Classifications

• • C—CHEMISTRY; METALLURGY
  • C03—GLASS; MINERAL OR SLAG WOOL
  • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
  • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
  • C03C23/0005—Other surface treatment of glass not in the form of fibres or filaments by irradiation
  • C03C23/0015—Other surface treatment of glass not in the form of fibres or filaments by irradiation by visible light
• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
  • G01N21/84—Systems specially adapted for particular applications
  • G01N21/88—Investigating the presence of flaws or contamination
  • G01N21/89—Investigating the presence of flaws or contamination in moving material, e.g. running paper or textiles
  • G01N21/892—Investigating the presence of flaws or contamination in moving material, e.g. running paper or textiles characterised by the flaw, defect or object feature examined
  • G01N21/896—Optical defects in or on transparent materials, e.g. distortion, surface flaws in conveyed flat sheet or rod
• • C—CHEMISTRY; METALLURGY
  • C03—GLASS; MINERAL OR SLAG WOOL
  • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
  • C03C3/00—Glass compositions
  • C03C3/04—Glass compositions containing silica
  • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
  • C03C3/078—Glass compositions containing silica with 40% to 90% silica, by weight containing an oxide of a divalent metal, e.g. an oxide of zinc
• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
  • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
  • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
  • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
  • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
  • G01N21/255—Details, e.g. use of specially adapted sources, lighting or optical systems
• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
  • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
  • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
  • G01N21/256—Arrangements using two alternating lights and one detector
• • C—CHEMISTRY; METALLURGY
  • C03—GLASS; MINERAL OR SLAG WOOL
  • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
  • C03C3/00—Glass compositions
  • C03C3/04—Glass compositions containing silica
  • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
  • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
  • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
  • C03C3/087—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal containing calcium oxide, e.g. common sheet or container glass
• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
  • G01N21/84—Systems specially adapted for particular applications
  • G01N21/88—Investigating the presence of flaws or contamination
  • G01N21/8806—Specially adapted optical and illumination features
  • G01N2021/8845—Multiple wavelengths of illumination or detection

Definitions

• Example embodiments of this invention relate to a method and/or system for detecting inclusions and/or other defects (e.g., micro inclusions such as nickel sulfide based inclusions/defects) in soda-lime-silica based glass, such as float glass.
• light e.g., visible light
• different wavelengths of reflected light e.g., refracted and/or scattered light
• inclusions can be detected based on differentiating between the different wavelengths.
• nickel sulfide inclusions have surface roughness features that will affect a given wavelength range (e.g., 400-500 nm) differently than another wavelength range(s) (e.g., 600-650 nm).
• nickel sulfide inclusions have surface roughness features that will diffract more blue light than red light, thereby providing different degrees of scattering at different wavelengths.
• nickel sulfide based inclusions may be detected based on different wavelengths being affected (e.g., diffracted and/or scattered) differently, whereas float glass itself absent inclusions or having inclusions with smooth mirror-like surfaces does not have such an effect.
• a molten material e.g., tin bath
• light from at least one light source(s) is directed at the resulting glass and inclusions may be detected based on analyzing and/or comparing reflected light (e.g., refracted and/or scattered light) as a function of wavelength (l). For example, significant differences in reflected light (e.g., refracted and/or scattered) at a given location may indicate the presence of a nickel sulfide based inclusion.
• the float glass ribbon is then forwarded to an annealing lehr for further processing and then may be cut to form solid glass articles, such as flat glass sheets.
• the glass batch often includes soda, lime and silica to form soda-lime-silica based flat glass.
• Float glass is widely used for windows in commercial and residential buildings, glass furniture, shower doors, and automotive windshields.
• float glass must be thermally tempered (undergo heating to at least 580 degrees C, followed by a rapid cooling) to ensure safety in case of breakage.
• Impurities from raw materials, sulfur from additive(s), and/or contaminations from the float process occasionally and unpredictably form unwanted chemical compounds (e.g., inclusions) during glass formation, which are undesirable defects in the glass.
• Nickel for example, is known to spontaneously bond with sulfur to form inclusions of or based on nickel sulfide (of any suitable stoichiometry such as NiS).
• NiS inclusions are known for causing spontaneous breakage of thermally tempered glass. Moreover, NiS inclusions/defects in thermally tempered glass have caused catastrophic glass failure over long periods of time in installed products. Rejecting defective annealed glass, therefore, serves at least two purposes: a) increase production yield during the expensive thermal tempering and heat soaking stages, and b) minimize catastrophic failures of glass in installed products.
• Nickel sulfide exists in different phases at different temperatures. For instance, two specific phases of NiS known are the alpha-phase and the beta-phase.
• nickel sulfide is relatively stable in the beta- phase form. Above this temperature, it is stable in the alpha-phase. Therefore, when glass is produced in a furnace, it is likely that any NiS inclusions will be in the alpha- phase. In typical annealed glass, the slow cooling process provided by the annealing lehr allows the NiS ample time to transform to its beta-phase as the glass cools.
• Nickel sulfide is a compound that comes in various forms as well.
• the most common forms of nickel sulfide are Ni 7 S6, NiS, NiSi . 03, M3S2 and NfSi+Ni.
• M7S6, NiS, and NiS 1.03 are yellow-gold in color and have a rugged surface similar to a golf ball. These three types are non-magnetic and have been found to cause failure in tempered glass.
• a method and/or system for detecting inclusions (e.g., nickel sulfide based inclusions/defects) in soda-lime-silica based glass.
• Inline systems and/or methods discussed herein may be used to detect, for example, inclusions and/or other defects in float glass, such as nickel sulfide inclusions and/or other micro-defects having a size of from about 30-200 pm, more preferably from about 40-150 pm, and/or may be used to differentiate such nickel sulfide based inclusions from other inclusions.
• the soda-lime-silica based glass comprises a base glass portion that includes, by weight percentage: S1O267 - 75 %, Na 2 0 10 - 20 %, CaO 5 - 15 %, Al 2 0 3 0 - 7 %, MgO 0-7%, and K 2 0 0 - 7 %.
• a colorant portion of the glass may further include one or more colorants such as iron, selenium, cobalt, erbium and/or the like.
• a method and/or system for detecting inclusions and/or other defects e.g., micro inclusions such as nickel sulfide based inclusions/defects
• soda-lime-silica based glass such as float glass.
• light e.g., visible light
• different wavelengths of reflected light e.g., refracted and/or scattered light
• inclusions can be detected based on differentiating between the different wavelengths.
• nickel sulfide inclusions have surface roughness features that will affect a given wavelength range (e.g., 400-500 nm) differently than another wavelength range(s) (e.g., 600-650 nm).
• nickel sulfide inclusions have surface roughness features that will diffract more blue light than red light, thereby providing different degrees of scattering at different wavelengths.
• nickel sulfide based inclusions may be detected based on different wavelengths being affected (e.g., diffracted and/or scattered) differently, whereas float glass itself absent inclusions or having inclusions with smooth mirror-like surfaces does not have such an effect.
• reflected light e.g., refracted and/or scattered light
• l wavelength
• a system for detecting an inclusion in glass including a base glass composition comprising: Si0 2 67 75 %, Na 2 0 10 - 20 %, CaO 5 - 15 %, Al 2 0 3 0 - 7 %, K 2 0 0 - 7 %, the system comprising: at least one light source for directing light toward the glass; and a processor configured to determine whether an inclusion comprising nickel sulfide is present in the glass based at least on a difference between first and second reflected wavelengths.
• a system for detecting an inclusion in glass including a base glass composition comprising: Si0 2 67 75 %, Na 2 0 10 - 20 %, CaO 5 - 15 %, Al 2 0 3 0 - 7 %, K 2 0 0 - 7 %, the system comprising: at least one light source for directing light toward the glass; and a processor configured to determine whether an inclusion comprising nickel sulfide is present in the glass based at least reflectance of first and second reflected wavelengths from the glass.
• Fig. 1 is a graph illustrating the absorption of nickel sulfide inclusions that may be present in float glass, versus wavelength (nm).
• Fig. 2 is a graph illustrating the transmission (%T) of an example soda-lime- silica based float glass, versus wavelength (nm).
• Fig. 3 includes a plurality of pictures of nickel sulfide inclusions (left two columns) and non-NiS metallic inclusions (right two columns) in glass with respect to incident blue light and incident red light at different contrast levels.
• Fig. 4 is a schematic diagram of a system for detecting inclusions in float glass according to an example embodiment of this invention.
• the soda-lime-silica based glass 1 comprises a base glass portion that includes, by weight percentage: S1O267 - 75 %, Na 2 0 10 - 20 %, CaO 5 - 15 %, Al 2 0 3 0 - 7 %, MgO 0-7%, and K 2 0 0 - 7 %.
• a colorant portion of the glass may further include one or more colorants such as iron, selenium, cobalt, erbium and/or the like.
• the glass 1 may be a different type of glass such as borosilicate glass, aluminosilicate glass, or the like.
• An example soda-lime-silica base glass 1 according to certain embodiments of this invention that may be made via the float process or other suitable process, on a weight percentage basis, includes the following basic ingredients:
• glass 1 herein may be made from batch raw materials silica sand, soda ash, dolomite, limestone, with the use of salt cake (S0 3 ) as a refining agent. Reducing and oxidizing agent(s) may also be used in certain instances.
• soda-lime-silica base glasses 1 herein may include by weight from about 10- 15% Na 2 0 and from about 6-12% CaO.
• the glass batch and/or final glass 1 may also include a colorant portion including material(s) such as iron, erbium, cobalt, selenium and/or the like in suitable amounts in order to provide coloration and/or absorption to the glass in a desired manner.
• the amount of total iron in the glass may be from about 0.05 to 1.2%, more preferably from about 0.3 to 0.8%. In the case of certain clear high transmission glasses, the total iron may be from about 0.005 to 0.025%.
• the total amount of iron present in the glass, and thus in the colorant portion thereof, is expressed herein in terms of Fe 2 0 3 in accordance with standard practice.
• the glass batch raw materials e.g., silica sand, soda ash, dolomite, limestone, colorant(s), etc.
• the glass melt is poured onto a bath of molten material such as tin (tin bath), where the glass is formed and continuously cooled to form a float glass ribbon.
• tin bath molten material
• the float glass ribbon proceeds toward an annealing lehr for slow cooling.
• lateral edge portion(s) of the glass sheet may be trimmed in a hot condition.
• the glass sheet typically reaches the beginning of the annealing lehr at a temperature of at least about 540 degrees C, more preferably at least about 580 degrees, C, with a possible range from about 540 (or 580) to 800 degrees C.
• the temperature of the glass sheet strip is slowly cooled from the annealing point (e.g., from about 538-560 degrees C) to a strain point of from about 495-560 degrees C, which may be referred to as an annealing range. While these temperature ranges are preferred for annealing, different temperatures may be used in certain instances.
• the continuous glass sheet may be supported by either rollers or gas during annealing. After annealing, the continuous glass sheet is moved on for further processing such as one or more of cutting, additional cooling, coating and/or the like.
• NiS is generally an opaque material, which makes it absorbent to certain light wavelengths for which glass is transparent.
• Float glass 1 for instance, is substantially absorbent in ultra-violet (UV) and near-infrared (NIR) regions.
• UV ultra-violet
• NIR near-infrared
• Fig. 4 illustrates an example system for detecting inclusions and/or other defects (e.g., micro inclusions such as nickel sulfide based inclusions/defects) in soda-lime- silica based glass 1, such as float glass moving in direction D on rollers 3.
• light e.g., visible light, which includes red, green and blue wavelengths
• L light from at least one light source LS
• different wavelengths of reflected light (e.g., refracted and/or scattered light) R, R’ from the at least one light source are analyzed and compared and inclusions can be detected based on differentiating between the different wavelengths.
• the light from the source(s) LS1, LS2 may or may not be focused on the glass 1, such as being focused on the upper surface of the glass.
• nickel sulfide inclusions in the glass 1 have surface roughness features that will affect a given wavelength range (e.g., 400-500 nm) differently than another wavelength range(s) (e.g., 600-650 nm).
• nickel sulfide inclusions have surface roughness features that will diffract more blue light than red light, thereby providing different degrees of scattering at different wavelengths such as at blue and red wavelengths.
• nickel sulfide based inclusions in the glass 1 may be detected based on different wavelengths being affected (e.g., diffracted and/or scattered) differently, whereas float glass itself absent inclusions does not have such an effect.
• color filter 1 may filter the visible light from light source LS1 so as to filter out green and blue light, so that light detector 1 receives and analyzed reflected (e.g., refracted and/or scattered) red light
• color filter 2 may filter the visible light from light source LS2 so as to filter out green and red light, so that light detector 2 receives and analyzed reflected (e.g., refracted and/or scattered) blue light.
• color filters are optional, and in embodiments where one or both of the color filters are not present the processing system may analyze and compare particular wavelengths.
• a computer and/or computer system including a processor and a comparator (which may be part of the processor), then analyzes the reflected red and blue light and determines whether nickel sulfide based inclusion(s) is/are present based on at least the difference between the reflected red and blue light from a given glass location.
• a nickel sulfide based inclusion is present in a given area/location of the glass 1 when the difference between (a) the brightness, intensity, degree, size, and/or amount of red light reflected (e.g., refracted and/or scattered) from that area/location, and (b) the brightness, intensity, degree, size, and/or amount of blue light reflected (e.g., refracted and/or scattered) from that area/location, is greater than a predetermined value.
• a nickel sulfide based inclusion(s) may indicate the presence of a nickel sulfide based inclusion(s).
• the system shown in Fig. 4 for detecting inclusions, such as nickel sulfide (of any stoichiometry) based inclusions, in the glass 1 may be located on the float line after the annealing lehr, and before or after a glass cutting station, in certain example embodiments of this invention. When inclusion(s) are found in the glass, that portion of the glass is discarded and/or not subjected to thermal tempering.
• the light source(s) LS1, LS2 may be pulsed or continuous in different example embodiments, and may be a single source or an array of light sources. Nickel sulfide based inclusions in the glass 1 are thus detected based on wavelength.
• Glass made in this manner, after passing the detection station with no inclusions being detected is useful, for example and without limitation, in glass window applications for buildings and/or vehicles, solar cell applications, furniture glass applications, and/or display glass applications.
• a method of detecting nickel sulfide (e.g., NiS) based inclusions is based on a nickel sulfide inclusion, due to its crystalline nature, has surface micro-roughness, and the size of this micro-roughness is at least on the scale of visible light (400-700 nm). Reflecting and then analyzing light of various colors (wavelengths) in this range from inclusions allows for discriminating between nickel sulfide inclusions/defects and other types of inclusions/defects.
• NiS nickel sulfide
• light from the same light source(s) is sent toward the glass from essentially the same angle (e.g., light from sources LS1 and LS2 is directed toward the moving glass in Fig. 4 from the same angle), but with at least two different colors, and then a processor is provided for analyzing (e.g., comparing) the images (e.g., see images in Fig. 3).
• a processor is provided for analyzing (e.g., comparing) the images (e.g., see images in Fig. 3).
• non-NiS inclusions such as metallic inclusions for example in the two right columns of Fig. 3
• the smooth surface of such inclusions will cause no significant difference in the reflected image off and around the inclusion between different colors, as shown in the two right columns of Fig. 3.
• Fig. 3 demonstrates an example comparison between a nickel sulfide inclusion (left two columns) and a non-NiS metallic inclusion (right two columns), under blue and red light at different contrast levels.
• Fig. 4 illustrates an example system and apparatus to detect the inclusions and identify their nature, such as whether or not nickel sulfide based inclusions are present and/or whether a given inclusion is nickel sulfide based.
• Row 1 illustrates less contrast in processing
• Row 3 in Fig. 3 illustrates more contrast in processing of the reflected signals
• Row 2 in Fig. 3 illustrates what occurs when a medium amount of contrast is used during processing of the reflected red and blue wavelengths.
• Row 3 with increased contrast used during processing the red and green reflected wavelengths, demonstrates that very different red and blue reflected images are provided for the nickel sulfide based inclusion in the left two columns (but not for the metallic inclusion in the right two columns).
• the detection of a significant different between the blue and red reflections off the inclusion evidences the presence of a nickel sulfide based inclusion.
• the defective glass may undergo a pass/reject algorithm, such that it may either be rejected or sent for a detailed identification of inclusions. If no nickel sulfide based inclusions are present, the glass 1 may still be used in production.
• a system and/or method of detecting nickel sulfide based inclusions in annealed or tempered glass are identified based on scattering light of at least two different colors (wavelengths) from the defect.
• the reflection of light of at least two different colors produces different reflected images of a nickel sulfide based inclusion due to slightly different diffraction of different wavelengths with morphological features of nickel sulfide based inclusions (e.g., see two left columns in third row of Fig. 3).
• the two colors of light are in the visible wavelength range.
• the first color may be blue (e.g., 400-480 nm) and the second color may be red (e.g., 650-700 nm).
• the two colors of light are in different spectral regions of the visible spectrum. While the two colors are preferably in the visible part of the spectrum, it is possible that one or more may be outside the visible spectrum. It is also possible that green light may replace red or blue.
• one of the two wavelengths of light may be in the visible spectrum, while the other is in the near infra-red (e.g., 700-1200 nm).
• one of the two wavelengths of light may be in the visible spectrum, while the other is in the UV portion of the spectrum, but at a wavelength longer than the absorption edge of glass (the absorption edge varies depending on the type of glass and can range from 200 to 380 nm).
• one of the two wavelengths of light may be in the near-IR, while the other is in the UV part of the spectrum.
• light of two or more wavelengths is used for the detection of inclusions such as NiS inclusions.
• the inclusion detection system may be inline or offline.
• a system for detecting an inclusion in glass including a base glass composition comprising: Si0 2 67 - 75 %, Na 2 0 10 - 20 %, CaO 5 - 15 %, Al 2 0 3 0 - 7 %, K 2 0 0 - 7 %, the system comprising: at least one light source for directing light toward the glass; and a processor configured to determine whether an inclusion comprising nickel sulfide is present in the glass based at least on a difference between first and second reflected wavelengths.
• the first wavelength may be a red wavelength and/or the second wavelength may be a blue wavelength.
• the first wavelength may comprise wavelengths in a range from about 650-700 nm.
• the second wavelength may comprise wavelengths in a range from about 400-480 nm.
• the reflected wavelengths may be wavelengths refracted and/or scattered by the inclusion in the glass.
• the at least one light source may comprise a first light source and a second light source, which may be oriented at substantially the same angle relative to the glass.
• a first color filter may be provided between the glass and the first light source, and a second color filter may be provided between the glass and the second light source.
• the processor may be configured for determining whether an inclusion comprising nickel sulfide is present in the glass based at least on a difference between first and second reflected wavelengths at least by analyzing at least one image comprising reflections from the inclusion.
• the processor may be configured to determine whether to pass or reject the glass based at least on whether an inclusion comprising nickel sulfide is detected.
• the light source may be located on and/or in a float line, and may be positioned after an annealing lehr of the float line.
• the processor may be configured to determine that the inclusion comprising nickel sulfide is present in the glass when a difference between (a) one or more of a brightness, intensity, degree, size, and/or amount of red light reflected from the inclusion, and (b) one or more of a brightness, intensity, degree, size, and/or amount of blue light reflected from the inclusion, is greater than a predetermined value.

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• 2019
  • 2019-03-07 BR BR112020013803-7A patent/BR112020013803B1/pt not_active IP Right Cessation
  • 2019-03-07 EP EP19715571.6A patent/EP3762344A1/en not_active Withdrawn
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