EP2142902A2 - Dispositif pour déterminer une propriété mécanique d'un échantillon lors d'un essai - Google Patents

Dispositif pour déterminer une propriété mécanique d'un échantillon lors d'un essai

Info

Publication number
EP2142902A2
EP2142902A2 EP08748771A EP08748771A EP2142902A2 EP 2142902 A2 EP2142902 A2 EP 2142902A2 EP 08748771 A EP08748771 A EP 08748771A EP 08748771 A EP08748771 A EP 08748771A EP 2142902 A2 EP2142902 A2 EP 2142902A2
Authority
EP
European Patent Office
Prior art keywords
indenter
sample
laser light
tip
heating
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Withdrawn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
EP08748771A
Other languages
German (de)
English (en)
Inventor
Wolfgang Stein
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.)
Surface Systems and Technology GmbH and Co KG
Original Assignee
Surface Systems and Technology GmbH and Co KG
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 Surface Systems and Technology GmbH and Co KG filed Critical Surface Systems and Technology GmbH and Co KG
Publication of EP2142902A2 publication Critical patent/EP2142902A2/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Withdrawn legal-status Critical Current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
    • 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
    • G01N2203/022—Environment of the test
    • G01N2203/0222—Temperature
    • G01N2203/0226—High temperature; Heating means

Definitions

  • the invention relates to a device for determining a mechanical property of a sample to be examined.
  • the progressive spread of micro and nanotechnology requires knowledge of the respective material properties in the respective dimension.
  • the so-called nanoindentation is a more and more used method for the quantitative measurement of the mechanical properties such as the elastic modulus, the fracture toughness and the hardness of the material.
  • nanoidentation With the help of the method of nanoindentation, also referred to as nanoidentation, such quantities in the range of, for example, very thin layers or also bulk material with high lateral resolution can be determined experimentally.
  • a so-called indenter formed as a type of microprobe is placed on the sample to be examined, and a force is exerted on the sample surface by this indenter, depending on the selected measurement specification.
  • the substance properties mentioned are usually measured at room temperature.
  • the known device comprises only a sample heating, which disadvantageously has an insufficiently stable temperature field, so that the measurement quality or the resolution of the nanoindentation is severely limited.
  • a first cause is in this known device is that the
  • the known device was operated at temperatures up to 500 ° C. As a result, the measuring accuracy of the measurements made by means of this known device for determining the properties of the material of the sample is adversely affected. In addition, comparatively much heating capacity is needed to heat the entire sample holder. Consequently, the maximum achievable
  • the object is achieved by a device according to claim 1.
  • the device according to the invention comprises means for laser heating of the indenter or the indenter tip.
  • the location of the energy supply is variable due to the very high energy density of the laser heating which can be controlled over a wide range and tuned to the geometry of the indenter present on the device according to the invention or adapted to the geometry of the indenter tip can be. This achieves a minimization of the energy transfer surface. It has also been recognized that this minimization greatly reduces or even completely eliminates the temperature drift known in the art, and consequently increases the accuracy of measurements for determining mechanical property.
  • this invention small-area, almost point-shaped laser heating, also referred to as Tippheizer, with a comparatively low laser power compared to the state of the art used for heating systems can be operated.
  • the device according to the invention may comprise a light guide, which brings the laser light up to the indenter, in particular up to the indenter tip.
  • a light guide which brings the laser light up to the indenter, in particular up to the indenter tip.
  • the end of the light guide can be arranged on the indenter or near the indenter.
  • the end of the light guide may have optics for improved focusing.
  • the arrangement of the end of the light guide can be done outside of the indenter, so that the heating takes place by Laseraristrahlung on the outside of the indenter. Structurally, the heating can thus take place stationary from the outside, decoupled from possible movements of the intender according to the invention, which are to be carried out in the context of measurements.
  • the light guide extends within the indenter, so that the light exit end is brought within Indenters up to the indenter tip.
  • the laser heating provided on the device according to the invention not only comprises a first optical waveguide but also one or more further optical waveguides.
  • the local landfill of the heating cable can be adapted to the requirements of the structural design of the device according to the invention.
  • the device has a sample holder, which is provided for receiving the sample to be examined.
  • the sample can be firmly connected to the sample holder.
  • the sample is bonded to an adhesive.
  • an adhesive chosen with high thermal conductivity.
  • the sample holder may be formed thermally insulating, so that a further increase in temperature stability is achieved.
  • the sample holder also has a high rigidity and a low thermal expansion.
  • a transparent to the laser light of the laser heating material can be selected.
  • quartz or sapphire can be used as material for this purpose.
  • This material for forming the sample holder is advantageously optically transparent.
  • this material has good properties in terms of insulation, stiffness and thermal expansion.
  • the device can be mechanically optimized to the extent that the temperature-related expansions affect only the sample and not on the holder.
  • the sample surface can be formed thermally and mechanically stable, so that the temperature-induced expansions of the surface and the drifting away of the surface are avoided. For this purpose, it can be provided that the sample holder takes place directly over the surface to be measured, so that the thermal expansion does not take place in the direction of the indenter tip.
  • the temperature control can be carried out with the aid of a thermocouple or a PT-100 element.
  • One or more of the measures proposed above for laser heating with the corresponding advantages can be used in further embodiments of Device according to the invention also find application for laser heating of the sample or samples to be examined, as far as the device according to the invention is designed for receiving a plurality of samples.
  • a defined temperature of the sample or of the indenter is to be set with the aid of the laser heating power, it is possible, for example, to use PT-100 elements or thermocouples.
  • an optionally integrated pyrometer can be used in a very advantageous manner for the optical temperature determination of the indenter.
  • the pyrometer can be arranged directly in the beam path of the laser.
  • a rapid temperature determination can be carried out and, in an advantageous embodiment, a desired temperature or a desired time-dependent temperature profile can be set by means of a control.
  • the pyrometer can be detected by means of a real-time
  • Calculator is read, preferably with a frequency of up to 20 kHz.
  • a device according to the invention has the advantage that a very fast control with control frequencies of up to 10 kHz can be used. It has been recognized that with the aid of such a device according to the invention, a very rapid temperature change of the sample to be examined is carried out, for example, from 50 ° C./second to 800 ° C./second, in particular in the range from 500 ° C./second to 700 ° C./second can be. In this way, such a device according to the invention opens up completely new dynamic possibilities. For example, multiple measurements of the sample can be made very rapidly at widely different temperatures. At the same time, the high measuring accuracies required to determine the properties of the sample are achieved.
  • the indenter on the rear side can be irradiated by means of laser light and thus heated.
  • the laser light is focused using an optical fiber, for example, on the indenter itself.
  • the laser light may also indirectly heat by being directed to the holder of the indenter. In any case, it is advantageously achieved that even with this heater, the area of heat transfer very is small and thus the associated advantages of a good temperature stability and a minimum drift of the device according to the invention is achieved.
  • the temperature control of the identifier of the adjustable sample temperature is readjusted, so that no temperature gradient is formed in the contact zone of the indenter with the sample, so that in this respect, the measurement influencing disturbances are completely avoided.
  • the measurements can be carried out with the aid of the device according to the invention with extremely high accuracy.
  • the device according to the invention can be used to determine a wide variety of
  • Material properties of a sample are used. For example, depending on the temperature, the penetration depth of the indenter can be determined and the hardness or the modulus of elasticity of the material of a thin layer or of a thin film can be determined. Also, scratch tests or friction force measurement can be performed with high measurement accuracy.
  • the device according to the invention also makes it possible to improve the quality of a tool or electronic component having one or more such thin layers by suitably selecting the layer material.
  • the device according to the invention can also be used to measure the dynamic
  • Hardness of thin films or films can be used. For example, with metal cutting using coated tools, knowledge of the dynamic material property is important in choosing a suitable coating for such a tool. Also in the field of wear-resistant materials for forming such layers, the use of the device according to the invention plays an important role, because in such friction and wear processes a significant heat development takes place and thus the selected layer must have suitable material properties even at high operating temperatures.
  • FIG. 1 shows a first embodiment of the indenter according to the invention with heating arranged internally for the heating in cross section;
  • Figure 2 shows a second embodiment of the indenter according to the invention with the
  • Figure 3 inventive indenter tip according to a third embodiment of the indenter according to the invention with heating arranged internally for heating when choosing a transparent to the wavelength of the laser light tip material in cross section.
  • the device according to the invention comprises a sample to be examined, which is connected to a sample holder.
  • the indenter tip of an indenter according to the invention is connected to the device according to the invention and arranged on the free sample surface of the sample.
  • a device according to the invention may comprise one or more laser heating systems, described in detail below.
  • FIG. 1 shows a first exemplary embodiment of an indenter 16 containing an indenter tip 15 for a device according to the invention.
  • the end of a partially illustrated indenter 15, 16 is shown, which comprises a pointed shaped portion whose pointed end can be brought into contact with the surface of a sample to be examined. This end has a pointed shape for the most punctual contact with the sample surface.
  • This End region of the indenter 16 is referred to below as tip 15 or indenter tip 15.
  • This indenter tip 15 is shown hatched in cross-section in FIG.
  • the indenter 16 has, for laser heating according to FIG. 1, a light guide 17 (glass fiber 17) shown hatched, which protrudes into the indenter 16, starting from the side of the indenter 16 facing away from the sample, and is only partially shown in FIG.
  • the end 18 of this optical waveguide 17 with or without optics for focusing the laser light guided by the optical waveguide 17 can be embodied on the indenter tip 15. Without optics, it is a structurally simpler embodiment that can be used to heat the indenter tip 15.
  • the device according to the invention has a fitted at the end 18 of the optical fiber 17 optics, a further increase of the local heating favoring focusing of the laser light can be achieved.
  • four lines are shown in FIG. 1, which connect the end of the light guide 18 with the tip 15. Depending on the focus, a more or less large part of the tip surface facing the light guide can thus be exposed to laser light within the indenter 16.
  • the indenter 26 according to the invention for forming a device according to the invention in a second embodiment according to Figure 2 means for heating, which cause the laser light is laterally brought up to the indentation tip 25.
  • a light guide 27 is likewise provided, the end 28 of which is arranged close to, but spaced apart from, the indenter tip 25 shown in cross-section by hatching.
  • the end 28 of the light guide 27, which is only partially shown in cross-section and hatched may likewise have an optical system for focusing the exiting laser light.
  • a light guide 27, 28 provided with optics effects an improved alignment of the exiting light on the outside of the indenter tip 25.
  • four are also shown in FIG Plotted lines connecting the end of the light guide 28 with the outer periphery of the tip 25. Depending on the focus can thus a more or less a large part of the optical fiber facing the tipping surface outside of the indenter 26 are exposed to laser light.
  • the measurement of the set tip temperature is of great importance. It is conceivable that a device according to the invention with an indenter according to FIG. 1 or 2 for the optical temperature measurement has a pyrometer. Alternatively, a temperature measurement by means of a thermocouple or resistance thermometer can be used. This temperature measurement can, like the laser heating of the indenter tip, be carried out optionally outside the indenter on its outside. However, means for measuring temperature can also be arranged in the interior of the indenter, starting from the side facing away from the sample side of the indenter in this protruding.
  • the indenter according to the invention has, for example, a diameter of from 3 millimeters to less than 1 millimeter.
  • the light guide used for laser heating for example, has a diameter of only 0.1 millimeters.
  • thermocouple or resistance thermometer is a time-lapse measurement method. Faster temperature measurements can be achieved with the help of a pyrometer.
  • the pyrometer can be arranged with the aid of suitable means directly in the beam path of the laser heating.
  • a control for the signal of such a pyrometer can be sampled, for example, at 10 kHz and consequently read out at several kHz, in particular 1 kHz to 8 kHz.
  • the indenter according to the invention as shown in FIGS. 1 or 2 can be brought into contact with this sample surface with its indenter tip, preferably in the direction perpendicular to the surface of the sample to be examined.
  • the device according to the invention may further comprise a sample holder for
  • the sample holder is mechanically stiff.
  • the sample can be clamped in the sample holder.
  • the device according to the invention may comprise means for forming a sample heating by means of laser light.
  • a light guide can be provided, is guided in the laser light of a laser source to the open end of the light guide.
  • This end can be arranged directly on the rear side of the sample facing away from the front side provided for contacting with the indenter so that laser light directly heats the rear side of the sample to be examined.
  • an optical or other temperature measurement can also be used as the temperature measurement for this heater, for example in the manner of an optical pyrometer, a thermocouple or a resistance thermometer previously described in connection with the tip heater.
  • a light guide can be used in an optical temperature measurement.
  • a particularly advantageous embodiment of the invention is formed by a laser heating with optical temperature measurement and temperature control, as far as both the indenter tip and the sample to be examined are laser-heated.
  • the laser heating can be formed by means of a system of several optical fibers.
  • a sample holder which accommodates the sample, which preferably comprises a carrier transparent to the wavelength of the laser light.
  • an adhesive for holding the sample it is advantageous in this context when using an adhesive for holding the sample to choose a transparent for the wavelength of the laser light adhesive.
  • the wavelength of the light for example, a wavelength in the range from the visible to the infrared (IR) range can be used.
  • an optical design of the device according to the invention for heating and temperature measurement of indenter and sample control can be provided so that the Pyrometerstrahlengang is coaxially integrated into the laser beam path and is coupled via a wavelength-dependent beam splitter.
  • a very rapid temperature control can be achieved.
  • temperature programs can be run which enable exact, time-dependent temperature ramps of up to several 100 ° C./second, for example 200 ° C./second to 700 ° C./second. This achieves a very fast and reliable detection of the measurement results for determining mechanical properties.
  • a rapid heating time in particular non-equilibrium processes, in particular thermally-induced material changes, can be investigated.
  • temperatures of at least up to 500 ° C, in particular in the range of 700 ° C to 900 ° C, preferably more than 1000 ° C to the melting temperature used materials can be achieved.
  • the inventive device with a coordinated combination of indenter-tip heating and sample heating and associated control advantageously avoids a falsification of the measurement temperature and thus the measurement results for determining the mechanical properties of the thin sample to be examined due to temperature differences between indenter and sample.
  • a control adapted to the laser heating and temperature measurement can ensure that the sample and the indenter or the indenter tip both have exactly the same temperature. This ensures an optimal evaluation for determining the mechanical property (s).
  • the device according to the invention comprises an indenter tip 35, which consists of a for the formed for laser heating laser wavelength transparent material is formed.
  • This indenter tip 35 is shown as part of an indenter not shown in the following in the figure 3 in cross-section ABCDEFG.
  • a device according to the invention can have a light guide 37, which is guided in the interior of the indenter, not shown in detail in FIG. 3 and hatched, partially in FIG. 3, which guides the laser light as far as the indenter tip 35. With transparent formation of the tip 35, this laser light will then enter the tip 35 after leaving the light guide 37 at the end 38 of this light guide 37 and then emerge at the side of the tip 35 facing the sample surface 33.
  • the tip 35 touches the surface of the sample 33 shown hatched in part in FIG. 3.
  • four lines are drawn in FIG. 3, which connect the end of the light guide 38 to the transparent tip 15 and then penetrate into it. Consequently, at least at the media boundary GEC of the tip 35, a further focusing in the direction E can be achieved by refraction.
  • the heating energy is predetermined, and thus possibly optimally concentrated on the sample area provided for heating and for subsequent measurement of the mechanical property (s).
  • the light will be absorbed at the location of the contact surface DEF between tip 35 and sample 31.
  • the local optical conditions due to focusing as a result of the refraction, the around the
  • Thickness BC the width AB and the angular size of the tip E of the tip 35 is concerned, more closely adjusted or appropriate conditions are taken into account. It will exploits the knowledge that these geometries and dimensions of the tip 35 form a function of the indenter material.
  • the temperature can be measured by means of a thermocouple or pyrometer.
  • a temperature measurement by means of a thermocouple a heating of the thermocouple by the laser or by the laser light is avoided by appropriate optical means and thus detects the temperature of the substrate or the sample surface directly.
  • a laser a diode laser or a solid-state laser can be used.
  • the respective ends of the light guide which are arranged at a distance from the tip, have four lines which are intended to represent light beams emerging for clarification.
  • the shaping of the outgoing light beam can be set with or without optical means at the end of the light guide.
  • the light spot can supply a partial area of the indenter or also the entire indenter surface which can be achieved in the respective position with laser light and thus set a desired energy distribution of the indenter heating.
  • this so-called object according to the invention forms at least at one end a indenter tip (p), or shortly as a tip (p) designated tip which in the device according to the invention for determining a mechanical property of a sample to be examined for the purpose of forming a force on the sample surface can be used.

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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 Or Analyzing Materials Using Thermal Means (AREA)
  • Length Measuring Devices By Optical Means (AREA)

Abstract

L'invention concerne un dispositif pour déterminer lors d'un essai une propriété mécanique d'un échantillon comportant un pénétrateur et des moyens de chauffage de ce pénétrateur par lumière laser. Le pénétrateur présente, à l'extrémité dirigée vers l'échantillon, une pointe. Le moyen de chauffage par lumière laser prévu pour ce pénétrateur consiste au moins en un conducteur optique pour la transmission de lumière laser jusqu'au voisinage du pénétrateur, notamment de la pointe du pénétrateur. En outre, l'invention concerne un pénétrateur à utiliser dans le domaine des nanotechnologies et présentant une forme allongée, une zone terminale conçue en pointe et des moyens de chauffage par lumière laser. Ce pénétrateur peut présenter un conducteur optique guidé au moins partiellement dans le pénétrateur et dont la sortie de prélèvement de lumière est située à proximité de la pointe du pénétrateur.
EP08748771A 2007-04-30 2008-04-23 Dispositif pour déterminer une propriété mécanique d'un échantillon lors d'un essai Withdrawn EP2142902A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102007020624A DE102007020624A1 (de) 2007-04-30 2007-04-30 Vorrichtung zur Bestimmung einer mechanischen Eigenschaft einer zu untersuchenden Probe
PCT/DE2008/000695 WO2008131731A2 (fr) 2007-04-30 2008-04-23 Dispositif pour déterminer une propriété mécanique d'un échantillon lors d'un essai

Publications (1)

Publication Number Publication Date
EP2142902A2 true EP2142902A2 (fr) 2010-01-13

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP08748771A Withdrawn EP2142902A2 (fr) 2007-04-30 2008-04-23 Dispositif pour déterminer une propriété mécanique d'un échantillon lors d'un essai

Country Status (4)

Country Link
US (1) US20100064783A1 (fr)
EP (1) EP2142902A2 (fr)
DE (2) DE102007020624A1 (fr)
WO (1) WO2008131731A2 (fr)

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US8683849B2 (en) * 2010-01-12 2014-04-01 Imi Cornelius, Inc. Method and apparatus for testing consistency of frozen beverages
GB2478134B (en) * 2010-02-25 2012-01-11 Micro Materials Ltd Heating in material testing apparatus
RU2548929C1 (ru) * 2013-12-18 2015-04-20 Шлюмберже Текнолоджи Б.В. Способ определения профиля прочности материалов и устройство для его осуществления
RU2619448C1 (ru) * 2016-04-20 2017-05-15 Федеральное государственное бюджетное образовательное учреждение высшего образования "Комсомольский-на-Амуре государственный технический университет" (ФГБОУ ВО "КнАГТУ") Маятниковый склерометр с лазерным устройством
RU2680853C1 (ru) * 2018-05-18 2019-02-28 Федеральное государственное бюджетное научное учреждение "Технологический институт сверхтвердых и новых углеродных материалов" Индентор-объектив
RU2709550C1 (ru) * 2018-11-28 2019-12-18 Федеральное государственное бюджетное учреждение науки Институт физики металлов имени М.Н. Михеева Уральского отделения Российской академии наук (ИФМ УрО РАН) Способ получения упрочненного никельхромборкремниевого покрытия на металлических деталях

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Also Published As

Publication number Publication date
WO2008131731A3 (fr) 2009-02-05
WO2008131731A2 (fr) 2008-11-06
US20100064783A1 (en) 2010-03-18
DE112008001743A5 (de) 2010-04-08
DE102007020624A1 (de) 2008-11-06

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