EP0731908A1 - Procedes et appareils d'essais de penetration, de rayure ou tribologiques - Google Patents

Procedes et appareils d'essais de penetration, de rayure ou tribologiques

Info

Publication number
EP0731908A1
EP0731908A1 EP95932849A EP95932849A EP0731908A1 EP 0731908 A1 EP0731908 A1 EP 0731908A1 EP 95932849 A EP95932849 A EP 95932849A EP 95932849 A EP95932849 A EP 95932849A EP 0731908 A1 EP0731908 A1 EP 0731908A1
Authority
EP
European Patent Office
Prior art keywords
scratch
sample
scattered light
indentation
raman scattered
Prior art date
Legal status (The legal status 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 status listed.)
Withdrawn
Application number
EP95932849A
Other languages
German (de)
English (en)
Inventor
Gillies David Pitt
Paul Hayward Ian
Paul Centre Suisse d'Electronique et ALERS
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Centre Suisse dElectronique et Microtechnique SA CSEM
Renishaw PLC
Original Assignee
Centre Suisse dElectronique et Microtechnique SA CSEM
Renishaw PLC
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
Priority claimed from GB9419724A external-priority patent/GB9419724D0/en
Priority claimed from GBGB9514366.5A external-priority patent/GB9514366D0/en
Application filed by Centre Suisse dElectronique et Microtechnique SA CSEM, Renishaw PLC filed Critical Centre Suisse dElectronique et Microtechnique SA CSEM
Publication of EP0731908A1 publication Critical patent/EP0731908A1/fr
Withdrawn legal-status Critical Current

Links

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
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/44—Raman spectrometry; Scattering spectrometry ; Fluorescence spectrometry
    • 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
    • G01N2203/0286—Miniature specimen; Testing on microregions of a specimen
    • 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
    • G01N2203/06—Indicating or recording means; Sensing means
    • G01N2203/0641—Indicating or recording means; Sensing means using optical, X-ray, ultraviolet, infrared or similar detectors

Definitions

  • An ultra microhardness tester is available from Centre Suisse d'Electronique et de Microtechnique SA (CSEM) , Maladiere 71, CH-2007, Neuchatel , Switzerland. This device measures the loading force and the penetration depth during a loading and unloading cycle with a specially shaped indentor, and provides information about the plastic and elastic deformation of the sample.
  • CSEM Centre Suisse d'Electronique et de Microtechnique SA
  • Fig 1 is a schematic diagram of a scratch testing machine
  • Fig 11 is a plan view of apparatus for tribological testing; and Fig 12 shows a modification of Fig 10.
  • the scratched sample 10 mounted on the table 52 of Fig 3 first of all the sample is viewed under the microscope 42, in order to discover the alignment of the scratch on the sample surface relative to the x and y axes of movement of the table 52. This is necessary because it is difficult or impossible to align the sample in exactly the same way as it was aligned on the table 12 of the scratch tester. Either the mirror 36 can be removed for this alignment, so that the alignment takes place using the microscope in the normal manner, illuminating the sample 10 with white light. Alternatively, the filters 38,44 and Raman analyser 46 may be temporarily removed from the optical path, again enabling an image of the sample 10 to be viewed in white light on the CCD 50.
  • this distance of 1250 ⁇ m along the track is easy to correlate with the exact position in the data acquired by the computer 24 of the scratch tester, e.g. by correlating it with the end point of the scratch. From the data acquired by the computer 24, it is possible to relate this distance of 1250 ⁇ m with the positions (and the corresponding instantaneous scratching loads) at which visible signs of damage are seen in the microscope 18, and at which increases are seen in the frictional force Ft and the acoustic emission AE.
  • diamond instead of diamond, it may b made of another suitable material such as A1 2 0 3 or sapphire
  • A1 2 0 3 or sapphire The scratch or indentation test is especially useful when the sample 10 has a very thin coating or surface film (not shown) , as explained in the above paper by Schumann.
  • the computer 54 is then able to output information, e.g. in graphical form, showing how the strains and stresses induced in the sample 10 vary during the cycle of an indentation or scratch test.
  • information e.g. in graphical form, showing how the strains and stresses induced in the sample 10 vary during the cycle of an indentation or scratch test.
  • changes in this data indicate critical points in the behaviour of the sample.
  • the stress/strain data derived may indicate critical points at which there is a breakdown in the cohesion or adhesion of the film or coating. Effects such as plastic deformation of the material of the film or coating may also be determined.
  • the Raman spectrometer in Figs 9 and 10 may make use of confocal techniques.
  • Figs 9 and 10 where the sample 10 comprises a thin film or coating on a substrate, it is possible to determine not only stress/strain data for the tip 74 and for the material of the coating, but also for the underlying substrate material, by monitoring suitable Raman peaks characteristic of the coating and the substrate respectively. This yields still further information about the properties of the interface between the coating and the substrate.
  • Raman data may also be obtained in the same way from a pin similar to the pin 86, but mounted in tribological apparatus of the type in which the pin undergoes reciprocating motion relative to the sample, rather than rotary motion.
  • the Raman scattered light from the tip 74 and sample 10 is collected by the lens 72. It is taken to a Raman analysis section according to Fig 9 via the optical fibre 70B.
  • the fibre 70B also has a filter 38B at its end, within the stylus 14.
  • the filter 38B is a narrow notch filter, designed to reject light having the same frequency as the laser. It therefore rejects Rayleigh scattered and reflected laser light, while passing the desired Raman signals.

Abstract

On décrit un appareil d'essai de rayure avec lequel une pellicule ou un revêtement déposé sur un échantillon (10) est rayé par un stylet (14), ce qui permet d'en examiner des qualités telles que la cohésion ou l'adhérence au substrat. En même temps ou après, la surface rayée est éclairée par une lumière laser, au travers d'un microscope (42) par exemple, pour produire une lumière diffusée Raman. Celle-ci repasse par le microscope (42) et est analysée, ce qui permet de déterminer des contraintes ou des tensions présentes dans la région rayée. Ceci permet d'obtenir des informations quantitatives sur la qualité de la pellicule ou du revêtement. On peut utiliser des procédés d'analyse Raman similaires pour effectuer des essais de pénétration et des essais tribologiques.
EP95932849A 1994-09-30 1995-10-02 Procedes et appareils d'essais de penetration, de rayure ou tribologiques Withdrawn EP0731908A1 (fr)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
GB9419724 1994-09-30
GB9419724A GB9419724D0 (en) 1994-09-30 1994-09-30 Methods and apparatus for identation or scratch testing
GB9514366 1995-07-13
GBGB9514366.5A GB9514366D0 (en) 1995-07-13 1995-07-13 Methods and apparatus for indentation, scratch or tribological testing
PCT/GB1995/002331 WO1996010737A1 (fr) 1994-09-30 1995-10-02 Procedes et appareils d'essais de penetration, de rayure ou tribologiques

Publications (1)

Publication Number Publication Date
EP0731908A1 true EP0731908A1 (fr) 1996-09-18

Family

ID=26305712

Family Applications (1)

Application Number Title Priority Date Filing Date
EP95932849A Withdrawn EP0731908A1 (fr) 1994-09-30 1995-10-02 Procedes et appareils d'essais de penetration, de rayure ou tribologiques

Country Status (2)

Country Link
EP (1) EP0731908A1 (fr)
WO (1) WO1996010737A1 (fr)

Families Citing this family (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB9514367D0 (en) * 1995-07-13 1995-09-13 Renishaw Plc Strain and/or stress sensitive devices
KR100579034B1 (ko) * 1998-03-11 2006-05-12 이 아이 듀폰 디 네모아 앤드 캄파니 막 또는 코팅의 긁힘 저항을 측정하는 검사 장치 및 방법
DE102004021888A1 (de) * 2004-05-04 2005-12-01 Bayer Materialscience Ag Verfahren zur Prüfung der Kratzfestigkeit von Kunststoffoberflächen
GB0510497D0 (en) * 2004-08-04 2005-06-29 Horiba Ltd Substrate examining device
JP5972531B2 (ja) 2008-02-26 2016-08-17 バッテル メモリアル インスティチュート 生物学的及び化学的マイクロスコピックターゲティング
FR2981452B1 (fr) * 2011-10-14 2013-12-20 Lorraine Inst Nat Polytech Dispositif de determination du comportement mecanique local d'une eprouvette de materiau
FR2989465B1 (fr) * 2012-04-12 2014-11-21 Total Sa Procede de determination de parametres geomecaniques d'un echantillon de roche
JP5944873B2 (ja) * 2013-09-20 2016-07-05 新日鉄住金マテリアルズ株式会社 炭化珪素単結晶ウェハの内部応力評価方法、及び炭化珪素単結晶ウェハの反りの予測方法
GB201317429D0 (en) * 2013-10-02 2013-11-13 Renishaw Plc Spectroscopy apparatus and method
EP3267177A1 (fr) * 2016-07-08 2018-01-10 Anton Paar TriTec SA Procédé d'évaluation automatisée de surface
US10258239B2 (en) 2017-05-30 2019-04-16 Vishal Khosla Method for in-line testing and surface analysis of test material with participation of raman spectroscopy
CN107589104B (zh) * 2017-08-08 2020-12-18 哈尔滨工业大学 基于力调制微刻划/微压痕过程制备拉曼增强基底上阵列微纳米结构的实验装置及方法
DE102017222198B4 (de) 2017-12-07 2020-01-02 Infineon Technologies Ag System und verfahren zur untersuchung von halbleitersubstraten
CZ308746B6 (cs) * 2020-07-10 2021-04-21 Univerzita Palackého v Olomouci Nástavec držáku vzorků pro hodnocení mechanické odolnosti tenkých vrstev a způsob hodnocení kvality mechanické odolnosti tenkých vrstev pomocí tohoto nástavce
EP4273533A1 (fr) 2022-05-06 2023-11-08 Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. Appareil de mesure de contrainte et procédé de mesure de contrainte mécanique
CN114918530A (zh) * 2022-06-30 2022-08-19 华中科技大学 一种激光原位辅助压痕/划痕装置及方法

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01189544A (ja) * 1988-01-25 1989-07-28 Shimadzu Corp 極微小硬度計
GB9112343D0 (en) * 1991-06-08 1991-07-31 Renishaw Transducer Syst Surface analysis apparatus
US5027650A (en) * 1990-05-08 1991-07-02 Gte Laboratories Incorporated Method for characterization of adhesion between hard materials
EP0740133B1 (fr) * 1991-11-16 1997-09-10 RENISHAW plc Illumination de l'échantillon pour appareil spectroscopique et procédé

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9610737A1 *

Also Published As

Publication number Publication date
WO1996010737A1 (fr) 1996-04-11

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