V. A. GLUSHCHENKOV et al.: A NON-DESTRUCTIVE METHOD FOR EVALUATING THE ADHESION ... 3–8 A NON-DESTRUCTIVE METHOD FOR EVALUATING THE ADHESION BETWEEN THE LAYERS OF METAL-POLYMER-METAL COMPOSITE MATERIALS NEPORU[NE METODE ZA OVREDNOTENJE ADHEZIJE MED PLASTMI KOMPOZITNIH MATERIALOV V SESTAVI KOVINA-POLIMER-KOVINA Vladimir A. Glushchenkov 1 , Heinz Palkowski 2,1,3 , Rinat Y. Yusupov 1 , Denis A. Matveev 1 , Mikhail V. Khardin 1,* 1 Samara National Research University, Metal Forming Department, Samara, Russia 2 Clausthal University of Technology, Institute of Metallurgy, Clausthal-Zellerfeld, Germany 3 Clausthal Center of Materials Technology, Clausthal-Zellerfeld, Germany Prejem rokopisa – received: 2023-02-07; sprejem za objavo – accepted for publication: 2023-07-31 doi:10.17222/mit.2023.727 Development of a non-destructive measuring technique for evaluating the bonding quality of metal-polymer-metal composite sheet materials is introduced. Sufficient adhesion is necessary to ensure further shaping steps or bearing loads when used with- out failure due to delamination. Much attention is paid to determining the quality of gluing. According to the patent-literature review, no non-destructive measuring or quality control of layers’ bonding quality over the entire surface has been found. Thus, a new technical solution is proposed for defining the quality of bonding between the layers by means of electrodynamic repul- sion forces arising from the pulse current passing over the metal layers of a composite in the counter direction. The feasibility of the method is tested in laboratory conditions. For its implementation, the necessary values of the test parameters are obtained, i.e., the values of the current transmitted through metal layers. In addition, the possibility of detecting local defects of different shapes and sizes with the proposed method is estimated. Keywords: sandwich composite sheet, adhesion strength, magnetic pulse, non-destructive measurement V ~lanku avtorji predstavljajo razvoj tehnik neporu{nega testiranja in ovrednotenja kvalitete vezave med plastmi kompozitne "sendvi~" plo~evine vrste kovina-polimer-kovina. Dobra vezava (adhezija) med plastmi te vrste kompozita je potrebna zato, da plo~evina prenese nadaljnje stopnje preoblikovanja ali obremenitve, ne da bi pri tem pri{lo do delaminacije oziroma razslojevanja. Veliko pozornosti je namenjeno dolo~evanju kvalitete lepljenja. Med pregledom razpolo`ljive patentne literature za te vrste metod, metod neporu{nega merjenja ali kontrolnih metod kvalitete vezave med posameznimi plastmi po celotni povr{ini so avtorji ugotovili, da le-te v pisni obliki ali predpisih ne obstajajo. Avtorji v ~lanku predstavljajo novo tehni~no re{itev za dolo~itev kvalitete vezave med plastmi polimera in kovine na osnovi nastajajo~ih elektrodinami~nih odbojnih sil pri prehodu preko kovinskih plasti kompozita v nasprotni smeri. Izvedljivost metode so avtorji testirali v laboratorijskih pogojih. Za izvedbo te metode so ugotovili potrebne testne parametre, kot so na primer vrednosti jakosti toka, ki se prena{a s kovinskih plasti. Dodatno so ocenili tudi kak{ne so mo`nosti, da s predlagano metodo dolo~ijo lokacijo prisotnih napak, njihovo obliko in velikost. Klju~ne besede: kompozitne "sendvi~" plo~evine, adhezijska trdnost, magnetni pulzi, neporu{ne metode testiranja 1 INTRODUCTION Among the composite materials used in mechanical engineering, a special one is a multilayer sheet material consisting of covering metal layers and a polymer core, thus having a "metal/non-metal/metal" combination. 1,2 In the automotive industry, steel-polymer-steel sheets or combinations of aluminum and polymers are already in use. 3,4 A new 3-layered material of aluminum cover sheets and a PP/PE polymeric core, abbreviated as Al-P-Al, for aerospace and automotive applications is developed. Similar lightweight materials can also be used for medi- cal purposes, e.g., for prosthetic applications. 5 As shown in Figure 1, for the industrial use the man- ufacturing of such materials includes gluing of the metal and the polymer. To improve the quality of bonding, an epoxy is used in such cases as the promoter. However, in the case of biomedical use, epoxies have to be avoided. Here, other solutions have been developed. 5–7 For testing the bonding quality, destructive test meth- ods are used in general, such as shear tests or pull-off tests. They require the cutting of the samples for testing (witnesses), which helps us define, for example, the strength of gluing layers in case of their separation. For such pull-off tests, a glue with a bonding strength higher than that between the layers of a sandwich has to be used between the open surfaces of a metal and bracket. For metals, metal bonding glues with a pull-off strength of more than 25 MPa are available, making sure that failure by rupture will occur between the layers of a sandwich Materiali in tehnologije / Materials and technology 58 (2024) 1, 3–8 3 UDK 544.23: 621.792.4 ISSN 1580-2949 Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 58(1)3(2024) *Corresponding author's e-mail: Khardin.mv@ssau.ru (Mikhail V. Khardin) with their lower bonding strength. For its testing, a sand- wich is glued to the brackets of a testing machine and this set-up is loaded with tension until failure of the sandwich or the brackets. At the same time, mechanical adhesion is estimated, i.e., the fastening strength of the glued surfaces. 8 Up to now, no non-destructive method for determining the quality of the adhesive strength has been known. A number of non-destructive methods for detecting local defects (glueline/separation defect) with acoustic, radioscopic, optical and other physical methods are known and available on the market. 9–11 However, they do not allow estimating the adhesive strength quantitatively in the local area of a defect. 12 The absence of a reliable quantitative non-destructive method of controlling the quality of glued layers in a sheet composite material makes its use more difficult in the industry manufacturing high-quality parts. On the other hand, highly controlled quality of bonding opens up the possibility of a wider use of sheet stamping opera- tions in manufacturing parts from a multi-layer compos- ite material. 13 Consequently, the development of a non-destructive quality control method for the analysis of the bonding quality between the glued metal and poly- mer is of specific interest. 2 EXPERIMENTAL PART 2.1 Material and methods Currents induce magnetic fields. When a pulse cur- rent is fed in the oncoming direction along two closely located conductors, a pulsed magnetic field is formed around each of them. The interaction of these fields leads to the creation of electrodynamic repulsion forces. 14 Using this physical phenomenon, a non-destructive testing method for determining the quality of bonding between layers of Al-P-Al composite materials is pro- posed as sketched in Figure 2. Metal sheets (1 and 3) with a polymer foil (2) be- tween them are connected to the output of the magnetic pulse installation (MIU). 15 Their electrical closure is car- ried out using the bracket (5) and clamping slats (4 and 6). When the battery is discharged by MIU capacitors to the metal sheets, the pulsed current I flows in the counter direction. In this case, electrodynamic forces arise, af- fecting the separation. If the value of force F, generated by the field, is greater than the predetermined adhesive strength between the layers, delamination will occur; if it is lower (with a given stock ratio), the integrity of the material is not violated and the material is recognized as suitable for further processing. 2.2 Samples for experimental verification of the pro- posed technical solution For our experiments, a layered composite (Al-P-Al) was used with a total thickness of 0.9 mm, consisting of two aluminum sheets (AlMn) – each 0.3 mm thick – sep- arated by a 0.3 mm thick polymer foil. The mechanical properties of the AlMn alloy in the annealed state are listed in Table 1; 16 so are the ones for the polymer, a thermoplastic polyolefin (polypropylene, polyethylene and talc, PP/PE). 17 Table 1: Mechanical properties of the AlMn alloy and polymer, PP/PE Material state Young’s modulus, GPa Yield strength, MPa Ultimate tensile strength, MPa Elongation to rupture, % AlMn annealed 69 127.4 49 20 PP-PE 11 – 33 ± 11 500 2.3 Breakdown voltage of the polymer layer In the process of a working cycle, when connecting to the MIU, a high-voltage potential is generated be- tween the plates, which can lead to an electrical break- down of the polymer. That is why it is necessary to de- termine its breakdown voltage. The samples are connected to the high-voltage output of the AID-70M testing machine allowing the testing of electrical insulat- ing materials (dielectrics) up to 70 kV. To prevent sur- V. A. GLUSHCHENKOV et al.: A NON-DESTRUCTIVE METHOD FOR EVALUATING THE ADHESION ... 4 Materiali in tehnologije / Materials and technology 58 (2024) 1, 3–8 Figure 1: Basic technological operations used for manufacturing multilayer composite materials Al-P-Al Figure 2: Scheme of the non-destructive testing set-up for magnetic pulse installation (MIU) to determine the bonding quality in Al-P-Al sandwich composites face breakdowns (over the ends), the polymer foil pro- trudes the metal sheets by about 15 mm at all sides for the tests. For the experimental investigation, samples sketched in Figure 3 were used. As a result, the breakdown volt- age of the polymer is 17 kV. This makes it possible to carry out experiments to assess the quality of gluing in a wide range of MIU modes, with different values of the current transmitted through the layers, and determine the geometric sample dimensions to verify the proposed technical solution for the gluing quality control. 2.4 Determination of the adhesion strength between the composite layers At this stage of processing MPM materials, their ad- hesive strength is appraised using experimental results of the pull-off or shear tests, therewith defining a tolerable process window and keeping the processing parameters within this field. Up to now, there has been no indicator for evaluating the adhesive strength to be used in-line and as a non-destructive test. The method introduced be- low could be a solution to this issue. The evaluation of the adhesion strength is carried out on Al-P-Al sheet samples of 10 × 10 mm 2 . Extension cords are attached to the metal parts by spot laser weld- ing to fix them in the taps of a Tinius Olsen H5KT test machine. Figure 4 shows the typical force-elongation di- agram. Up to point A a pure elastic deformation of the test sample is given, while seperation between the Al-P lay- ers occurs within section A–B, see Figure 4. The experiments performed allow determining the adhesion strength indicator to be ~(40–50) N. This indi- cator has to be compared with the experimental values of the electrodynamic forces obtained with the proposed test method. 2.5 Determination of electrodynamic efforts The magnitude of the electrodynamic forces between two infinitely thin conductors of the same length is de- fined with equation (1) 18 FI I k k =⋅⋅⋅ ⋅ 0 12 4 F (1) where the magnetic air permeability μ 0 equals 4π×10 –7 H/m, I 1 , I 2 – currents flowing in the parallel conductors, k – geometric factor or circuit coefficient of the electro- dynamic forces, k F – coefficient taking into account the shape and size of conductors. The geometric factor depends on the length of the conductors, i.e., their range distances: k l a a l a l =⋅+ ⎛ ⎝ ⎜ ⎞ ⎠ ⎟ − ⎡ ⎣ ⎢ ⎢ ⎤ ⎦ ⎥ ⎥ 2 1 2 (2) l – length of the conductors, a – axial distance between them. Given that the distance between the conductors is sig- nificantly lower than their length, we get: k l a = 2 k F takes into account the shape of the cross-section of the conductors, that is, the form of the power lines of the magnetic field. This calculation is carried out with the help of Dwight’s diagrams. 19 The discharge current of the capacitor battery is vari- able. The value of I max is tens of kA. For the calculation, the following current equation is used: V. A. GLUSHCHENKOV et al.: A NON-DESTRUCTIVE METHOD FOR EVALUATING THE ADHESION ... Materiali in tehnologije / Materials and technology 58 (2024) 1, 3–8 5 Figure 3: Sample drawing for experimental studies of the adhesion strength Figure 4: Indicator chart of testing for the separation of Al-P-Al sand- wich I I D = max 2 Given the same current value for both conductors (in our case, for both sheets of the composite) we obtain an expression to calculate the maximum electrodynamic force: FI l a k max =⋅⋅⋅ − 10 72 DF (3) For the sample dimensions used in the experiments (a = 0.6 mm, b = 0.3 mm, H=10mm,L = 100 mm) it is not possible to find the proper k F coefficient in Dwight’s diagram, as with (a–b)/(h+b) = 0.03 and h/l = 30; a curve with such values is missing there. To find the fitting values of the electrodynamic forces affecting the separation of the composite layers, the method of their determination through the kinematics of the strip moving under the action of these forces is pro- posed. On two non-glued plates, the current also skips in the counter direction. The emerging electrodynamic force causes acceleration on one of the sheets (F = m·a). High-speed recording of this process allows us to photo- graph the kinematics of the central free-moving strip in the initial time stage and calculate the value of F. Figure 5 present the principal sketch of the measur- ing arrangement created for this purpose and the devices used. 20 The principle of the operation is as follows: launch- ing of the camera (6) and charging of the battery to the desired level of the magnetic-pulse installation capaci- tors take place simultaneously (1). Both the light source and the synchronization unit (3) are activated (7) due to the signals from the computer (4) and the camera (6). The synchronization unit with a defined delay gives off a triggering pulse to the discharge of the magnetic-pulse installation and the oscilloscope sweep (2). The delay time (delay) of the discharge current is less than 1 μs. At the same time, the signal of the discharge current from sensor 9 is recorded with the oscilloscope. A diagram of the operation of the measuring set-up is shown in Figure 6. The first graph shows the longest cycle of the camera sweep drive. Below is the charging cycle of the capaci- tors that provide the subsequent pulsed discharge. Next, the backlight turns on to ensure filming. When the lamp is in the operating mode during time t 1 , synchronization occurs; after interval t 2 the magnetic-pulse installation is turned on and the capacitor bank is discharged. Simulta- neously with the beginning of the discharge, the camera is turned on, carrying out frame-by-frame shooting. The frame frequency (FPS) of shooting in the experi- ments is 29740 frames/s. Consequently, the time be- tween the frames is 33.6 μs. Figure 7 shows four frag- ments of the sample movement. Starting with the third 6 Materiali in tehnologije / Materials and technology 58 (2024) 1, 3–8 V. A. GLUSHCHENKOV et al.: A NON-DESTRUCTIVE METHOD FOR EVALUATING THE ADHESION ... Figure 7: Fragments of recording the layer repulsion process Table 2: Dependence of the sample movement on time Sample movement, mm Time t,s ·10 –6 00 0 33.6 0.4·10 –3 67.2 1.2·10 –3 100.8 Figure 5: Sketch of the measuring arrangement for recording the movement of the strip under the influence of electrodynamic load 1 – magnetic-pulse installation, 2 – oscilloscope, 3 – synchronization unit, 4 – computer, 5 – display, 6 – high-speed film camera, 7 – pulse backlight, 8 – sample, 9 – pulse current sensor Figure 6: Diagram of the operation of the measuring set-up frame (67.2 μs), the sample is observed, as indicated by the arrows. Numerical results of processing the records are given in Table 2. The obtained values allow calculating the accelera- tion (a = 531462.49 m/s 2 ) and, knowing the mass of the moving section (m = 0.25 × 10 –3 kg), the electrodynamic force (F = 132.87 N). In addition, the data obtained allow us to get the value of the k F and apply it in further calculations: k F Ik F D = ⋅⋅⋅ = ⋅⋅ ⋅ = −− max . . 210 13287 2 10 295602 125 0006 72 7 Thus, all the necessary values included in Equation (1) are obtained to determine the electrodynamic forces arising from the non-destructive quality control of the composite layers. 3 RESULTS The purpose of the experimental studies is to find the dependence of the force of the metal strip – adhesive strength – on the value of the current transmitted by the metal layers, i.e., to find the minimum current value, at which a high-quality sandwich sample remains undam- aged while delamination is observed in a sample with a weak bond. After each discharge, a visual and instrumental con- trol of the samples is carried out for the impairment of the adhesive strength of the layers: possible deformation of the metallic layers is recorded using a simple dial gauge. In the absence of any defects, indicated by deforma- tions, a sample is connected again to the MIU and a higher current is created. The current is measured using a RGA belt (a current sensor) and its value is presented on the oscilloscope screen. Results of testing defect-free specimens are listed in Table 3. Table 3: Experimental results: height of sample delamination h at cur- rent flow I d Sample no. Current I d ,k À Height of delami- nation h,mm 1 12.83 0 13.59 0 14.16 0 16.57 0 17.50 0.19 2 15.86 0 17.11 0.17 3 15.80 0 17.19 0.15 Thus, with a current value of (17.11–17.50) kA, a delamination between metal an polymer is observed, having a bulge of around (0.15–0.19) mm. This current value corresponds to an electrodynamic force of (44–46) N, which corresponds to the experimentally ob- tained value of the force of (40–50) N (see Figure 4). The results obtained allow a construction based on the dependence of the electrodynamic force on the value of the pulse current passed through the metal layers of the three-layered Al-P-Al composite (Figure 8). If the adhesion strength (F set ) is specified for a com- posite material in technical conditions, then, considering the safety coefficient – for example, 1.2 (F set /1.2) – we find the adequate value of the current being tested (cur- rent I) with the help of the constructed graph (Figure 8), and through it, we determine the condenser discharge en- ergy of the magnetic-pulse installation, which must be used for a non-destructive test. If, with this current value (discharge energy of the capacitor battery), no delami- nation is observed, the logical conclusion is that the bonding quality corresponds to the required one. V. A. GLUSHCHENKOV et al.: A NON-DESTRUCTIVE METHOD FOR EVALUATING THE ADHESION ... Materiali in tehnologije / Materials and technology 58 (2024) 1, 3–8 7 Figure 8: Dependence of the electrodynamic force on the current flow through the metal layers Figure 9: Samples with local defects 4 DISCUSSION 4.1 Possibility to use this method to detect local defects This non-destructive method is suitable for determin- ing the quality of bonding in general. The question to be answered now is how sensitive it is, e.g., when detecting local defects in a bonding structure. Therefore, three-lay- ered Al-P-Al samples with the same dimensions as be- fore were used, but with pre-established macroscopic lo- cal defects of different dimensions in the core material. Circles with diameters of 3, 6, 8 mm, located in the cen- ter of the composite as single circles or several ones set in a row were cut into the polymer, see Figure 9. An increase in the diameter of the defects leads to a decrease in the current, at which delamination of a sam- ple occurs. In all the cases, the place of the gap defect is clearly seen when the current is passing through. The analysis of defective samples carried out during the test has shown that delamination in an Al-P-Al sand- wich with a circular defect of 3 mm and height of 0.1–0.3 mm is observed at a current, I d , of (16 ÷ 17) kA. The variation in the values for one testing set is ex- plained by the differences in the bonding quality of each sample (standard deviation) and placing the defects (geo- metrical deviations). However, according to the data ob- tained we can see some dependence of the current mag- nitude required for delamination on the size of the defect: the smaller the diameter of the defect, therewith the ratio of the defect, the higher is the force (current) re- quired for delamination of the layers. The observed local deformation of the strip above the defect proves the possibility of using the proposed method of control for detecting local defects as well. 5 CONCLUSIONS A non-destructive method for testing the quality of bonding between the layers in Al-P-Al composite sheet materials, i.e., metal/dielectric intermediate layer/metal, is introduced. The first experimental tests show its basic applicability. Defects due to delamination can be de- tected and correlated with electrodynamic forces and currents. Moreover, implemented defects of a macro- scopic size lead to a characteristic change in the currents needed for delamination, depending on the size of a de- fect. This method also has a potential for detecting smaller defects in such composites. 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