WO2020099071A1 - Procédé de contrôle des propriétés adhésives d'une couche, notamment d'une couche de protection contre l'usure - Google Patents

Procédé de contrôle des propriétés adhésives d'une couche, notamment d'une couche de protection contre l'usure Download PDF

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Publication number
WO2020099071A1
WO2020099071A1 PCT/EP2019/078551 EP2019078551W WO2020099071A1 WO 2020099071 A1 WO2020099071 A1 WO 2020099071A1 EP 2019078551 W EP2019078551 W EP 2019078551W WO 2020099071 A1 WO2020099071 A1 WO 2020099071A1
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WO
WIPO (PCT)
Prior art keywords
layer
treatment
states
evaluating
tested
Prior art date
Application number
PCT/EP2019/078551
Other languages
German (de)
English (en)
Inventor
Richard Braak
Ulrich May
Original Assignee
Robert Bosch Gmbh
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 Robert Bosch Gmbh filed Critical Robert Bosch Gmbh
Priority to CN201980074540.5A priority Critical patent/CN113015898B/zh
Publication of WO2020099071A1 publication Critical patent/WO2020099071A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/40—Investigating hardness or rebound hardness
    • G01N3/42—Investigating hardness or rebound hardness by performing impressions under a steady load by indentors, e.g. sphere, pyramid
    • G01N3/46—Investigating hardness or rebound hardness by performing impressions under a steady load by indentors, e.g. sphere, pyramid the indentors performing a scratching movement
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N19/00—Investigating materials by mechanical methods
    • G01N19/04—Measuring adhesive force between materials, e.g. of sealing tape, of coating
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/40—Investigating hardness or rebound hardness
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02—Details not specific for a particular testing method
    • G01N2203/026—Specifications of the specimen
    • G01N2203/0262—Shape of the specimen
    • G01N2203/0278—Thin specimens
    • G01N2203/0282—Two dimensional, e.g. tapes, webs, sheets, strips, disks or membranes

Definitions

  • the invention relates to a method for testing the adhesive properties of a layer, in particular a wear protection layer, on a substrate and also to a device which is suitable for carrying out such a method.
  • Tests are known for hard material layers with which the adhesive strength or quality of adhesion can be assessed.
  • a high load is usually applied to the layer system and the damage caused is analyzed optically.
  • An established standard test method that serves to determine the adhesive strength of layers on substrates is the test method according to VDI standard 3198, in which a typically conical diamond tip is pressed into the layer to be tested at a high load of 1500 Newtons a chipping image is recorded, which is only roughly classified on the basis of schematic comparison images and therefore only provides reliable results for standard damage images.
  • the method according to the invention comprises the method steps of a) introducing at least one scratch mark into the surface of the layer in order to cause at least local damage in the layer, b) detecting a state of the layer at least in the region of the at least one scratch mark, c ) Treating the layer, the treatment being carried out as a temperature treatment and / or chemical treatment and / or ultrasound treatment, d) detecting a state of the layer immediately after its treatment, and e) comparing the respectively recorded states of the layer with one another and Evaluation in order to determine the spread of the damage and to determine the adhesive properties of the layer.
  • the basic idea of the invention is therefore that slight damage to the layer to be tested is initially initiated, and then after detection of the damaged state of the layer, treatment is carried out which serves to advance the initiated damage to the layer, for example by means of stress corrosion cracking. in order to obtain more information about the adhesion or adhesive strength of the layer, and the treatment used can be carried out in different ways in order to achieve the desired effect.
  • the treatment can be carried out as a temperature treatment, for example in a heating furnace, in a preset temperature region for a predetermined time.
  • the layer to be tested is exposed to a chemical in a chemical bath for a certain time.
  • the layer to be tested is exposed to a high-frequency alternating load, which is generated, for example, by means of an ultrasound sonotrode, for a predetermined time.
  • a high-frequency alternating load which is generated, for example, by means of an ultrasound sonotrode, for a predetermined time.
  • the state of the layer achieved after the treatment is recorded, so that a comparison between the states of the layer recorded at different times is made possible, on the basis of which a spread of the damage occurring during the treatment as a measure of the adhesive strength of the layer is evaluable.
  • An embodiment of the invention can consist in that at least one adhesion impression is made in the surface of the layer prior to the introduction of the at least one scratch mark, wherein the at least one adhesion impression can be designed as Vickers indentation in order to minimize cracks in the layer to be tested bring in.
  • a pyramid-shaped diamond tip is typically pressed into the layer to be tested with a defined load, the load being able to lie in a force range ranging from approximately 1 N to approximately 2000 N. It is characteristic of this that, in addition to a compressive stress acting in the radial direction, a tensile stress acting in a circular direction is additionally introduced directly around the Vickers impression, while at the same time a pure compressive stress range acts somewhat displaced, thereby promoting the occurrence of buckling effects. However, these buckling effects occur primarily when the at least one scratch track can interact with the tension field generated by the previously introduced identification.
  • the method according to the invention therefore takes into account the normal response behavior of a layer with poor adhesion, which is characterized precisely by the occurrence of buckles, that is to say partial detachments of the layer at the interface with the substrate, and takes place primarily in the printing area, in contrast to the state of the art nik, in which the high tensile stresses introduced during the impression make the occurrence and the examination of a damage progress more difficult.
  • a particularly preferred embodiment of the invention can consist in that according to step a) a plurality of roughly parallel scratch marks are introduced into the surface of the layer and that at least two adhesion impressions are introduced into the layer, the adhesion impressions being arranged directly adjacent to one another. This makes a relative Generates a large area of tension with relatively minor damage in the layer to be tested than is possible with just a single scratch mark and a single impression of liability.
  • the at least one scratch mark introduced according to step a) is expediently arranged in the immediate vicinity of the previously introduced at least one impression of liability.
  • the specific stress field generated by the impression of adhesion in the layer initially remains - not least due to the inherent stresses inherent in the layer - and can then interact with the at least one scratch mark introduced thereafter, so that a pure compressive stress range that is on the outer periphery of the liability pressure exists, can lead to a voltage increase or pressure increase in the vicinity of the scratch track subsequently introduced, if the scratch track and the impression of adhesion are close enough together and, consequently, a cooperation-based overlay effect is made possible, which can only cause buckling effects.
  • An embodiment variant of the invention can consist in that a temperature pretreatment of the layer to be tested is carried out before the introduction or impressing of the at least one adhesion impression. This allows advance, i.e. at the beginning of the method according to the invention, it is determined whether the interface between the substrate and the layer is subject to thermal aging.
  • the at least one scratch track is designed as a nanoscratch.
  • the at least one scratch mark can be designed as an engraving, since engraving devices are easier to handle than nano-identification devices.
  • a further development of the invention provides that when comparing and evaluating, the number and / or size of bubble-shaped delamination and / or their respective distance from an identification is / are taken into account as a measure of the adhesive properties of the layer to be tested. Based on such parameters, not only a qualitative but also quantitative analysis is possible, which Ne classification within a linear scale allows, since at the end of the evaluation chain there is a final result as a measure of the adhesive strength of the layer to be tested, because the occurrence or spread or absence of bubble-shaped delaminations or buckles basically provides information about the physical size G, which characterizes the adhesion of a layer as the energy release rate and thus serves as a parameter.
  • a further development of the invention can consist in that, when comparing and evaluating as a measure of the adhesive properties of a layer to be checked, a speed v is taken into account with which one or more delamination (s) is dependent on a period of time At Step c) spreads out the treatment carried out and a growth length As obtained and detected. By basing the evaluation on the speed of the spread of damage, a classification can be made on a linear scale.
  • a device which is suitable for carrying out such a method comprises means for introducing at least one scratch mark into the layer, means for detecting the states of the layer, means for treating the layer, and means for comparing and evaluating the respectively detected states of the layer.
  • the means for detecting the states of the layer have a light microscope device and / or a scanning microscope device.
  • FIG. 1 shows a flowchart with the essential method steps of the method according to the invention according to a first embodiment
  • Fig. 3 is a light micrograph of a layer in a state after two immediately adjacent high-load impressions were pressed into the layer by means of a Vickers pyramid and then five nano-scratches running approximately parallel to one another in close proximity to the two high-load impressions have been incised into the layer, wherein in the state then detected by light microscopy, a damage progress is depicted, which is essentially based on a dark area as a moving buckle, ie manifested as a partial detachment of the layer,
  • 4A shows a classification scheme according to a first embodiment for evaluating the adhesive strength of a layer to be tested with a total of four evaluation levels
  • 4B shows a classification scheme according to a second embodiment for evaluating the adhesive strength of a layer to be tested with a total of five evaluation levels
  • FIG. 5 is a block diagram of a device used to carry out the method according to the invention with a device for introducing scoring tracks in the layer, a device for detecting states of the layer, a device for treating the layer, a device for comparing and evaluating the detected states and a device for identifying Vickers impressions in the layer.
  • FIG. 1 shows a flowchart 100 with the essential method steps 110 to 160 of a first embodiment of the method according to the invention, which is used to characterize the adhesive properties, ie the adhesive strength of a layer on a substrate.
  • the adhesive properties ie the adhesive strength of a layer on a substrate.
  • at least one nanoscratch is introduced into the surface of the layer in a step 110, in the preferred exemplary embodiment five nano-scratches running parallel to one another, in order to damage the layer to a slight extent.
  • the surface of the layer in the damaged area is then optically detected in a step 120 immediately following it by means of a light microscope image or a scanning electron microscope image.
  • the sample is then post-treated in step 130 in order to increase the degree or extent of the damage that occurred in step 110.
  • This aftertreatment can be carried out as a temperature treatment, for example at a temperature of about 100 ° C. and higher, alternatively as a chemical treatment or as an ultrasound treatment.
  • the chemical treatment can be carried out for example with fuels and / or acids or alkalis; For example, stress corrosion cracking can often be accelerated by immersion in a water bath.
  • the ultrasound treatment can be carried out by means of an ultrasound sonotrode, for example in order to cause cavitation erosion in the layer to be tested.
  • the sample is immersed in a container filled with liquid and ultrasonic waves generated by an ultrasonic sonotrode arranged in the vicinity of the sample then cause rapidly collapsing bubbles in the liquid, which leads to successive erosion of the layer material of the sample.
  • step 140 which occurs immediately after the end of the aftertreatment 130, the state of the layer is optically detected analogously to step 120, whereupon in a step 150 the recording according to step 140 is compared with the recording according to step 120 by the degree or extent of to determine possible damage.
  • step 160 the result of comparison step 120 is evaluated according to an evaluation scale which comprises at least four categories.
  • FIG. 2 shows a flow diagram 100 ′ with the essential method steps of a second embodiment of the method according to the invention.
  • the same reference numerals denote the same method steps as in FIG. 1.
  • This second embodiment differs from the first embodiment shown in FIG. 1 in that, in addition to steps 110 to 160, optional pretreatment steps 101, 102 in addition to steps 110 to 160 upstream.
  • a sample to be examined which comprises the layer applied to a substrate, is one Exposed to temperature pretreatment, which can be done, for example, by storing the sample on a heating device or in a heating furnace.
  • the preferred temperature range is between approximately 300 ° C. and approximately 500 ° C.
  • a Vickers adhesion impression is made on the surface of the layer, which serves to introduce a compressive stress into the layer, which can increase the mechanical stress occurring in an immediately subsequent method step.
  • FIG. 3 shows - to illustrate the second embodiment of the method according to the invention - a light microscope image 200 of a layer after steps 102 and 110 have been carried out in succession and then the state of the layer has been recorded by means of the light microscope image 200 in accordance with step 120.
  • Five nanoscratches 201, 201-1, 201-2, 201-3, 201-4, which are introduced into the layer approximately parallel to one another by means of a nanoindentation device, and two adhesive impressions 202, 202 ' are recorded on the light microscope image 200.
  • an engraving device can be used instead of a nano-identification device.
  • the nanoscratches 201, 201-1, 201-2, 201-3, 201-4 cause damage initiation in the layer.
  • a stress field is generated in the layer by the adhesive impressions 202, 202 ' , which were introduced into the layer by the introduction of the nanoscratches 201, 201-1, 201-2, 201-3, 201-4, because directly around the respective impression in addition to a compressive stress in the radial direction and a tensile stress in the circular direction, ie in the circumferential direction of the rectangular outer boundary of the respective impression is introduced.
  • FIG. 4A shows a first exemplary embodiment of a classification scheme 300 suitable for evaluating the adhesive strength of a layer to be tested, which has at least four evaluation levels S1, S2, S3, S4, which are arranged at a distance from one another along a rating scale 301.
  • the evaluation level S1 corresponds to a final state of a layer to be tested, in which, due to the comparison of the light microscopic images according to steps 120 and 140, adhesive damage to the layer cannot be detected, since the light microscopic images (according to steps 120 and 140) are not detectable Show change of state.
  • the evaluation level S1 therefore corresponds to an approximately maximum layer quality.
  • the evaluation level S2 corresponds to a final state in which the light microscopic recordings (according to steps 120 and 140) only show a difference or a deterioration in state if an identification step 102 has also been carried out and thus a buckling effect in connection with step 110 3 in the second recording according to step 140 is recognizable or detectable, whereas there is no substantial difference between the recording according to step 140 compared to the recording according to step without step 102, ie when the second embodiment of the method according to the invention is implemented 120 results, so that in no deterioration in condition can be detected in this case.
  • An even finer classification or classification in the range of the rating levels S1 to S3 can be achieved by analyzing occurring buckles, i.e.
  • bubble-shaped releases using parameters that determine the number and size of the buckles and the respective distance of the buckles from the center of a relevant one Include identification (according to step 102) and are symbolized in FIG. 4A with the aid of an arrow Pfl, an increase in the buckling effect being associated with the direction of the arrow.
  • the evaluation level S3 corresponds to a final state in which - on the basis of a comparison of a recording according to step 140 with a recording according to step 120 - a clear deterioration in the condition can be detected, which is manifested by means of one or more delamination (s) after treatment step 130.
  • the evaluation level S4 corresponds to a final state in which the layer quality reaches a minimum quality level if - based on a comparison of a recording according to step 140 with a recording according to step 120 - a large-scale delamination of the layer can be detected.
  • An even finer subdivision in the range of the evaluation levels S3 to S4 can be achieved by examining the speed v of a delamination progress in a layer to be tested and analyzing it as a parameter, which is symbolized in FIG. 4A by an arrow Pf2.
  • the end result at the end of an evaluation chain provides a value as a measure of the adhesive strength, which can be classified on a linear scale.
  • a value W resulting at the end of the evaluation chain can be compared with a product or application-specific reference or threshold value W ref , which can be derived, for example, from empirical observations or studies on layers of different quality, in order to assess whether a Layer is still usable or unusable. If the value W exceeds such a reference or threshold value W ref , the relevant layer is classified as unusable, ie classified as a committee, whereas if the value W is below it, the relevant layer is classified as usable.
  • FIG. 4B shows a second exemplary embodiment of a classification scheme 300 ' suitable for evaluating the adhesion of a layer to be tested, which has five evaluation stages S1, S2, S3, S4, S5 spaced apart from one another along an evaluation scale 301 ' .
  • the second exemplary embodiment of the classification scheme differs from the first exemplary embodiment only in that a fifth evaluation level S5 is additionally provided.
  • the evaluation level S4 is characterized in that the layer is detached over a large area around the impression area by means of the identification step 102, while the evaluation level S5 has an even larger area of liability that extends far beyond the impression area of the identification.
  • the evaluation level S5 therefore represents a minimum quality level in this second exemplary embodiment.
  • the device 400 shown in FIG. 5 and used to carry out the method according to the invention essentially comprises a device 401, which is used to introduce a scratch mark into a respective layer and is designed, for example, as an engraving device or nano-identification device, a device 402 for detecting states of the respective layer, a device 403 for treating the respective layer, a device 404 which is used for comparing and evaluating the respectively recorded states of the respective layer and is designed as a computing device, and an input direction 405 for identifying Vickers impressions in the respective layer.
  • the devices 401, 403, 405 are connected to one another via a transfer path 406 for the exchange of samples.
  • the device 402 and the comparison and evaluation device 404 are operatively connected to one another via a signal and / or data transmission line 404 ′ , so that the comparison and evaluation device 404 designed as a process computing device in the exemplary embodiment, image data from the device 402 according to the method steps 150 , 160 can receive and process.
  • the method according to the invention serves to check the adhesive properties of a layer on a substrate and comprises the method steps of a) introducing 110 at least one scratch mark 201, 201-1, 201-2, 201-3, 201-4 into the surface of the layer, to at least locally damage the layer, b) detecting 120 a state of the layer at least in the area of the at least one scratch mark 201, 201-1, 201-2, 201-3, 201-4, c) treating 130 of the layer, the treatment being carried out as a temperature treatment and / or chemical treatment and / or ultrasound treatment, d) detecting 140 a state of the layer immediately after its treatment, and e) comparing 150 the respectively detected states of the layer with one another and evaluating them 160 in order to determine the spread of the damage and to determine the adhesive properties of the layer in a classifying manner, the number and / or size v.
  • a speed v can be taken into account as a measure of the adhesive properties of a layer to be tested, at which speed one or more delamination (s) 204 depends on a time period At of the treatment carried out according to step c) and on a result achieved and detected Spreading / spreading growth length As.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
  • Investigating Materials By The Use Of Optical Means Adapted For Particular Applications (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

L'invention concerne un procédé servant à contrôler les propriétés adhésives d'une couche, notamment d'une couche de protection contre l'usure, sur un substrat, comprenant les étapes suivantes : a) incorporation (110) d'au moins une trace de rayure (201, 201-1, 201-2, 201-3, 201-4) dans la surface de la couche afin d'endommager la couche au moins localement, b) détection (120) d'un état de la couche au moins dans la zone de l'au moins une trace de rayure (201, 201-1, 201-2, 201-3, 201-4), c) traitement (130) de la couche, le traitement étant réalisé sous la forme d'un traitement thermique et/ou d'un traitement chimique et/ou d'un traitement par ultrasons, d) détection (140) d'un état de la couche immédiatement après son traitement, et e) comparaison (150) des états respectivement détectés de la couche les uns avec les autres et évaluation (160) afin d'identifier une propagation du dommage et effectuer à partir de celle-ci une détermination de classification des propriétés adhésives de la couche.
PCT/EP2019/078551 2018-11-12 2019-10-21 Procédé de contrôle des propriétés adhésives d'une couche, notamment d'une couche de protection contre l'usure WO2020099071A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201980074540.5A CN113015898B (zh) 2018-11-12 2019-10-21 用于检测层、尤其是防磨损层的粘附特性的方法

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DE102018219231.6A DE102018219231A1 (de) 2018-11-12 2018-11-12 Verfahren zum Prüfen der Hafteigenschaften einer Schicht, insbesondere einer Verschleißschutzschicht
DE102018219231.6 2018-11-12

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WO2020099071A1 true WO2020099071A1 (fr) 2020-05-22

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WO (1) WO2020099071A1 (fr)

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DE102023000767A1 (de) 2023-03-02 2024-03-07 Mercedes-Benz Group AG Verfahren und Vorrichtung zum Prüfen einer auf einer Oberfläche haftenden Schicht

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CN105424474A (zh) * 2015-11-03 2016-03-23 北京交通大学 一种评估钢结构厚板内部损伤累积的方法
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BURNETT P J ET AL: "The relationship between hardness and scratch adhession", THIN SOLID FILMS, ELSEVIER, AMSTERDAM, NL, vol. 154, no. 1-2, 12 November 1987 (1987-11-12), pages 403 - 416, XP025787157, ISSN: 0040-6090, [retrieved on 19871112], DOI: 10.1016/0040-6090(87)90382-8 *
C.V. FALUB ET AL.: "In vitro studies of the adhesion of diamond-like carbon thin films on CoCrMo biomedical implant alloy", ACTA MATERIALIA, vol. 59, 2011, pages 4678 - 4689
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DE102018219231A1 (de) 2020-05-14
CN113015898B (zh) 2024-02-09

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