Film/Substrate Adhesion Assessment by Scratch Tests Performed With Different Indenters

2014 ◽  
Author(s):  
Vincent Le Houérou ◽  
Leandro Jacomine ◽  
Christian Gauthier
Keyword(s):  
Interfacial Adhesion ◽  
Scratch Test ◽  
Scratch Resistance ◽  
In Situ Observation ◽  
Brittle Behavior ◽  
Adhesion Measurement ◽  
Extensive Growth ◽  
Energy Dissipated ◽  
Film Substrate ◽  
Industrial Solutions

In most cases, scratching of the surface of a polymeric glass elicits brittle behavior and industrial solutions like coating have been successfully used to improve the scratch resistance. The origin of the success of the coating technique is still of great research interest since one of the limitations of this technique is the risk of cracking and chipping. In terms of interfacial adhesion characterization, a wide variety of methods have been used to assess this property of material systems. Nevertheless, the adhesion of coatings still remains to be successfully determined in a test which can reproduce the damage undergone by the coated surface during its real lifetime. In this context, scratch test constitutes a good candidate. The present study deals with the scratching technique as an interfacial adhesion measurement in coated systems. Using a single-asperity scratching device allowing in-situ observation of the scratch, the fracture of a thin nano-composite coating deposited on its substrate was investigated under different conditions of temperature and scratching speed. Four types of fracture kinetics were observed depending on these two variables. One of these exhibits a stable blister growth at the same speed as the movement of the indenter over hundreds micrometers. This slow and extensive growth of a blister was obtained at 80 °C at a scratching speed of 10 μm/s. When the blister has reached a certain size, it propagates with the indenter without increasing further in size: it constitutes the steady state blister growth. A variational form of the energy balance of a blistering process is proposed, which permits to assess the adhesion of the system. Actually, the energy spent in the delamination process can be determined by following the delaminated area during the blistering process with regard to the scratching distance. The main difficulty is to estimate the energy dissipated in plastic flow. Different tests were conducted with various indenters: spheres with different radius and roughness. Thanks to this multi-criterion approach, it was possible to fit a unique value of the adhesion in the case of experimental stable blistering growths. The results are discussed with regard to reliability and probe characteristics.

Determination of the Adhesive Strength of Film-Substrate Interfaces Using the Constant Depth Scratch Test

1995 ◽  
Vol 390 ◽  
Author(s):  
I. Dutta ◽  
J. C. Campbell
Keyword(s):  
Aluminum Nitride ◽  
Interfacial Adhesion ◽  
Polycrystalline Diamond ◽  
Sample Surface ◽  
Scratch Test ◽  
Constant Depth ◽  
Theoretical Formulation ◽  
Set Up ◽  
Film Substrate

ABSTRACTA constant depth scratch test (CDST) has been recently developed to quantify the shear strength of film-substrate interfaces. This test is capable of measuring interfacial adhesion as a function of position on the sample surface during a continuous scratch. Unlike many of the currently available tests which are applicable to a limited array of materials systems, or are experimentally complex, this test is quite versatile, and is relatively straightforward to conduct and interpret because of the constant depth geometry. The theoretical basis and the experimental set-up for the test have been previously presented. In this paper, extensions of the theoretical formulation to account for different debonding behaviors of different film-substrate systems are discussed. Experimental results generated with a number of systems, including chromium on glass, gold on aluminum nitride, gold on aluminum nitride with a chromium inter-layer, and polycrystalline diamond on aluminum nitride are presented.

Measurement of Adhesion at Film -Substrate Interfaces by Constant Depth Scratch Testing

1994 ◽  
Vol 338 ◽  
Author(s):  
I. Dutta ◽  
D. P. Lascurain ◽  
E. D. Secor
Keyword(s):  
Interfacial Adhesion ◽  
Interfacial Shear Strength ◽  
Scratch Test ◽  
Interface Strength ◽  
Constant Depth ◽  
Scratch Testing ◽  
Glass Substrates ◽  
Film Substrate ◽  
Scratch Tests ◽  
Theoretical Developments

ABSTRACTQuantitative tests for interfacial adhesion between films and substrates are of criticalimportance in micro-electronic applications. However, many of the available tests are applicable to a limited array of materials systems, or are experimentally complex. In thispaper, a constant depth scratch test, which has been designed to circumvent the limitations associated with currently available tests, is presented along with theoretical developments for the quantification of interfacial shear strength. Because of a fixed scratchgeometry, the test is amenable to straightforward analytical formulations unlike other versions of scratch tests. It is unique in its experimental simplicity, and allows evaluation of interface strength as function of position on the sample. Sample outputs from the test based on Cr films on glass substrates are presented.

Evaluation of Abrasive Wear of Polymeric Materials Using Single-Pass Pendulum Scratching

2002 ◽  
Author(s):  
Marcelo Torres Piza Paes ◽  
Antonio Marcos Rego Motta ◽  
Lauro Lemos Lontra Filho ◽  
Juliano Ose´ias de Morais ◽  
Sine´sio Domingues Franco
Keyword(s):  
Deep Water ◽  
Wear Mechanisms ◽  
Degradation Mechanism ◽  
Single Point ◽  
Polymeric Materials ◽  
Scratch Resistance ◽  
Wear Behaviour ◽  
Sediment Layer ◽  
Materials Used ◽  
Energy Dissipated

Scratching abrasion due to rubbing against the sediment layer is an important degradation mechanism of flexible cable in deep water oil and natural gas exploitation. The present study was initiated to gain relevant data on the wear behaviour of some commercial materials used to externally protect these cables. So, Comparison tests were carried out using the single-point scratching technique, which consists of a sharp point mounted at the extremity of a pendulum. The energy dissipated during the scratching is used to evaluate the relative scratch resistance. The results showed, that the contact geometry strongly affects the specific scratching energy. Using SEM imaging, it was found, that these changes were related to the operating wear mechanisms. The observed wear mechanisms are also compared with those observed on some cables in deep water operations.

Interfacial adhesion of nanoporous zeolite thin films

2006 ◽  
Vol 21 (2) ◽  
pp. 505-511 ◽  
Author(s):  
Lili Hu ◽  
Junlan Wang ◽  
Zijian Li ◽  
Shuang Li ◽  
Yushan Yan
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Interfacial Adhesion ◽  
Interfacial Strength ◽  
Future Generation ◽  
In Situ Growth ◽  
Seeded Growth ◽  
Si Substrates ◽  
Film Substrate

Nanoporous silica zeolite thin films are promising candidates for future generation low-dielectric constant (low-k) materials. During the integration with metal interconnects, residual stresses resulting from the packaging processes may cause the low-k thin films to fracture or delaminate from the substrates. To achieve high-quality low-k zeolite thin films, it is important to carefully evaluate their adhesion performance. In this paper, a previously reported laser spallation technique is modified to investigate the interfacial adhesion of zeolite thin film-Si substrate interfaces fabricated using three different methods: spin-on, seeded growth, and in situ growth. The experimental results reported here show that seeded growth generates films with the highest measured adhesion strength (801 ± 68 MPa), followed by the in situ growth (324 ± 17 MPa), then by the spin-on (111 ± 29 MPa). The influence of the deposition method on film–substrate adhesion is discussed. This is the first time that the interfacial strength of zeolite thin films-Si substrates has been quantitatively evaluated. This paper is of great significance for the future applications of low-k zeolite thin film materials.

Experimental and Three-Dimensional Finite Element Study of Scratch Test of Polymers at Large Deformations

2004 ◽  
Vol 126 (2) ◽  
pp. 372-379 ◽  
Author(s):  
J. L. Bucaille ◽  
E. Felder ◽  
G. Hochstetter
Keyword(s):  
Strain Hardening ◽  
Penetration Depth ◽  
Large Deformations ◽  
Numerical Study ◽  
Scratch Test ◽  
Scratch Resistance ◽  
Plastic Strains ◽  
Thermosetting Polymer ◽  
Scratch Tests ◽  
Hardening Coefficient

An experimental and numerical study of the scratch test on polymers near their surface is presented. The elastoplastic response of three polymers is compared during scratch tests at large deformations: polycarbonate, a thermosetting polymer and a sol-gel hard coating composed of a hybrid matrix (thermosetting polymer-mineral) reinforced with oxide nanoparticles. The experiments were performed using a nanoindenter with a conical diamond tip having an included angle of 30 deg and a spherical radius of 600 nm. The observations obtained revealed that thermosetting polymers have a larger elastic recovery and a higher hardness than polycarbonate. The origin of this difference in scratch resistance was investigated with numerical modelling of the scratch test in three dimensions. Starting from results obtained by Bucaille (J. Mat. Sci., 37, pp. 3999–4011, 2002) using an inverse analysis of the indentation test, the mechanical behavior of polymers is modeled with Young’s modulus for the elastic part and with the G’sell-Jonas’ law with an exponential strain hardening for the viscoplastic part. The strain hardening coefficient is the main characteristic parameter differentiating the three studied polymers. Its value is equal to 0.5, 4.5, and 35, for polycarbonate, the thermosetting polymer and the reinforced thermosetting polymer, respectively. Firstly, simulations reveals that plastic strains are higher in scratch tests than in indentation tests, and that the magnitude of the plastic strains decreases as the strain hardening increases. For scratching on polycarbonate and for a penetration depth of 0.5 μm of the indenter mentioned above, the representative strain is equal to 124%. Secondly, in agreement with experimental results, numerical modeling shows that an increase in the strain hardening coefficient reduces the penetration depth of the indenter into the material and decreases the depth of the residual groove, which means an improvement in the scratch resistance.

scholarly journals Scratch Behaviour of Silicon Solid Solution Strengthened Ferritic Compacted Graphite Iron (CGI)

2018 ◽  
Vol 925 ◽  
pp. 318-325
Author(s):  
Rohollah Ghasemi ◽  
Anders E.W. Jarfors
Keyword(s):  
Solid Solution ◽  
Normal Load ◽  
Scratch Test ◽  
Scratch Resistance ◽  
Compacted Graphite Iron ◽  
Depth Of Penetration ◽  
Scratch Depth ◽  
Compacted Graphite ◽  
Diamond Indenter ◽  
Different Content

The present study focuses on scratch behaviour of a conventional pearlitic and a number of solid solution strengthened ferritic Compacted Graphite Iron (CGI) alloys. This was done by employing a single-pass microscratch test using a sphero-conical diamond indenter under different constant normal loads conditions. Matrix solution hardening was made by alloying with different content of Si alloy; (3.66, 4.09 and 4.59 wt%. Si) which are named as low-Si, medium-Si and high-Si ferritic CGI alloys, respectively. A good correlation between the tensile and scratch test results was observed explaining the influence of CGI’s matrix characteristics on scratch behaviour both for pearlitic and fully ferritic solution strengthened ones. Both the scratch depth and scratch width showed strong tendency to increase with increasing the normal load, however the pearlitic one showed more profound deformation compared to the solution strengthened CGI alloys. Among the investigated alloys, the maximum and minimum scratch resistance was observed for high-Si ferritic CGI and pearlitic alloys, respectively. It was confirmed by the scratched surfaces analysed using Scanning Electron Microscopy (SEM) as well. In addition, the indenter’s depth of penetration value (scratch depth) was found as a suitable measure to ascertain the scratch resistance of CGI alloys.Keywords: Silicon solution strengthening, CGI, Abrasion, Scratch testing, Scratch resistance

Validity of Adhesion between Films and Substrate with Friction-Detected Scratch Test

1993 ◽  
Vol 308 ◽  
Author(s):  
Ru Wang
Keyword(s):  
Friction Coefficient ◽  
Critical Load ◽  
High Speed ◽  
Sudden Change ◽  
High Speed Steel ◽  
Scratch Test ◽  
Optical Microscope ◽  
Film Substrate ◽  
Film Failure ◽  
Ti Films

ABSTRACTThe validity of Lc of film failure is studied with friction — detected scratch test . The specimens used in the experiment are ion-plated TiN and Ti films,Chemical-Plated NiPCu films on steel of various hardness,ion beam mixed plated TiN films on optical glass,The morphology of failed films was studied under optical microscope and scanning electronmicroscope,The composition of starting failure of films was analyzed with electro — probe. It is found that in the curves of scratch tests of ion-plated TiN and Ti films on high-speed steel,the load corresponding the sudden change of the horizontal force is the same as the critical load of film failure,however,the critical load obtained in the scratch test of the ion-plated TiN and Ti films on soft steel is the some deference compared with optical microscope analyzed, that is principally due to the property of films and substrates (hardness and coefficient).The morphology and mechanism of ion — plated TiN and Ti films on high —speed steel are also studied in the paper.The adhesion between film and substrate is an effective method in evaluating the films property. After apprasing the effectiveness of acoustic emission monitoring scratch test, someone think that no matter coated with hard or soft film it is effective on the brittle hard substrate. However,there exist errors to different extent on other film-substrate system,and the scratch test is inapplicable for soft film-soft substrate system[1]. P. A. Steinmann pointed out while studying the factors influnceing the critical load Lc,that friction coefficient is a key factor on Lc,it provided valuable information in measuring Lc,but it think it is imporsible to measure Lc totally dependent on sudden change friction or friction coefficient, howeveer, for a specific coating substrate system,it is acceptable to say that Lc is dependent on friction coefficient[2]. This paper study experimentally on the friction detected scratch test and found out that effectiveness of Lc varies substantially in different film-substrate system. The author studiied the regularity of various system and discuse the season. The failure morphology and principles of ion-plated TiN and Ti film on highspeed steel are also analyzed in this paper.

Controlled Plasma Nitriding for an Optimum Balance between PACVD TiBN Coating Scratch Resistance and Substrate Toughness

2008 ◽  
Vol 373-374 ◽  
pp. 312-317
Author(s):  
Y. He ◽  
I. Apachitei ◽  
Jie Zhou ◽  
Twan Walstock ◽  
J. Duszczyk
Keyword(s):  
Fracture Toughness ◽  
Plasma Nitriding ◽  
Scratch Test ◽  
Scratch Resistance ◽  
Diffusion Layers ◽  
Load Carrying ◽  
Duplex Process ◽  
Duplex Surface Treatment ◽  
Composite Hardness ◽  
Optimum Balance

The plasma nitriding (PN) process in the duplex surface treatment was controlled to create nitrided diffusion layers with depths of 0, 5, 15 and 80 m in the substrate of the DIN 1.2367 hot-work tool steel with the maximum microhardness values of 600, 700, 820 and 1000 HV, respectively. The scratch properties, i.e. the critical loads of cohesion (LC1), adhesion (LC2), breakthrough (LC3) and worn out (LC4), of the PACVD TiBN coating (boride, 5-7 at.%) on these substrates increased linearly with the maximum hardness of the PN diffusion layer. Instead of the composite hardness, the peak scratch hardness was used to describe the load-carrying capacity of the TiBN coating and PN substrate. Deep tensile cracks in the PN substrate with a hardness value of 1000 HV formed during the scratch test at a load as low as 90 N, indicating the low fracture toughness of the substrate. Therefore, an optimum balance between the scratch properties of the coating and the good fracture toughness of the nitrided substrate must be achieved through exercising the control of the PN and PACVD duplex process.

scholarly journals Воздействие дуплексной обработки на механические свойства нержавеющей стали марки 316L

2020 ◽  
Vol 46 (21) ◽  
pp. 14
Author(s):  
А.С. Гренадёров ◽  
А.А. Соловьёв ◽  
К.В. Оскомов
Keyword(s):  
Mechanical Properties ◽  
Surface Hardness ◽  
Chemical Vapor ◽  
Scratch Test ◽  
Nitrogen Plasma ◽  
Nitrogen Atmosphere ◽  
Hydrocarbon Films ◽  
Ion Plasma ◽  
316L Steel ◽  
Film Substrate

The results of experimental research on modifying the surface layer of 316L steel by duplex treatment are presented. The latter includes ion-plasma treatment in a nitrogen atmosphere with subsequent plasma-enhanced chemical vapor deposition of hydrocarbon films doped with silicon and oxygen (a-C:H:SiOx). Mechanical properties of steel surface (hardness, modulus of elasticity, plasticity index, plastic deformation resistance) were determined by the nanoindentation method, and adhesion of the films was evaluated by a scratch test. It was found that the greatest improvement in the mechanical properties of the film-substrate system occurs after the deposition of a-C:H:SiOx film on a surface previously hardened in a nitrogen plasma.

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