MXPA00008237A - Test apparatus and method of measuring mar resistance of film or coating - Google Patents

Test apparatus and method of measuring mar resistance of film or coating

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Publication number
MXPA00008237A
MXPA00008237A MXPA/A/2000/008237A MXPA00008237A MXPA00008237A MX PA00008237 A MXPA00008237 A MX PA00008237A MX PA00008237 A MXPA00008237 A MX PA00008237A MX PA00008237 A MXPA00008237 A MX PA00008237A
Authority
MX
Mexico
Prior art keywords
sample
analysis
indentor
scratch
tip
Prior art date
Application number
MXPA/A/2000/008237A
Other languages
Spanish (es)
Inventor
Li Lin
Original Assignee
Ei Du Pont De Nemours And Company
Li Lin
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ei Du Pont De Nemours And Company, Li Lin filed Critical Ei Du Pont De Nemours And Company
Publication of MXPA00008237A publication Critical patent/MXPA00008237A/en

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Abstract

This invention concerns a test apparatus and procedure used for quantitative and qualitative characterization of scratch and mar behavior of films or coatings, more particularly automotive coatings. The apparatus includes a micro-indentor that penetrates and scratches the coating to be characterized together with interrelated components for measuring the force applied, the length and depth of the identor penetration, the geometry of the disturbed coating surface as well as means for measuring, analyzing and comparing test results.

Description

ANALYSIS DEVICE AND METHOD FOR QUANTIFYING THE RESISTANCE TO DETERIORATION OF A FILM OR COVERING Background of the Invention The present invention is generally oriented to the analysis of the mechanical properties of films and coatings, and more particularly is directed to analyzing the resistance to deterioration and scratches of the coatings and to an analysis apparatus that is used in the present. In principle, the process of. deterioration can be caused by the contact of a coated surface, with a solid body in motion, which induces wear on the coated surface. An example of the deterioration process can be observed in automotive body coatings, which are typically exposed to damage by abrasive elements, such as dust, dirt, surface wear during a car wash and REP .: 122031 action of the elements in the open. The deterioration of the coated surface results in a loss of its aesthetic appearance. Scratches or deterioration of a coated surface is especially undesirable in translucent or pigmented coatings that have a lot of luster. The resistance to deterioration and scratches of a coating depends on the physical properties, such as the stress limit, hardness, Young's modulus and resistance of the coating composition. The above physical properties are greatly affected by the properties, such as the glass transition temperature, and the chemical structure of the polymers included in the coating compositions. Therefore, the quantification of scratch resistance and deterioration of the coating becomes very important in the selection of components, such as polymers, which are used in the coating compositions. For example, when comparing the resistance to deterioration of a coating composition containing a type of polymer against that containing a different polymer, this can be used to decide which polymer is best suited to provide a coating with an optimum luster to long term with other physical properties. A method, which is intended to rub a sandpaper of a well-defined structure, in a prescribed manner, against a coated surface to induce damage to the covered surface. The multiple points of contact in the sand particles of the sandpaper induce damage, which is then quantified visually, typically on a scale of 0 to 10, where the number 10 does not represent any damage and 0 represents a total damage . Alternatively, the damage that is induced in a coating is compared visually against damage in a coating with a different coating composition under the same conditions of analysis to determine which coating has less damage. However, due to the subjective nature of any visual observation, which tends to vary from person to person, the above analyzes are not objective enough. In addition, sandpaper, although standardized, tends to have different grain structures, which can greatly affect the damage that occurs in the coating. It is also very difficult to quantitatively quantify the damage produced by multiple points of contact of the sand particles in the sandpaper. In addition, the digital pressure that is applied by the analyzer during the prescribed rubbing action tends to vary. As a result, the damage resulting from this also tends to vary from one analysand to the next. Therefore, there is a need for a deterioration resistance analysis apparatus that is less subjective and much more reproducible than the non-reproducible subjective analysis methods currently used. An apparatus is described in the literature by Wu in J. Mater. Res., Vol. 6, No. 2, pages 407 to 426, February 1991. The apparatus defined in that article is not robust enough for reproducible quantifications on a wide variety of coated substrates under conditions of high specific yield.
Brief Description of the Invention The present invention has as an objective an apparatus for quantifying the resistance to deterioration of a sample of analysis comprising: A system for conducting the indentor, this system is mounted on a support support of this apparatus which comprises: A system for driving the indentor which has an indentor placed in it, and a system to perceive the path of this indentor to and from the surface of this sample of analysis; and A system for directing the sample of analysis, this system is placed on a base of this apparatus comprising: A fastening system to ensure this sample of analysis to it, with the surface of this sample of analysis in perpendicular relation with the indentor , and a mounting means for traversing the analysis sample in a direction tangential to that of the indentor, such that when the indentor tip is simultaneously driven in this analysis sample, a scratch occurs on the surface of the film or area. The present invention is also directed to a method for quantifying the resistance to deterioration of a test sample comprising: securing this test sample in a mounting system of an apparatus; place an indentor in relation perpendicular to the exposed surface of this sample of analysis, in such a way that the tip of this indentor is in contact with this surface of this sample of analysis; drive this tip of this indentor on the surface of this sample of analysis at a certain speed while simultaneously running the analysis sample in a tangential direction relative to the indentor at a certain speed in a certain direction to scratch this surface of this sample of analysis and so produce a scratch on it.
Brief Description of the Figures Figure 1 is an interpretation of a three-dimensional atomic pressure microphotograph (AFM) of a micro-scratch that occurs during the visco-plastic deformation of a film or coating. Figure 2 is an interpretation of a three-dimensional AFM of a micro-scratch that occurs during the fragmented deformation of a film or coating. Figure 3 is a schematic design of various components of an apparatus of the present invention. Figure 4 is a three-dimensional view of the means for conducting the injector of the apparatus of the present invention. Figure 5 is a perspective view of the means for conducting the injector of the apparatus of the present invention. Figure 6 is a three-dimensional schematic view of the means for directing the analysis sample of the apparatus of the present invention.
Figure 7 is a plan view of a fastening system and a portion of a mounting system of the system for directing the analysis sample of the apparatus of the present invention. Figure 8 is a side view taken along the section of lines 8-8 of Figure 7. Figures 9, 10 and 11 are graphs showing the results of a typical micro-scratch experiment obtained at use the apparatus of the present invention.
Detailed Description of the Preferred Modalities As used herein: A "film" means a substantially flat unfixed layer, such as a polyester film or sheet A "coating" means an adherent layer of a composition of a coating that is applied to a surface of the substrate . The apparatus and method of this invention are directed to the quantification of the resistance to deterioration and scratches of a film or coating. The apparatus produces a micro-scratch on a coated surface to be analyzed that closely mimics the deterioration and scratch resistance typically seen on a film or coated surface. The phenomenon of scratching and damage by deterioration is complex and the applicant has determined that a microgrooder or rail that is left on a coated surface during scratching and damage by deterioration have two distinct elements. Damage due to deterioration, as seen in Figure 1, may be in the form of a substantially uniform rail that occurs during the visco-plastic deformation of the film or coating, or, as seen in Figure 2, may be in the form of a Rail with cracks that occurs during fractured deformation of the film or coating. The visual effect of these two different types of damage to the observer is significantly different. The applicant has discovered that the damage shown in Figure 1 is much more noticeable to trained experts than to the ordinary person, while the damage shown in Figure 2 is remarkable, even for the ordinary person who is not trained to look for such defects. Therefore, the present invention provides a much more objective analysis that is capable of inducing such damages in the coating under predetermined reproducible conditions. The present invention generally provides an analysis apparatus having means for deforming, i.e., micro-scratching, an analysis surface, capturing the deformation information in graphical and visual form of the analysis surface, and analyzing scratch damage. The diagrams in Figure 3 provide the various components of the analysis apparatus 1 of the present invention. The analysis apparatus 1 includes a base 2 positioned on a platform 3 which is substantially insulated from vibrations to substantially prevent the transmission of vibrations to the apparatus 1. Conventional systems for the reduction of vibrations, such as air dampers ( not shown) are well suited to support platform 3. An example of a system for vibration reduction is the Research Series Table Top Model No. RS4000-48-12 supplied by Newport Corporation, Irvine, California. The base 2 is provided with a support bracket 4 having a mechanical arm 5 which is mounted on it. The mechanical arm 5 is preferably adjustable, so that the mechanical arm 5 can be positioned above or below the support support 4. The system for driving the indentor 6 is fastened to the mechanical arm 5. The system for directing the The analysis sample 8 is placed in the base 2. The apparatus 1 also includes a conventional computing system 10, such as an IBM compatible computer which works with the Windows® NT Operating System which is available from Microsoft Corporation of Redmond, Washington. The computer system 10 includes a 12 A system for , conditioning the input and output signals from and to the driving system of the indentor 6 and a system for directing the analysis sample 8 to control the movements of an indentor 32 placed in the driving system of the indentor 6 and a sample of analysis 56 (shown in Figures 6 and 8), which may be in the form of a film or coating that is applied onto a substrate. The movements of the indentor 32 and of the analysis sample 56 are controlled according to a computation program that is provided by LABVIEW® Version 5.0.1 Programmable Software available from the National Instrument Company of Austin, Texas. The computer system 10 also includes conventional systems for producing processable data resulting from scratching the surface of the analysis sample 56; conventional systems for storing the processable data; and systems for viewing the processable data in a graphical or visual form, such as on a CRT 12 screen or on a chart plotter (not shown). A video system 14 is used to capture the deformation that occurs on the surface of the sample of analysis 56 during the experiment, and to carry out afterwards the analysis of the damage by the scratch. Also a video system 14 is very useful for placing the indentor-32, for leveling the sample of analysis 56, and for configuring the experiments. The video system 14 is a conventional system, which preferably is connected to a conventional video recording system (not shown) to store the images that are produced in the video system 14 during the experiment. Optionally, a microscope (not shown) can be used to observe the damage to the analysis coating. Preferably, the apparatus 1 is placed inside a thermally insulated chamber (not shown) to maintain all the components of the apparatus 1 at a constant temperature, preferably at room temperature. Preferably, a series of light sources are strategically placed within the isolated chamber to make adjustments to various components of the apparatus 1 and to illuminate the tip of the indentor 32 and the surface of the sample of analysis 56 during the video capture of a scratch that occurs on the surface of the sample of analysis 56 during the analysis. In greater details, Figures 4 and 5 show the details for the driving system of the indentor 6 that includes the system 7 for the impulse of the indentor having the indentor 32 placed there and a system 9 for perceiving the path of the indentor 32 towards and from the surface of the test sample 56. The system 7 for the injector impulse includes an immobile support 14 attached to the mechanical arm 5. Both ends of a mobile clamp 20 are connected to the immobile support 14 by means of a first flexible means 22 that is connects to the ends of the clamp 18 of the stationary support 14 in order to provide a single degree of freedom to the movable clamp 20. The ends of the clamp 24 of a movable clamp 20 are connected to both ends of a clamping part of the indentor 28 by means of a second flexible system 30 to provide a one-degree freedom to the indentor holder part 28. The first flexible system 22 and the second flexible system and each one includes a pair of diaphragm springs which are connected to each end of the clamps 18 and 24 of the stationary support 14 and the mobile clamp 20, respectively. The diaphragm springs are made of an iron-nickel alloy, available from Hamilton Precision Metals, Inc. of Lancaster, Pennsylvania, which not only has a constant elastic modulus over a wide temperature range and high pressure production, but also This alloy has a lower coefficient of thermal expansion compared to other spring materials. The above-described double cantilevered beam structure of fixed ends of the first flexible system 22 and of the second flexible system 30 is designed to resist against the bending states and tangential pressures in such a manner, that only a single degree of freedom is allowed, generally in a vertical direction. The indentor 32 is positioned centrally on the indentor plate 28, equidistant from either end of the indentor plate 28 to further ensure that the indentor 32 is provided with only one degree of freedom of movement, i.e. without undulating movements or rotary. The shape of the tip of the indentor 32 can be rounded with a radius in the range from one miera to 10 microns. Alternatively, it may have a pyramidal shape. The tip of the indentor 32 is made of diamond, corundum, topaz or quartz. The degree of desired hardness of the tip depends on the hardness of the test sample 56. Diamond tip is preferred. A prototype of the indentor 32 is available in indentor from the Synton Company of Lyss, Switzerland, which has a rounded tip with a radius of 3 microns. The system for the pulse 7 of the indentor also includes an energy system 16 placed on a stationary plate 14. A drive core 17 of an energy system 16 is fixed to a mobile clamp 20, such that when the system energy 16 is energized, the movable clamp 20 and the indentor plate 28 having the indentor 32 positioned therein, run only in a direction perpendicular to that of the surface of the analysis sample 56. The, energy system 16, of Preferably, it includes a low-voltage piezo-transducer (LVPZT) and a controller, which provide power to the LVPZT. These LVPZT are stretched when an electrical voltage is applied. Therefore, one is able to provide accurate and continuous movement to the indentor 32 in a predetermined manner. The total movement of the indentor 32 is up to about 90 micrometers with a resolution of 2 nanometers that can be obtained by using the Model LVPZT Nos. P-840.60 or P-841.60 together with its controllers, available from Physi Instremente, (Pl) GmBH & Co, through its subsidiary Polytec Pl Inc. of Auburn, Massachusetts, with an operating voltage of up to 120 Volts. The resulting normal pressure that is experienced on the surface of the analysis sample 56 is up to 100 milli-newtons with a resolution of 2 micro-newtons. The system 9 for sensing the path of the indentor 32 to and from the surface of the analysis sample 56 includes a first perception system 34, which quantifies the penetration of the tip of the indentor 32 into the analysis sample 56 and a second detection system. perception 36 for quantifying the normal pressure experienced by the analysis sample 56 when the tip of the indentor 32 penetrates the analysis sample 56. The first perception system 34 and the second perception system 36 respectively generate data on the penetration of the tip and normal pressure, which are transmitted to the system to condition the input and output signals 12 A of the computer system 10. Based on this data, the system 12 A controls the energy that is supplied to the power system 16 and the movements of the indentor 32 and of the sample of analysis 56 in accordance with the computer program provided by the computer system 10. A prime The immobile component of a first sensing system 34 is mounted on a pair of support studs 38 positioned on either side of the immobile support 14 and of the movable bracket 20. The support studs 38 which are fixed to the immobile support 14 they allow the mobile clamp 20 and the indentor bra 28 to move freely. A first mobile component of a first sensing system 34 is mounted on the indentor holder 28, such that when the holder of the indentor 28 travels, the interspace between the first immobile component and the first moving component of the first system perception 34 varies according to the movement of the fastener 28, therefore it generates an analogous output, which is transmitted to the system to condition the input and output signals 37 A. Similarly, a second immobile component of a second perception system 36 it is mounted on a movable clamp 20 and a second movable component of a second sensing system 36 is mounted on the indentor holder 28, such that when the holder of the indentor 28 travels, the intermediate space between the second immobile component and the second moving component of the second perception means 36 varies according to the normal pressure experienced by the analysis sample 56, and therefore, generates an analog output signal, which is transmitted to the system to condition the input and output signals 12 A. The first perception system 34 and the second perception system 36 may be the same, such as, for example, the capacitive sensor Model D-050-00 available from Physik Instremente, (Pl) GmBH & Co, through its subsidiary Polytec Pl Inc. of Auburn, Massachusetts. Figures 6, 7 and 8 provide details for the system 8 to direct the analysis sample. Figure 6 provides details of the mounting system 11 for moving the analysis sample 56 in a direction tangential to that of the indentor 32 such that when the tip of the indentor 32 is driven simultaneously in the analysis sample 56, a scratch on the surface of the sample of • analysis 56. Figures 6, 7 and 8 provide details of a fastening system 13 that secures the analysis sample 56 to it, with its surface exposed in a perpendicular relationship with that of the indentor 32. As seen in Figure 6, the mounting system 11 includes a first fixed mount block 40 - to the base 2 of the apparatus 1 and a second frame block 42 fixed above the first frame block 40, in such a way that the fastening system 13 which is fixed on top of the second frame block 42, can be moved and placed precisely along the X and Y axes. In the input signals of the computer system 10, the pulse system 60 for the first mount block 40 and the drive system 58 for a second mount block 42 provide the movement along the X and Y axes of the fastening means 13 which is fixed above the second mounting block 42. One of the suitable mounting systems is the Nanomover ™ System available from Melles Griot, Irvine, California. These micro-positioners have a resolution of 50 nanometers with an absolute accuracy of ± 1 miera and a total transfer range of 25 mm. As seen in Figures 6, 7 and 8 the fastening system 13 includes a support block for the specimen holding part 44 which is secured above the block of the second mounting block 42. If desired, an absorbent film of the vibrations 62 and a silicone compound can be provided between the support block 42 for the specimen holding part and a second mount block 42 to further reduce the transmission of any high frequency noise from the second mount block 42 to the support block 44 for the specimen holding part. Preferably, a pair of conventional single-axis incunable platforms (not shown) that are placed at 90 ° to one another are provided between the support block 44 for the specimen holding part, and a second mount block. 42 to facilitate leveling of the analysis sample 56 that is secured with the fastening system 13. For example, the single-axis incunable platforms (Model No. TGN 80) available from Newport Company of Irvine, California) are well suited for this purpose. The platforms have a transfer range of ± 2.5 ° with a resolution of 20 arcsec and a sensitivity of 2 arcsec. A pair of wedging blocks 49 are secured to the support block 44 for the sample holding piece and a block A '46 is connected to the wedging blocks 49 by a third flexing system 48 which is connected to the stretches of the block-A '46 to provide a single degree of freedom to block I' 46 along the direction shown. The third flexing system 48, each includes a pair of diaphragm springs which are connected to each side of the wedging block and to each section of the A-block 46. The diaphragm springs are made of a nickel-iron alloy, available from Hamilton Precision Metals, Inc. of Lancaster, Pennsylvania. Block A '46 is placed above the surface of the support block 44 of the specimen holder to allow free reciprocating movement along the arrow shown. A specimen holding part 50 is fixed above the A-block 46. The specimen holding part 50 is provided with a pair of holding presses for sample 52, which pass over a pair of frame rods. . Each sample securing press 52 is provided with an immobilizing screw 54 such that the analysis sample 56 can be secured by tightening the clamping presses 52 around the analysis sample 56 by means of two locking screws 54. Apparatus 1, furthermore, includes a third perception system 51 for quantifying the tangential pressure experienced by the analysis sample 56 during the scratching of the analysis sample by the tip of the indentor 32 as it is transferred through the analysis sample 56 A third motionless component of a third sensing means 51 is mounted on the support block 44 for the specimen holding part and a third moving component of a third sensing system 51 is mounted on one side of the A-block 46., sthat when the indentor 32 scratches the surface of the analysis sample 56, the intermediate space between the third immobile component and the third moving component of a third perception system 51, varies according to the tangential pressure experienced by the sample of analysis 56. An analogous output signal resulting from this, then transmitted to the systems to condition the input and output signals 12 A '. A third perception system 51 may be the same as the first perception system 34, or be the second perception system 36, as for example, the capacitive sensor Model D-050-00 available from Physik Instremente, (Pl) GmBH &; Co, through its subsidiary Polytec Pl Inc. of Auburn, Massachusetts. According to the size of the diaphragm springs, in the first flexing system 22, the second flexing system 30 and the third perception system 51, and by the pressure of the energy system 16, these analysis apparatuses 1 can be modified to provide an apparatus 1 with different degrees of analysis and resolution capability, suitable for various analysis applications. The apparatus 1 is capable of producing micro-scratches in coatings or films having a thickness in the range of 1 to 1000 microns to quantify their resistance to deterioration. In carrying out such analyzes, the analysis sample 56 is secured in a sample holder 50. The analysis sample 56 is then initially leveled, when using a leveling with an air bubble leveler and preferably, with platforms incunables on a single axis to substantially level the exposed surface of the test sample 56 by scanning the surface of the test sample 56. By using the adjustable mechanical arm 5, the indentor 56 is placed near the test sample 56 and when using the video system 14, the tip of the indentor 32 approaches a distance of 5 microns from the exposed surface of the sample of analysis 56. Which occurs when the tip of the indentor and its reflection, substantially touch one with the other. In general, the final adjustments are made by using the transfer provided by the power system 16, which when energized, pushes the mobile clamp 20 which in turn pushes the indentor holder 28. which has an indentor 32 to make contact with the exposed surface of the test sample 56. When such contact occurs, a second perception system 36 provides the normal pressure experienced by the surface of the test sample 56. The normal pressure is adjusted at a constant normal pressure that is insufficient to produce any significant damage to the underlying surface of the test sample 56. Typically, such normal pressure is around 20 micro-newtons (μN) for the resinous coatings. First, to the surface of the test sample 56 to be scratched, an outline scan is made by scanning the tip of the indentor 32 in a determined direction on the surface at a given speed provided by the displacement of the mount system 11 to through a certain distance, typically 3 mm, and by fixedly determining the normal pressure with which the tip of the indentor 32 touches the surface of the test sample 56 at a level profiled enough to determine its contour without altering or damaging the surface , that is, at a normal pressure of 20 micro-newtons (μN). The normal pressure is maintained at the contour level during the surface contour scan by using continuous feedback from a closed loop control system provided by the mount system 11 and a computer system 10. The resulting data is stored at way of data from the scan of the contour prior to scratching in the memory system of the computer system 10. A downward scratch is then carried out by driving the tip of the indentor 32 at a certain speed on the surface of the sample of analysis 56 while simultaneously moving the surface of the analysis sample 56 at a speed provided by the mounting system 11 in the same direction determined through the same determined distance, when referring to the stored data from the previous contour scan scratch Therefore, when using the data prior to scratching, during the declining scratch on the surface of the sample of analysis 56, any errors that may contribute to the variation of surface, that is, valleys and ridges, of the sample of analysis 56 is eliminated. As a result, the tip of the indentor produces a scratch at the desired depth that is not affected by variations in the surface of the analysis sample 56. The resulting signals are stored as data from the contour scan by a displacement of the tip in the memory system of the computer system 10. Generally, during a declining scratch, the normal pressure experienced by the surface of the test sample 56 starts at zero. After a delay of 5 seconds, while the analysis sample 56 continues to move, the normal pressure increases steadily at a rate of 0.02 milli-newtons per second up to a defined maximum. If desired, the speed that increases gradually can be maintained at a constant level. Finally, an outline scan is made to the scratch surface by scanning it with the tip of the indentor 32 at a certain speed that is provided by a displacement of the mount system 11 through the same determined distance at the same level of the scan of the contour by normal pressure, that is to say a normal pressure of 20 μN, in the same determined direction that is established during the exploration of the previous contour to the scratch of the surface. The normal pressure is maintained at the level of the contour scan during scanning of the scratch contour by using a continuous feedback from a closed loop control system that is provided by the mounting system 11 and a computer system 10. The resulting signals are stored as post-scratch contour scan data in the memory system of a computer system 10. The data from the scan of the contour prior to scratching, the displacement of the tip and the posterior scratch are they process in processable data, which can then be visualized graphically or visually in a visualization system 12 to determine the resistance to deterioration of the sample of analysis 56.
In addition, the normal pressure experienced by the analysis sample 56, while the tip is driven in the analysis sample 56, is quantified and stored as contour scan data at normal pressure. The tangential pressure experienced by the test sample 56 during scratching of the test sample 56 is also quantified and stored as contour scan data by tangential pressure. The contour scan data by normal and tangential pressure are integrated into the processable data. The analysis sample 56 that is analyzed using the method of and the apparatus 1 of the present invention includes various coatings. Figure 9 shows the results of a micro-scratch experiment which is obtained in a clear envelope envelope having a thickness of approximately 30 μm which is made of an acrylic-styrene / melamine composition which is applied on a black base covering. The indentor 32 with a diamond tip having lμm is used.
Figures 10 and 11 show the results of a micro-scratch experiment that are obtained by using two different compositions of a translucent coating. The trace A in the graphs of Figures 9, 10 and 11 represents the outline before the scratch of an undamaged surface of an analysis sample 56, the trace D represents the outline of the displacement of the tip of the indentor 32 while penetrating into the sample of analysis 56 on the determined distance, the trace B represents an outline of the posterior scratch of the scratch. As seen from trace D and trace B, the coating makes a significant recovery after scratching the surface. The traces E and B are profiles of the normal pressure and tangential pressure that the sample of analysis 56 undergoes before the experiment. The damage to the coating is obtained by subtracting the depth of the contour previous to the scratch of stroke A from the depth of the outline of the rear scratch of stroke B.
In the first region of the scratch, the lines A and B overlap, which means that the deformation of the coating is fully recovered, that is, the deformation is elastic. As the pressure increases, the two lines begin to diverge, which means the beginning of the visco-plastic deformation, an enlarged version can be observed in Figure 1. The amount of deformation increases smoothly while the pressure is increased normal. At a distance of approximately 4.1 mm in Figure 9 (normal pressure 3 mN) and approximately 2.15 mN (normal pressure of 1.8 mN) in Figure 10, the character of stroke N undergoes an abrupt change. The tangential pressure as shown by the outline of stroke D and the displacement contour of the tip as shown in trace C begins to fluctuate rapidly indicating that a fracture has occurred, an enlarged version can be seen in Figure 2 While the normal pressure increases more, both the frequency and the magnitude of the break increase and eventually debris is generated. Compared to Figures 9 and 10, the data from the coating analysis shown in Figure 11 indicate that the coating shown in Figure 11 has a much lower deterioration resistance, since the fracture state occurs earlier. , while the same scratch occurs. In addition, the longer the period during which the coating remains in the elastic or visco-plastic zones, and the closer the trace B follows the trace A, the better is the resistance to deterioration of the coating. The present invention can also be used to compare the resistance to deterioration of various surfaces by causing the indentor 32 to penetrate to a uniformly determined depth, at a determined speed and at a certain normal pressure and then to compare the micro-scratches that occur on the various surfaces. Alternatively, the apparatus of the present invention can be used to determine the roughness of the surface of the coatings or films, the hardness of the films or coatings, such as by expolarizing an outline of the surface of the test sample or quantifying the uniformity of the thickness of the films or coatings by penetrating the tip of the indentor through the entire thickness of the film. The present invention is very convenient for quantifying the resistance to deterioration of various types of coatings, such as translucent and pigmented coatings that are used as automotive, maintenance, wood, plastic or paper coatings.; Scratch-resistant coatings that are applied over eyeglass lenses (goggles); antireflective and anti-glare coatings that are applied to camera or binocular lenses; various metallic coatings, such as in electrodeposition or electroplating, and coatings of chromium and titanium dioxide (TIN) in metal substrates and in electroplated nickel, copper, silver and gold coatings on metallic substrates. It is noted that in relation to this date, the best known method for the applicant to carry out the aforementioned invention, is the conventional one for the manufacture of the objects or products to which it refers.
Having described the invention as above, property is claimed as contained in the following:

Claims (23)

  1. CLAIMS 1. An apparatus for quantifying the resistance to deterioration of an analysis sample, characterized in that it comprises: a system for driving the indentor, this system is mounted on a supporting support of the apparatus comprising: a system for driving the indentor, which has an indentor that is placed to this, and a system to perceive the path of this indentor to and from the surface of this sample of analysis; and a system for directing the sample of analysis, this system is placed on a base of the apparatus comprising: a means of securing to secure the sample of analysis thereto, with the surface of the sample of analysis in perpendicular relation with the indentor, and a mounting system for traversing the analysis sample in a direction tangential to that of the indentor, such that when the indentor tip is simultaneously driven on the analysis sample, a scratch occurs on the surface of the film or of the plane.
  2. 2. The apparatus according to claim 1, characterized in that the system for directing the sample of analysis further comprises a third perception system for quantifying the tangential pressure that the sample of analysis undergoes during scratching of the sample of analysis by the indentor.
  3. 3. The apparatus according to claim 1 or 2, characterized in that it also comprises a computer system comprising: a system for conditioning the input and output signals to and from a system for driving the indentor, and this system directs the analysis sample to control the movements of the indentor and this analysis sample is in compliance with a computer program; systems for producing processable data resulting from scratching the surface of the sample of analysis; systems for storing this processable data; and systems to visualize the processable data in a visual or graphic form.
  4. 4. The apparatus according to claim 3, characterized in that the processable data comprises: data of the scan of the contour before the scratch which result when the tip is made to run along the surface of the sample of analysis before the surface is scratch the tip. contour scan data by the displacement of the tip that result when the tip is driven on the sample of analysis; post-scratch contour scan data that results when the tip is traversed along the scratch and contour scan data by normal pressure that results when the tip is driven over the test sample.
  5. 5. The apparatus according to claim 4, characterized in that the processable data further comprises the contour scan data by tangential pressure that result during scratching of the test sample.
  6. 6. The apparatus according to claim 1, characterized in that the system for the impulse of the indentor comprises: an immobile clamp fixed to a mechanical arm of this support bracket; a power system fixed to the stationary clamp to provide movement to the movable clamp that is flexibly connected to the stationary clamp by a first bending system that provides a single degree of freedom to the movable clamp; and an indentor fastener that is flexibly connected to the movable clamp by a second flexing system that provides a single degree of freedom to the indentor fastener, such that when the power system is energized, this movable clamp and this indentor holder having the indentor placed therein, moves only in a direction perpendicular to the surface of the sample of analysis.
  7. 7. The apparatus according to claim 6, characterized in that the energy system comprises a low-voltage piezo-transducer.
  8. 8. The apparatus according to claim 6, characterized in that the first and second flexible system each comprise a pair of diaphragm springs.
  9. 9. The apparatus according to claim 6, characterized the first flexible system or means comprises a pair of diaphragm springs which are connected at both ends of these movable clamps and of these immobile clamps.
  10. 10. The apparatus according to claim 6, characterized in that the second bending system comprises a pair of diaphragm springs which are connected at both ends of the indentor holder and of this movable clamp.
  11. 11. The apparatus according to claim 6, characterized in that the first bending system comprises three pairs of diaphragm springs which are connected radially in three positions on these movable clamps and in these immobile clamps, in such a way that each pair of these diaphragm springs are at 120 ° from each other.
  12. 12. The apparatus according to claim 1, characterized in that this system for perceiving the path of this indentor comprises: a first perception system to quantify the penetration of this indentor in this sample of analysis; and a second perception system to quantify the normal pressure experienced by this sample of analysis when this indentor penetrates this sample of analysis.
  13. 13. The apparatus according to claim 12, characterized in that this first perception system comprises a first immobile perception component that is mounted on a support post that is fixed to this immobile clamp and a second mobile perception component that is fixed to the fastener of the indentor. The apparatus according to claim 13, characterized in that this first immobile component of perception and this first mobile component of perception form a pair of capacitive sensors. 15. The apparatus according to claim 12, characterized in that this second perception system comprises a second immobile perception component that is fixed to the mobile clamp and a second mobile perception component that is fixed to the indentor holder. 16. The apparatus according to claim 15, characterized in that this second immobile component of perception and the second mobile component of perception form a pair of sensors-capacitors. 17. The apparatus according to claim 1, characterized in that this tip of this indentor is of diamond, corundum, topaz or quartz. 18. The apparatus according to claim 1, characterized in that this coating is a translucent coating that is applied on a car body, prescription glasses, lenses, wooden substrates, plastic substrates, or on a paper substrate. 19. A method for quantifying the resistance to deterioration of a test sample, characterized in that it comprises: secure this sample of analysis to a mounting system of an apparatus; place an indentor in relation perpendicular to the exposed surface of this sample of analysis, in such a way that the tip of this indentor is in contact with the surface of this sample of analysis; push this point of this indentor on the surface of this sample of analysis at a determined speed while simultaneously scanning this sample of analysis in a direction tangential to that of this indentor, at a certain speed in a certain direction to scratch this surface of this sample of analysis to produce a scratch. • The method according to claim 19, characterized in that it also comprises: produce signals in response to this scratch of this sample of analysis and convert these signals into actionable data; visualize these processable data visually or graphically. 21. A method for quantifying the resistance to deterioration of a test sample characterized in that it comprises: secure this sample of analysis to a mounting system of an apparatus; place an indentor in a relation perpendicular to that of the exposed surface of this sample of analysis, in such a way that the tip of this indentor is in contact with this surface of this sample of analysis; trace a contour of the surface of this sample of analysis at a certain distance when this tip crosses over this sample of analysis in a direction tangential to that of this indentor in a certain direction and store the data of the exploration of the contour previous to the scratch that result drive this point of this indentor on the surface of this sample of analysis at a certain speed that while simultaneously traveling this sample of analysis in a direction tangential to that of this indentor at a certain speed in this direction determined for this determined distance that is obtains by establishing a reference for these contour exploration data prior to scratching to produce a scratch on this surface of this analysis sample, and storing the contour scan data by the tip displacement resulting therefrom; trace a contour of the scratch on the surface of this sample of analysis as you trace this tip over the scratch in a direction tangential to that of this indentor in this determined direction for this determined distance and store the contour scan data posterior to the scratch that they result from this; processing these contour exploration data prior to scratching, tip displacement and post scratch in processable data; visualize these processable data in a visual or graphic form. The method according to claim 21, characterized in that this step of tracing the outline of the surface and this step of tracing the outline of the scratch on the surface comprises: establishing a normal pressure with which this tip touches the surface or scratches at a sufficient contour level to determine its contour without altering the surface or scratch; and maintaining this normal pressure at this level of exploration during this step of scanning the contour of the surface and this step of scanning the contour of the scratch on the surface by using a continuous feedback from a closed loop control system . 23. The method according to claim 21, characterized in that it also comprises: quantify the normal pressure experienced by this test sample while this tip is driven in this test sample and store the scan data that result from this; to quantify the tangential pressure that this sample of analysis undergoes during this scratch of this sample of analysis and to store the data of the exploration of the contour by tangential pressure that result from this; and integrate these data from the normal pressure scan and these tangential pressure scan data into these processable data.
MXPA/A/2000/008237A 1998-03-11 2000-08-23 Test apparatus and method of measuring mar resistance of film or coating MXPA00008237A (en)

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Application Number Priority Date Filing Date Title
US60/077,518 1998-03-11

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MXPA00008237A true MXPA00008237A (en) 2001-07-09

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