EP2263076A1 - Procédé d'essai thermographique de matériaux non métalliques, en particulier de matériaux non métalliques revêtus, ainsi que leur procédé de fabrication, et objets fabriqués selon ce procédé - Google Patents

Procédé d'essai thermographique de matériaux non métalliques, en particulier de matériaux non métalliques revêtus, ainsi que leur procédé de fabrication, et objets fabriqués selon ce procédé

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Publication number
EP2263076A1
EP2263076A1 EP09725446A EP09725446A EP2263076A1 EP 2263076 A1 EP2263076 A1 EP 2263076A1 EP 09725446 A EP09725446 A EP 09725446A EP 09725446 A EP09725446 A EP 09725446A EP 2263076 A1 EP2263076 A1 EP 2263076A1
Authority
EP
European Patent Office
Prior art keywords
coating
layer
metallic
ceramic
silicon nitride
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Withdrawn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
EP09725446A
Other languages
German (de)
English (en)
Inventor
Andreas Ortner
Klaus Gerstner
Ralph Neubecker
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.)
Schott AG
Original Assignee
Schott AG
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 Schott AG filed Critical Schott AG
Publication of EP2263076A1 publication Critical patent/EP2263076A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/72—Investigating presence of flaws
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/38—Concrete; Lime; Mortar; Gypsum; Bricks; Ceramics; Glass
    • G01N33/388—Ceramics

Definitions

  • thermographic testing of non-metallic materials in particular coated non-metallic materials, as well as processes for their preparation and according to the method produced body
  • the invention relates to a method for thermographic testing of non-metallic materials, in particular coated non-metallic materials.
  • Thermographic testing methods have been used, for example, to test metallic materials
  • WO 2006/037359 A1 discloses a thermographic process in which the time course of the
  • thermographic testing of coated turbine blades is known. With the thermographic measurement of coated metallic body is provided by the high thermal conductivity of the metal over the very reduced thermal conductivity of the coating, a fairly acceptable temporal temperature profile for determining material parameters.
  • layers containing ceramic or particles, including sintered particles can for example be optically barely or not distinguishable from the coated ceramic substrate.
  • the object of the invention is to enable or to improve the testing or even the measurement of layer jobs, in particular non-metallic layer jobs, on non-metallic materials.
  • thermographic processes which can be coated, even coated non-metallic.
  • thermography still meaningful and even beyond can be calibrated and metrologically usable to achieve results.
  • a very important application of this process is in the testing of barrier coated fused silica crucibles, such as quartz crucibles for silicon production.
  • Silicon is often melted in silicon nitride coated fused silica crucibles to silicon ingots, also referred to as ingots.
  • the silicon nitride coating prevents the molten silicon from reacting with the crucible material and damaging or even penetrating the crucible.
  • the previous test method for evaluating the protective layer quality consists of a visual inspection during the spraying of the first layer with a Siliziumnitridschlicker, which is subsequently fixed by a thermal process.
  • the optical test had to be carried out during the spraying, since this layer can hardly be perceived after thermal fixing with visual means. It is used in this procedure Essentially a thin white film is applied to a white substrate.
  • silicon nitride slip as understood is any liquid-viscous mixture in which silicon nitride is dispersed and / or dissolved.
  • the invention provides a method for the thermographic examination of non-metallic materials, in particular coated non-metallic materials, wherein at least part of the surface of the non-metallic material, preferably a part of the surface provided with a non-metallic coating, in particular by means of a short energy pulse, preferably a light pulse or by periodic heat input, a heating made and the temporal and local temperature history recorded at least at several consecutive times.
  • the invention also provides bodies prepared according to the invention, the layers of which only have a deviation of less than 20 ⁇ m, as a rule even less than 5 ⁇ m, from their nominal layer thickness, which is of great advantage, in particular for barrier coatings.
  • the Fourier down-transformed of the recorded temporal temperature profile was determined spatially resolved and for a time t or a defined Phase shown after the entry of the energy pulse spatially resolved, thereby detecting the thermal diffusion of the energy or heat pulse through the layer and based on their thickness.
  • the convolution signal of the time profile of the energy pulse with the recorded temporal temperature profile could advantageously also be determined spatially resolved for a shift time t and displayed in a spatially resolved manner.
  • the coating with a water and particles, in particular sinterable particles, containing suspension, in particular a slurry, preferably by
  • the sinterable particles preferably comprise silicon nitride and / or the ceramic material comprises a SiO 2 -containing ceramic, in particular quartz.
  • thermographic test was carried out prior to the thermal fixing process, because then it was possible to ensure, even before the thermally stressing and energy-intensive fixing process, that the required minimum layer thickness was present at all points of the coating.
  • At least one drying step was carried out at a temperature of more than 20 ° C. and for a period of more than 2 hours, preferably of more than 3 hours and most preferably of more than 5 hours.
  • the measurement was also surprisingly meaningful when the non-metallic material comprised a ceramic and the coating a barrier coating.
  • Silicon nitride layer covered which are virtually indistinguishable from each other, could still be achieved metrologically relevant results.
  • the ceramic had a wall thickness of about 5 mm to 50 mm at the coated location and the silicon nitride coating a thickness of 50 microns to 500 microns.
  • the ceramic had a wall thickness of about 15 mm at the coated location and the silicon nitride coating a thickness of 100 ⁇ m to 300 ⁇ m. Even if the layer system was a multi-layer system, relevant statements of the test method could be obtained without the multilayer structure significantly falsifying the measurements.
  • the multi-layer system comprised silicon nitride layers, which were applied layer by layer by means of a slurry and subsequently by means of a thermal
  • the method was also applicable if the material had the shape of a, preferably rectangular crucible, since even at oblique angles, for example in the crucible corners, unexpectedly precise results were obtained.
  • a threshold value for the layer thickness of the coating it was possible to specify a threshold value for the layer thickness of the coating to be tested at a defined time after the energy input, which threshold value could be used as a measure of a minimum layer thickness for the test for each location of the coating.
  • thermographic test method according to the invention in particular also with the drying steps, it was also successfully attempted to use this test method also for measuring purposes.
  • sample body comprising a non-metallic material
  • the sample body had layers with different predetermined layer thicknesses at different points and the values associated with these predetermined layer thicknesses are determined for calibrating the measured values.
  • the invention also encompasses a method for producing a non-metallic body with a non-metallic coating, a method for thermographic examination and a method for measuring the layer thickness, as will be described in more detail below.
  • the non-metallic layer on the non-metallic body for example of barrier layers, it is also used. This can reduce costs and avoid hazards, as faulty
  • Production results can be minimized and layer thicknesses can be provided at a high quality level.
  • Coating are part of the present invention.
  • the invention also provides bodies prepared according to the invention whose layers have only a deviation of less than 20 .mu.m, usually even less than 5 .mu.m, from their nominal layer thickness, because iteratively can not be applied correctly Make corrections that can even be made automatically when the imaging values are acquired.
  • FIG. 1 shows typical absorption bands in the near, middle and far infrared spectral range, as can be obtained, for example, in the atmosphere.
  • FIG. 2 shows a typical thermographic structure by means of which exemplary measurements were carried out for the invention
  • FIG. 3 shows a thermographic image of the phase difference obtained in the thermographic structure shown in FIG. 2 (thus after the Fourier transformation) of a quartz material body partially coated with silicon nitride layer
  • FIG. 4 shows a representation of the temperature profile
  • Figure 5 is a double logarithmic representation of
  • FIG. 6 shows a two-dimensional representation of the height level of a quartz material or quartz body measured with a white light interferometer, which, like the body, is shown in FIG in Figure 3 is partially coated with a silicon nitride layer, with a line drawn across a coated portion and a not 7 shows a mean height profile calculated from the two-dimensional white light interferometer recording of FIG. 6, which extends along the line shown in FIG. 6, FIG.
  • FIG. 14 is a photographic Representation of the in FIG. 14 shown Quarzgut-, in particular quartz crucible, obliquely from above, substantially from the same direction as shown in Figures 11 to 13 shown,
  • FIG. 16 shows the local measured by pulse thermography
  • FIG. 17 shows the local measured by pulse thermography
  • FIG. 18 shows the temperature distribution at a quartz material coated with six different layer thicknesses, in particular quartz bodies.
  • the layer quality which means the existence of a minimum layer thickness, their intactness, such as freedom from cracks and delamination from the coated surface, is of grave importance.
  • Siliconware used crucibles can greatly increase their service life, if it can be ascertained with certainty that these crucibles still have the necessary minimum layer thickness for the production process of the ingot at all necessary points, in particular the points in contact with silicon.
  • each layer can then be reliably examined before the thermally stressing and energy-intensive and cost-intensive fixing process in its layered quality and either released or otherwise reworked, which was extremely helpful, in particular with spatially resolved measurements.
  • FIG. 1 shows exemplary typical absorption bands in the near, middle and far infrared spectral range, as obtained, for example, in the atmosphere.
  • thermographic examination could considerably improve the quality of the measurements.
  • At least one drying step was carried out at a temperature of more than 20 ° C. for a period of more than 2 hours, preferably of more than 3 hours and most preferably of more than 5 hours.
  • FIG. 2 shows, by way of example only, the test setup by means of which exemplary measurements were carried out for the invention.
  • the reference numeral 1 is a thermal camera provided, which had about 600 by 500 pixels spatial resolution and which recorded the image of the surface of a provided with a coating 5 ceramic body 2.
  • the surface of the body 2 was illuminated as homogeneously as possible in order to ensure a homogeneous over the surface of the body 2 energy input.
  • the flash units 3 and 4 were operated synchronized with the thermal camera 1, so that a fixed temporal image sequence of two-dimensional data could be recorded.
  • the short-term light output of all flash units is defined here, regardless of whether it takes place absolutely simultaneously or offset by a small amount of time.
  • the workpiece used in carrying out the method according to the invention was a ceramic Quarzgut-, in particular quartz body, on whose surface four differently coated areas I to IV were encountered, see for example Figure 18.
  • Silicon nitride crystals in a glassy solidified matrix reduces the hardness of Si 3 N 4 compared to Si carbide, but allows the stem-like recrystallization of the ⁇ -silicon nitride crystals during the sintering process, which results in a significantly increased fracture toughness compared to silicon carbide and boron carbide.
  • the high fracture toughness in combination with small defect sizes gives
  • Silicon nitride the highest strength among the engineering ceramic materials.
  • the combination of high strength, low coefficient of thermal expansion and relatively low modulus of elasticity makes Si 3 N 4 ceramics particularly suitable for components subject to thermal shock and is used, for example, as an insert for cast iron materials (inter alia in interrupted section) or for handling aluminum melts.
  • Silicon nitride ceramics are suitable for use temperatures up to about 1300 0 C with a suitable choice of a refractory glass phase (for example, by the addition of yttria). This definition should also apply to the purposes of the present invention.
  • a silicon nitride-containing layer which contains particulate non-sintered, particulate sintered and / or ceramic constituents is also referred to as the silicon nitride layer.
  • ceramics are largely formed from inorganic, fine-grained raw materials with addition of water at room temperature and then dried objects which are in one subsequent firing above 900 0 C to harder, more durable objects are sintered.
  • the term also includes materials based on metal oxides.
  • quartz is in this description, a high-Si02-containing refractory material, in particular a high-Si02 ceramic, understood, whose SiO 2 content is greater than 98%.
  • high-purity quartz as this is preferably used, the SiO.sub.2 content is more than 99.99%, this material being produced as a sintered ceramic from an aqueous slip, thus an aqueous, paritcular SiO.sub.2-containing suspension.
  • Region IV had no coating, whereas the coating in regions III to I became progressively thicker. See, for example, FIG. 18.
  • the coating thicknesses were about 70 ⁇ m in the region I, about 140 ⁇ m in the region II and about 220 ⁇ m in the region III.
  • the coating was a barrier coating, which included in particular a silicon nitride layer, as used for example in the production of silicon.
  • the various thicknesses were obtained by multiple application of a Siliziumnitridschlickers, which is subsequently baked or fixed by means of a thermal fixing process on the surface has been.
  • This coating was applied with the suspension containing water and particles, in particular sinterable particles, preferably by spraying, brushing, rolling, dipping and / or by means of a laminar film coating.
  • the coating was subsequently subjected to a thermal fixation process.
  • the particles preferably comprise silicon nitride and / or the ceramic material comprises a SiO 2 -containing ceramic, in particular quartz.
  • thermographic image of the surface of the Quarzal institutions 2 directly after an energy input by means of a light pulse, the flash units 3 and 4 showed almost no difference in the intensity recorded by the different pixels of the thermal camera directly after exposure.
  • Figure 18 The thermographic image of the surface of the Quarzal couples 2, directly after an energy input by means of a light pulse, the flash units 3 and 4 showed almost no difference in the intensity recorded by the different pixels of the thermal camera directly after exposure.
  • Coating 5 provided points and was heated at the same points without coating substantially the same.
  • thermographic image of the surface of the Quarzal couples at a defined time after the light pulse showed a locally attributable to the layer thickness intensity curve, as with increasing layer thickness and the intensity recorded by the individual pixels of the thermal camera 1 increased.
  • An InSb quantum detector with a pixel count of 640x512 pixels was used, as it is marketed for example by Thermosensork GmbH.
  • Quantum detector type designation InSb 640 SM made by Thermosensorik GmbH.
  • the FPA (Focal Plane) camera offers a resolution of 640 x 512 pixels with a readout frequency of 100 Hz for the full screen, which can be increased by limiting the field of view to up to 1000 Hz.
  • the InSb detector is sensitive in the wavelength range from 1 ⁇ m to 5 ⁇ m, which is limited to the range of 3 ⁇ m to 5 ⁇ m due to the limited transmission behavior of the 28 mm objective used.
  • the light sources were two high-performance flash lamps with a total energy of 12 kJ.
  • the flash duration was slightly more than 10 mS and intensity or the maximum energy input of the flash units 12 kJ per pulse, the distance of the flash units to the measured surface was between 20 and 40 cm.
  • a video sequence of the sample is taken by the camera for a set period of time: the sequence includes a short time before the flash is fired, the flash itself and the subsequent cooling of the sample.
  • the sequence length was set to 300 images at a recording frequency of 100 Hz. The measurements were carried out with maximum flash power of 12 kJ.
  • the Fourier transform of the recorded temporal temperature profile was determined spatially resolved and displayed spatially resolved for a time t or a defined phase after the entry of the energy pulse, thereby detecting the thermal diffusion of the energy or heat pulse through the layer and thereupon its thickness.
  • the convolution signal of the time profile of the energy pulse with the recorded temporal temperature profile could advantageously also be determined spatially resolved for a shift time t and displayed in a spatially resolved manner.
  • Flash devices in mathematical approximation is essentially a Dirac pulse.
  • FIG. 3 in which a quartz body 2 coated with a silicon nitride layer 5 is shown.
  • thermographic structure shown in Figure 2 was used.
  • Figure 4 shows a representation of the temperature profile upon diffusion of a Dirac temperature pulse in a semi-infinite homogeneous medium with a heat-imparting constituent starting from the surface as Function of Time
  • Figure 5 is a double logarithmic representation of the temperature profile upon diffusion of a Dirac temperature pulse in a semi-infinite homogeneous medium with a heat-imparting component of the surface starting as a function of time, the location of the heat accumulation of the peak in Figure 5 assigned is.
  • FIG. 6 shows a two-dimensional representation of the local layer thickness profile measured with a white light interferometer on the surface of a quartz body 2, which is partially coated with a silicon nitride layer 5, along a coated section and along an uncoated section of its surface.
  • FIG. 7 shows the local layer thickness or height profile, measured with a white light interferometer, along the line drawn in FIG. 6, which extends transversely to a coated section and an uncoated section.
  • non-destructive white-light interferometry can only be used for small areas and for essentially two-dimensional bodies, that is to say bodies having only a few micrometers of height difference and, consequently, is not suitable for larger areas and three-dimensional bodies having a greater height difference.
  • interferometers must be adjusted with an accuracy in the wavelength range, both at a distance and with respect to their tilting relative to the measurement surface, which practically precludes their use for mass production.
  • the heat pulse passes without any further action from the surface into the interior of the material and the flash duration is so short that the energy input occurs substantially everywhere on the exposed surface at the same time, this pulse usually proceeds perpendicularly to the surface in the volume and the Infrarotkamrea and also used for lighting flash units or lamps must not be aligned exactly to this surface to be measured.
  • the Fourier transform or convolution that is performed essentially measures the shape of the signal and less its absolute value. But precisely its shape is decisive for the measured layer thickness, as will be shown later.
  • Intensity threshold for the individual pixels are given at a defined time after the energy input, which could be specified and used as a measure of a minimum layer thickness for the test for each location of the coating.
  • this method proved to be surprisingly precise and even allowed a calibration based on a multiple coated specimen with locally different layer thicknesses.
  • test also includes a measurement, in particular a measurement based on a calibration, as described in more detail below.
  • FIG. 8 shows in its upper area a two-dimensional representation of the local intensity curve as described above on the surface of a quartz body which is coated with several silicon nitride layers which run stepwise, from left to right, in number at the surface of the quartz body and thus in their total thickness, and in their lower section, individual measurements made on each step of the same body for calibration purposes using a confocal reference method.
  • a confocal reference method a method was used, as described for example in DE 10 200 40 49541.
  • the respective sample body had at different points layers with different predetermined layer thicknesses, which are shown for example in Figures 9 and 10 as measuring points in their respective abscissa.
  • the ordinates of FIGS. 9 and 10 respectively show values designated as IR count values which correspond in height to the value of the above-described Fourier signal and similarly also to that of the described convolution signal.
  • FIG. 9 shows a two-dimensional representation of a calibration obtained with the coated fused quartz material, in particular quartz bodies, illustrated in FIG. 8, in which locally measured layer thicknesses of the silicon nitride layer applied to the quartz body were assigned to the absolute gray values obtained by pulse thermography.
  • the layer thickness of a layer to be measured can now be obtained by comparison and / or linear interpolation for each location with the calibrated values shown, for example, in FIG.
  • FIG. 10 shows a two-dimensional representation of one of the similar calibrations shown in FIG. 9, in which the absolute gray values obtained by pulse thermography and thus their layer thickness values were determined for two different distances.
  • the two images were taken in each case for a distance of the infrared camera to the measured surface of 450 mm and 650 mm and show very clearly that this distance has only a very small influence on the measured layer thickness.
  • the local resolution was in the lateral direction, thus substantially parallel to the surface of the sample body about 50 pixels (dots) per cm and perpendicular to the surface of the sample body thus in its depth about 20 ⁇ m as explained above.
  • FIG. 11 shows the locally measured intensity and therefore layer thickness profile on the surface of a quartz crucible, which had no coating at all, viewed obliquely from above, as measured by pulse thermography.
  • FIG. 12 shows the locally measured intensity and thus layer thickness profile on the surface of a quartz crucible, which is completely coated with a silicon nitride layer, which was applied to it in a first coating step with a spray coating, seen obliquely from above, in FIG pulsation thermometrically measured local intensity and thus layer thickness profile at the surface of the quartz crucible shown in Figure 12, which is additionally completely coated with a second silicon nitride layer, which was applied in a second coating step with a spray coating on the first layer, seen obliquely from above, and FIG.
  • FIG. 14 shows the local intensity and intensity measurements by pulse thermography thus layer thickness profile at the surface of the quartz crucible shown in Figure 12 and Figure 13, which is additionally completely coated with a third silicon nitride layer, which was applied in a third coating step with a spray coating on the second layer, after a drying time of about 20 minutes after the third spray coating seen obliquely from above,
  • Figure 15 shows a photographic representation of the in
  • Figure 14 shown quartz crucible, obliquely from above, substantially from the same direction as shown in Figures 11 to 13 shown,
  • the ceramic had a wall thickness of about 5 mm to 50 mm at the coated point and the silicon nitride coating had a thickness of 50 ⁇ m to 500 ⁇ m.
  • the ceramic had a wall thickness of about 15 mm at the coated point and the silicon nitride coating a thickness of 100 ⁇ m to 300 ⁇ m.
  • the silicon nitride layer system was a multilayer system which acted as a barrier to the molten silicon.
  • the crucible was rectangular and had a depth of about 50 cm with a width of about 40 cm by 40 cm.
  • Further preferred dimensions of the rectangular crucible were preferably at its first bottom side 650 to 950 mm by 650 to 950 mm at its second bottom side and 400 to 600 mm in height at its side walls. These crucibles were coated in their interior either over the entire surface or almost the entire surface, this means with an upper edge of a few, that is up to 10 cm, coated so that the layer was within the specified deviations from the nominal layer thickness.
  • FIG. 16 shows the locally measured intensity intensity and thus layer thickness profile on the pulse-thermographically measured surface
  • FIG. 17 shows the locally measured intensity and therefore layer thickness profile measured on the surface of a further quartz crucible, which has an intact silicon nitride layer, seen obliquely from above, as measured by pulse thermography.
  • the invention allows by their method non-metallic body with non-metallic coating to produce, in particular ceramic body with ceramic coating, which particularly high
  • the material or the crucible material can also consist of sintered silicon nitride, graphite, and / or fiber-reinforced graphite.
  • the method according to the invention is used during the coating and before the thermal fixation of the ceramic layer, it is possible to detect points with too low a coating and to locally repair them.
  • a deviation of less than 20 microns from the target layer thickness could be achieved. In most cases, this deviation was less than 5 microns, of which target layer thickness in an area of the surface of 10 by 10 cm, preferably 100 by 100 cm.
  • a relevant coating area is understood to mean the area which later comes into contact with the semiconductor melt and consequently has to provide the barrier properties. This relevant area can also be have an upper edge of a few cm, which is still outside this precise layer thickness.
  • thermographic lock-in process in which, instead of a heat pulse, a periodic heat input, for example as a sinusoidal function over time, was measured and measured synchronously.
  • this method is an excellent means for testing the coating quality, especially of ceramic barrier layers on ceramic substrates, including three-dimensional ceramic substrates.
  • ceramic materials or bodies are also to be understood as meaning glass-ceramic materials or bodies.

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Abstract

L'invention concerne un procédé pour l'essai thermographique de matériaux non métalliques, en particulier de matériaux non métalliques revêtus, procédé selon lequel on procède à une chauffe au moins dans une partie de la surface du matériau non métallique, de préférence dans une partie de la surface munie d'un revêtement non métallique, en particulier à l'aide d'une impulsion d'énergie de courte durée, de préférence d'une impulsion lumineuse, ou par un apport périodique de chaleur, et l'évolution temporelle et spatiale de la température est enregistrée au moins à plusieurs instants successifs. L'invention concerne également un procédé de fabrication reposant sur l'utilisation de ce procédé, et des objets fabriqués selon ledit procédé de fabrication.
EP09725446A 2008-03-28 2009-03-28 Procédé d'essai thermographique de matériaux non métalliques, en particulier de matériaux non métalliques revêtus, ainsi que leur procédé de fabrication, et objets fabriqués selon ce procédé Withdrawn EP2263076A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102008016272 2008-03-28
PCT/EP2009/002284 WO2009118199A1 (fr) 2008-03-28 2009-03-28 Procédé d'essai thermographique de matériaux non métalliques, en particulier de matériaux non métalliques revêtus, ainsi que leur procédé de fabrication, et objets fabriqués selon ce procédé

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