantification of the oscillation of permittivity to evaluate the state of continuous conductive filler in composites. According to theories, the electrons in conductive fillers and interfacial polarization between fillers and matrix would be influenced by fillers' environment, resulting in the changed oscillation of complex permittivity.
(79) Woven carbon fibre is a type of continuous conductive filler. In this example, commercial woven carbon fibre was employed to prepare carbon fibre reinforced polymer composite (CFRP) and verify the disclosed methodology. The detection on defects in CFRP by this method is not only focused on static detection, but applicable for stochastic damages occurred during the assembling of small pieces of CFRP. During the manufacturing of CFRP, three main factors determining the final properties of CFRP should be taken into account: 1) unwoven fibre randomly dispersed inside; 2) impurity; 3) orientation of carbon fibre mats.
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(81) As shown in
(82) As shown in
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(85) As is shown in
(86) Another important parameter for CFRP fabrication is the orientation of carbon fibre mats, which is closely related to the mechanics of products. In order to demonstrate the relevance of the non-destructive testing methods to the determination of relative orientation of carbon fibre mats, orientations of 0 degree and 45 degree in CFRP were prepared.
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Example 6
(89) In addition to the defects during manufacturing, defects that form during the use of CFRP can also be detected by the non-destructive testing method. These defects include fibre breaking, de-bonding between fibre and matrix, delamination and so on. In order to demonstrate the detection of such defects by the non-destructive testing method, three types of defect were simulated as shown in
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(91) As shown in
(92) As shown in
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(94) The above examples demonstrate that the non-destructive testing methods may be used to identify characteristics of the internal structure of composite materials. The methods may also be used to detect different defects and the precise dispersion state detectable by proper calibration according customized requirements. For example, a criterion to evaluate filler dispersion (and distribution) and defect level (excellent, good, satisfactory and bad) may be established based on the calculated standard deviation.
(95) This method described in this invention allowed the simple, direct and non-destructive evaluation of conductive filler dispersion (and distribution) or detection of the defects in CFRC composites. By monitoring and quantifying the oscillation of dielectric permittivity, the localized filler dispersion and defects can be evaluated.
(96) The method mentioned in this disclosure have been verified by various conductive fillers and matrices. The composites containing conductive fillers are promising in many commercial and military applications, such as electromagnetic interference shielding, lightning-strike protection microwave absorption, anti-corrosion, thermal diffusion, electrically conductive composites and carbon fibre reinforced composites.
(97) This method can be carried out with commercially available instruments (Vector Network Analyser) by connecting a computer, to directly quantify the oscillation of dielectric permittivity. The non-destructive testing method opens up a new dimension to determine the filler dispersion (and distribution) and defects detection. Attributed to the sensitive response of fillers to electromagnetic signal, this method could be one of the most sensitive methods in the field of non-destructive testing.
(98) Whilst the foregoing description has described exemplary embodiments, it will be understood by those skilled in the art that many variations of the embodiments can be made within the scope and spirit of the present invention.