WO2022234181A1 - Procédé de bombardement électronique de matériau luminescent - Google Patents

Procédé de bombardement électronique de matériau luminescent Download PDF

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WO2022234181A1
WO2022234181A1 PCT/FI2022/050266 FI2022050266W WO2022234181A1 WO 2022234181 A1 WO2022234181 A1 WO 2022234181A1 FI 2022050266 W FI2022050266 W FI 2022050266W WO 2022234181 A1 WO2022234181 A1 WO 2022234181A1
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combination
group
elements
cations
periodic table
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Mika LASTUSAARI
Isabella PÖNKKÄ
Minnea TUOMISTO
Hannah BYRON
Sami VUORI
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Pure Luminescence Technologies Oy
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    • C09K11/58—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold
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    • C09K11/61—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing fluorine, chlorine, bromine, iodine or unspecified halogen elements
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    • C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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    • C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
    • C09K11/677—Germanates
    • 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
    • G01J1/00—Photometry, e.g. photographic exposure meter
    • G01J1/58—Photometry, e.g. photographic exposure meter using luminescence generated by light

Definitions

  • the present invention relates to luminescent materials and their treatment by electron bombardment.
  • the present invention also relates to a method for increasing intensity of optically stimulated luminescence of such materials, and to a method for decreasing afterglow of such materials. Further, the invention relates to a method for increasing contrast of an image selected from computed radiography, computed tomography and digital radiography, the material used for imaging comprising the present material.
  • a method for treating a luminescent material by electron bombardment In particular, a material represented by formula (I) is treated by electron bombardment
  • - M’ represents a monoatomic cation of an alkali metal selected from Group 1 of the IUPAC periodic table of the elements, or any combination of such cations;
  • - M represents a trivalent monoatomic cation of an element selected from Group 13 of the IUPAC periodic table of the elements, or of a transition element selected from any of Groups 3 - 12 of the IUPAC periodic table of the elements, or any combination of such cations;
  • - M’ represents a monoatomic cation of an element selected from Group 14 of the IUPAC periodic table of the elements, or of an element selected from any of Groups 13 and 15 of the IUPAC periodic table of the elements, or of Zn, or any combination of such cations;
  • - X represents an anion of an element selected from Group 17 of the IUPAC periodic table of the elements, or any combination of such anions, or wherein X is absent;
  • - X’ represents an anion of one or more elements selected from Group 16 of the IUPAC periodic table of the elements, or any combination of such anions, or wherein X’ is absent;
  • - M represents a dopant cation of an element selected from rare earth metals of the IUPAC periodic table of the elements, or from transition metals of the IUPAC periodic table of the elements, or of Ba, Sr, Tl, Pb, or Bi, or any combination of such cations, or wherein M”” is absent; with the proviso that at least one of X and X’ is present, the electron bombardment being carried out in a vacuum chamber having a pressure enabling formation of an electron beam.
  • a method for increasing intensity of optically simulated luminescence of a material represented by formula (I), by carrying out the electron bombardment treatment described above According to a third aspect, there is provided a method for decreasing afterglow of a material represented by formula (I), by carrying out the electron bombardment described above.
  • Figure 1 illustrates the decrease of optically stimulated luminescence afterglow in electron bombarded material of formula (I) according to one embodiment compared to non-treated material.
  • Figure 2 illustrates the decrease of optically stimulated luminescence afterglow in electron bombarded material of formula (I) according to another embodiment compared to non-treated material.
  • Figure 3 illustrate the decrease of optically stimulated luminescence afterglow in electron bombarded material of formula (I) according to a further embodiment compared to non- treated material.
  • Figure 4 illustrates the decrease of normal afterglow in electron bombarded material of formula (I) according to one embodiment compared to non-treated material.
  • Figure 5 illustrates the decrease of normal afterglow in electron bombarded material of formula (I) according to another embodiment compared to non-treated material.
  • Figure 6 illustrates the increase of intensity of optically stimulated luminescence in electron bombarded material according to an embodiment.
  • Figure 7 illustrates the increase of intensity of optically stimulated luminescence in electron bombarded material according to a further embodiment.
  • Figure 8 illustrates the increase of intensity of optically stimulated luminescence in electron bombarded material according to another embodiment.
  • Figure 9 illustrates the effect of the time of electron bombardment on the intensity of optically stimulated luminescence according to an embodiment.
  • Figure 10 illustrates the effect of the time of electron bombardment on the intensity of optically stimulated luminescence according to the embodiment of Figure 9.
  • Figure 11 illustrates the effect of heat treatment and electron bombardment on the intensity of optically stimulated luminescence according to an embodiment.
  • Figure 12 illustrates the effect of an UV radiation on CR image, according to an embodiment.
  • Figure 13 illustrates the effect of an UV radiation on CR image, according to another embodiment.
  • Figure 14 illustrates ultraviolet enhancement of polymer emission for an embodiment.
  • Figure 15 illustrates ultraviolet enhancement of polymer emission for another embodiment.
  • Figure 16 illustrates ultraviolet enhancement of polymer emission for a further embodiment.
  • the expression “monoatomic ion” should be understood as an ion consisting of a single atom. If an ion contains more than one atom, even if these atoms are of the same element, it is to be understood as a polyatomic ion. Thus, in this specification, unless otherwise stated, the expression “monoatomic cation” should be understood as a cation consisting of a single atom.
  • the present description relates to a method for treating a luminescent material by electron bombardment.
  • the material to be treated is represented by formula I
  • - M’ represents a monoatomic cation of an alkali metal selected from Group 1 of the IUPAC periodic table of the elements, or any combination of such cations;
  • - M represents a trivalent monoatomic cation of an element selected from Group 13 of the IUPAC periodic table of the elements, or of a transition element selected from any of Groups 3 - 12 of the IUPAC periodic table of the elements, or any combination of such cations;
  • - M’ represents a monoatomic cation of an element selected from Group 14 of the IUPAC periodic table of the elements, or of an element selected from any of Groups 13 and 15 of the IUPAC periodic table of the elements, or of Zn, or any combination of such cations;
  • - X represents an anion of an element selected from Group 17 of the IUPAC periodic table of the elements, or any combination of such anions, or wherein X is absent;
  • - X’ represents an anion of one or more elements selected from Group 16 of the IUPAC periodic table of the elements, or any combination of such anions, or wherein X’ is absent;
  • - M represents a dopant cation of an element selected from rare earth metals of the IUPAC periodic table of the elements, or from transition metals of the IUPAC periodic table of the elements, or of Ba, Sr, Tl, Pb, or Bi, or any combination of such cations, or wherein M”” is absent; with the proviso that at least one of X and X’ is present, the electron bombardment being carried out in a vacuum chamber having a pressure enabling formation of an electron beam.
  • the material of formula (I) is an optically active material that is configured to be able to retain radiation such as X-radiation exposed thereon, i.e. the material is able to trap therein the radiation that it is exposed to, and to release the retained radiation as visible light when being subjected to optical stimulation, i.e. the retained radiation may be released from the material later at a desired point of time.
  • the present description thus concerns the materials represented by formula (I), which are electron bombarded after their manufacture.
  • the present electron bombardment reduces the OSL afterglow of the materials, and increases the OSL signal intensity.
  • Electron bombardment is a generally known ionization method in which electrons interact with solid or gas phase atoms or molecules to produce ions. Ionization by electron bombardment uses highly energetic electrons to produce ions, which leads to extensive fragmentation. Electron bombardment is non-selective ionization method which provides high ionization efficiency and sensitivity.
  • the material is preferably treated with the electron bombardment in powder form.
  • the powder sample is spread as a thin surface onto a sample holder which is then put into a vacuum.
  • the sample is being bombarded, typically small area at a time until the whole sample surface has been treated.
  • the apparatuses for carrying out electron bombardment are known as such.
  • the electron bombardment of material having the formula (I) is carried out in a vacuum chamber having a pressure enabling formation of an electron beam. For some typical equipment, this means a pressure of at most 15 Pa.
  • the vacuum chamber has a pressure of at most 10 Pa, for example at most 5 Pa.
  • the vacuum chamber can for example have a pressure of 1, 3, 5, 1, 10 or 12 Pa up to 3, 5, 7, 10, 12 or 15 Pa.
  • the electron bombardment is carried out using a voltage of 0.1-50 kV.
  • the voltage can be from 0.1, 1, 5, 8, 10, 12, 15, 18, 20, 22, 25, 28, 30, 32, 35, 37, 40, 42, 45 or 47 kV up to 1, 5, 8, 10, 12, 15, 18, 20, 22, 25, 28, 30, 32, 35, 37, 40, 42, 45, 47 or 50 kV.
  • the electron bombardment is carried our using a current of 0.01-0.5 mA.
  • the current can be from 0.01, 0.05, 0.1, 0.15, 0.2, 0.25, 0.3, 0.35, 0.4 or 0.45 mAup to 0.05, 0.1, 0.15, 0.2, 0.25, 0.3, 0.35, 0.4, 0.45 or 0.5 mA.
  • the electron bombardment is carried out for a period of time.
  • the time used for electron bombardment is typically selected based on the other process parameters.
  • the material is exposed to the electron bombardment for a time period of 1 to 40 minutes.
  • the time could be even less than one minute or more than 40 minutes, such as 45 minutes or an hour.
  • the time can be from 1, 2, 3, 4, 6, 9,10, 15, 20, 25 or 30 minutes up to 2, 3, 4, 6, 9, 10, 15, 20, 25, 30, 35 or 40 minutes.
  • M’ represents a monoatomic cation of an alkali metal selected from a group consisting of Na, Li, K, Rb, Cs, and Fr, or any combination of such cations.
  • M’ represents a monoatomic cation of an alkali metal selected from Group 1 of the IUPAC periodic table of the elements, or any combination of such cations, with the proviso that M’ does not represent the monoatomic cation of Na alone.
  • M’ represents a combination of at least two monoatomic cations of different alkali metals selected from a group consisting of Li, Na, K, Rb, Cs, and Fr.
  • M’ represents a combination of at least two monoatomic cations of different alkali metals selected from Group 1 of the IUPAC periodic table of the elements. In one embodiment, M’ represents a combination of at least two monoatomic cations of different alkali metals selected from Group 1 of the IUPAC periodic table of the elements, wherein the combination comprises at most 98 mol-%, at most 95 mol-%, at most 90 mol- %, at most 85 mol-%, at most 80 mol-%, at most 70 mol-%, at most 60 mol-%, at most 50 mol-%, at most 40 mol-% of the monoatomic cation of Na, or at most 30 mol-% of the monoatomic cation of Na, or at most 20 mol-% of the monoatomic cation of Na.
  • M’ represents a monoatomic cation of Li. In one embodiment, M’ represents a monoatomic cation of K. In one embodiment, M’ represents a monoatomic cation of Rb. In one embodiment, M’ represents a monoatomic cation of Cs. In one embodiment, M’ represents a monoatomic cation of Fr.
  • M represents a trivalent monoatomic cation of a metal selected from a group consisting of A1 and Ga, or a combination of such cations. In one embodiment, M” represents a trivalent monoatomic cation of B. In one embodiment, M” represents a trivalent monoatomic cation of a transition element selected from Period 4 of the IUPAC periodic table of the elements, or any combination of such cations. In one embodiment, M” represents a trivalent monoatomic cation of an element selected from a group consisting of Cr, Mn, Fe, Co, Ni, and Zn, or any combination of such cations.
  • M’ represents a monoatomic cation of an element selected from a group consisting of Si, Ge, Al, Ga, N, P, and As, or any combination of such cations. In one embodiment, M’” represents a monoatomic cation of an element selected from a group consisting of Si and Ge, or a combination of such cations. In one embodiment, M’ represents a monoatomic cation of an element selected from a group consisting of Al, Ga, N, P, and As, or any combination of such cations. In one embodiment, M’” represents a monoatomic cation of an element selected from a group consisting of Al and Ga, or a combination of such cations. In one embodiment, M’” represents a monoatomic cation of an element selected from a group consisting of N, P, and As, or any combination of such cations. In one embodiment, M’” represents a monoatomic cation of Zn.
  • X represents an anion of an element selected from a group consisting of F, Cl, Br, I, and At, or any combination of such anions. In one embodiment, X represents an anion of an element selected from a group consisting of F, Cl, Br, and I, or any combination of such anions. In one embodiment, X is absent.
  • X’ represents an anion of an element selected from a group consisting of O, S, Se, and Te, or any combination of such anions. In one embodiment, X’ represents an anion of one or more elements selected from a group consisting of O, S, Se, and Te, or any combination of such anions. In one embodiment, X’ represents a monoatomic or a polyatomic anion of one or more elements selected from a group consisting of O, S, Se, and Te, or any combination of such anions. In one embodiment, X’ represents an anion of
  • X’ is (SO 4 ) 2 In yet another embodiment X’ is absent.
  • the proviso that at least one of X and X’ is present should in this specification, unless otherwise stated, be understood such that either X or X’ is present, or such that both X and X’ are present.
  • the material is doped with at least one transition metal ion.
  • the material is represented by formula (I), wherein M” represents a cation of an element selected from transition metals of the IUPAC periodic table of the elements, or of Ba, Sr, Tl, Pb, or Bi, or any combination of such cations.
  • M” represents a cation of an element selected from transition metals of the f-block of the IUPAC periodic table of the elements.
  • M” represents a cation of an element selected from transition metals of the d-block of the IUPAC periodic table of the elements.
  • M represents a cation of an element selected from a group consisting of Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Ag, W, and Zn, or any combination of such cations.
  • M” represents a cation of Ti.
  • M” represents a dopant cation of an element selected from rare earth metals of the IUPAC periodic table of the elements.
  • M” represents a cation of an element selected from a group consisting of Yb, Er, Tb, and Eu, or any combination of such cations.
  • M” represents a combination of two or more dopant cations.
  • the material is represented by formula (I), wherein M”” is absent. In this embodiment, the material is not doped. In one embodiment, the material represented by the formula (I) comprises M”” in an amount of 0.001 - 10 mol-%, or 0.001 - 5 mol-%, or 0.1 - 5 mol-% based on the total amount of the material.
  • the material represented by formula (I) comprises residuals. These residuals originate from the manufacturing process of the material, and may be present in an amount of up to 1 mol-%, or even more, such as up to 10 mol-%. In one embodiment, the material represented by formula (I) is selected from a group consisting of:
  • Some further suitable materials are where the amount of Sr varies from 3 to 6 mol-%.
  • the material may also comprise Cu, for example in the amount of 1 mol-%.
  • Some suitable materials represented by formula (I) can be selected from a group consisting of:
  • the material may be synthesized by a reaction according to Norrbo et al. (Norrbo, L; Gluchowski, P.; Paturi, P.; Sinkkonen, J.; Lastusaari, M., Persistent Luminescence of TenebrescentNa 8 Al 6 Si 6 O 24 (Cl,S) 2 : Multifunctional Optical Markers. Inorg. Chem. 2015,
  • NaCl, KC1 and/or RbCl can be used as the starting materials.
  • the at least one dopant may be added as an oxide, such as TiO 2, a chloride, a sulfide, a bromide, or a nitrate.
  • the material can be prepared as follows: Zeolite A may first be dried at 500 °C for 1 h. The initial mixture may then be heated at 850 °C in air for e.g. 2 h, 5 h, 12 h, 24 h, 36 h, 48 h, or 72 h. The product may then be freely cooled down to room temperature and ground. Finally, the product may be re-heated at 850 °C for 2 h under a flowing 12 % H 2 + 88 %
  • the as-prepared materials may be washed with water to remove any excess LiCl/NaCl/KCl/RbCl impurities. The purity can be verified with an X-ray powder diffraction measurement.
  • the material is prepared in powder form, and is typically also used in powder form.
  • the particle size of the power is typically about 5-10 ⁇ m 2 , as measured by transmission electron microscopy, the area is determined from the pictures with a watershed segmentation algorithm in the ImageJ program.
  • the material treated has formula (II) (M , ) 8 (M”M , ”) 6 O 24 (X,S) 2 :M”” formula (II) wherein
  • - M’ represents a monoatomic cation of an alkali metal selected from Group 1 of the IUPAC periodic table of the elements, or any combination of such cations;
  • - M represents a trivalent monoatomic cation of an element selected from Group 13 of the IUPAC periodic table of the elements, or of a transition element selected from any of Groups 3 - 12 of the IUPAC periodic table of the elements, or any combination of such cations;
  • - M’ represents a monoatomic cation of an element selected from Group 14 of the IUPAC periodic table of the elements, or any combination of such cations;
  • - X represents an anion of an element selected from Group 16 of the IUPAC periodic table of the elements, or from Group 17 of the IUPAC periodic table of the elements, or any combination of such anions;
  • the material of the present description is typically non-toxic and non-expensive and also has the benefit of being reusable and recyclable.
  • the present description also relates to the present method of electron bombardment, followed by treating the electron bombarded material with heat treatment.
  • the present electron bombardment can be carried out on a material that has been heat treated as explained below.
  • the manufacturing process of these materials includes re-heating (as will be explained below), and therefore the present heat treatment is a further re-heating of the material.
  • the present heat treatment reduces the OSL afterglow of the materials, and increases the OSL signal intensity.
  • the heat treatment is carried out for a period of time. It is presently believed that as long as the temperature is not too high, there is no clear upper limit for the period of time useful for heating, but that after a certain period of time, further heating time does not have a noticeable effect on the material.
  • the material is heated for a period of time of 15-600 minutes, such as for example from 15, 20, 25, 30, 45, 60, 90, 120, 150, 180, 210, 240, 270, 300, 330, 360, 390, 420, 450, 480, 510 or 540 minutes up to 30, 45, 60, 90, 120, 150, 180, 210, 240, 270, 300, 330, 360, 390, 420, 450, 480, 510, 540, 570 or 600 minutes.
  • 15-600 minutes such as for example from 15, 20, 25, 30, 45, 60, 90, 120, 150, 180, 210, 240, 270, 300, 330, 360, 390, 420, 450, 480, 510, 540, 570 or 600 minutes.
  • the temperature used for the heat treatment is 250-900 °C, such as for example from 250, 260, 270, 280, 290, 300, 310, 320, 330, 340, 350, 360, 370, 380, 390, 400, 420, 440, 460,
  • the heat treatment is carried out at a temperature of 400-600 °C, for example for 45-75 minutes. It is believed that this temperature range is especially suitable for increasing OSL intensity of at least certain materials according to formula (I). According to another embodiment, the heat treatment is carried out at a temperature of 400-700 °C, for example for 45-75 minutes. It is believed that this temperature range is especially suitable for decreasing the normal afterglow of at least certain materials according to formula (I). According to yet another embodiment, the upper temperature limit of the heat treatment is 850 °C.
  • the heat treatment is typically carried out in an oven.
  • the material may be either gradually heated together with the oven, or it may be placed from room temperature to a ready- heated oven.
  • the material may pass through a series of ovens, having increasing temperatures.
  • the temperature difference between two consecutive ovens may be 50 or 100 °C.
  • other types of devices can be used, such as chambers, furnaces etc.
  • the heat treatment is followed by cooling of the material in a step-wise manner.
  • the material may for example be allowed to cool together with the oven, meaning that the cooling is gradual, i.e. the steps are small.
  • the material may also be cooled by passing it through a series of ovens having decreasing temperatures. For example, the temperature difference between two consecutive ovens may be 50 or 100 °C.
  • the cooling may also be carried out by removing the material from the hot oven to room temperature.
  • the heat treatment is carried out in an atmosphere of air, nitrogen, argon, oxygen or mixtures thereof.
  • a reducing gas may also be used during the heat treatment.
  • the electron bombarded material or the electron bombarded and heat treated material is further arranged in a polymer matrix.
  • the thus obtained product is thereafter treated with ultraviolet (UV) irradiation.
  • UV ultraviolet
  • ultraviolet irradiation treatment can be used to further improve optical properties of the material of formula (I).
  • Ultraviolet irradiation treatment enables increasing luminescence and optically stimulated luminescence intensity in computed radiography (CR) imaging, in digital radiography (DR) imaging and computed tomography (CT) imaging.
  • the imaging techniques may use plates or detectors, or a combination of plates and detectors.
  • the detectors may be for example X-ray detectors.
  • the material of formula (I) is believed to require being arranged in a polymer matrix.
  • the polymer matrix acts as an energy converter that absorbs ultraviolet emission from the material, converts it to such wavelengths that can be read by CR plate reader and emits it to the reader.
  • ultraviolet treatment makes more of the optically stimulated luminescence of the material of formula (I) visible to the CR plate reader, i.e. converts especially the high-energy part of the optically stimulated luminescence into wavelengths that CR reader can see (blue light).
  • Ultraviolet radiation enhances the blue emission of the polymer by widening the excitation band of the polymer.
  • the CR image becomes brighter and/or higher in contrast.
  • ultraviolet irradiation treatment of the material arranged in polymer matrix results in increased optically stimulated luminescence signal. It has been noted that the ultraviolet treatment does not seem to affect the material as such, but only the polymer matrix, especially the surface of the polymer matrix.
  • the material can be arranged in a polymer matrix by using tape casting, also known as knife coating or doctor blading.
  • Tape casting is a process where a thin sheet of ceramic or metal particle suspension fluid is cast on a substrate.
  • the fluid may contain volatile nonaqueous solvents, a dispersant, (a) binder(s) and the dry matter, i.e. the material having formula (I).
  • the process may comprise preparing the suspension and applying it onto a surface of a substrate.
  • the binder may create a polymer network around the dry matter particles, while the plasticizer may function as a softening agent for the binder. When combining these substances, the tape may become resistant against cracking and flaking off when bent.
  • the dispersant may be used to de-aggregate the particles and homogenize the suspension.
  • the material is arranged in a polymer matrix by mixing the material with the tape casting components.
  • Any suitable and typical tape casting components can be used, as known in the art.
  • the tape casting components comprise ethanol Aa, ethyl methyl ketone, triton X-100, benzyl butyl phthalate and polyvinyl butyral.
  • the polymer matrix i.e. tape-casting polymer
  • the polymer matrix can comprise one or several different polymers. Any polymer capable to act as an energy converter, i.e. capable to be excited by the optically stimulated luminescence emission, can be used. According to one embodiment, the polymer can be benzyl butyl phthalate or polyvinyl butyral or any combination thereof.
  • the material, tape-casted in a polymer matrix, forms an image detector that can be used in computed radiography imaging after the beneficial UV treatment.
  • the ultraviolet irradiation is made using an irradiation with wavelength of 200 to 310 nm.
  • the exposure time for the UV irradiation is for example 10 seconds to 30 minutes.
  • the time can thus be for example from 10, 15, 30 or 45 seconds or from 1, 5, 10 or 20 minutes up to 15, 30 or 45 seconds or 1, 5, 10, 20, 25 or 30 minutes.
  • the ultraviolet irradiation intensity used is 4 to 6 mW/cm 2 .
  • ultraviolet irradiation treatment can be performed for example with wavelength of
  • the present materials may be used in X-ray imaging, in computed radiography (CR) imaging, in digital radiography (DR) imaging and in computed tomography (CT) imaging.
  • the imaging techniques may use plates or detectors, or a combination of plates and detectors.
  • the detectors may be for example X-ray detectors. These plates and detectors may comprise the present material that has been treated, or the plate or detector (also called in general image detectors) may first be formed and thereafter the material may be treated as discussed.
  • the material according to formula (I) may be attached to a surface for example as a coating or a film.
  • the substrate of the plate or detector may comprise or consist of glass or polymer.
  • the substrate may comprise or consist of a glass layer or a polymer layer.
  • the substrate may comprise (a) further layer(s).
  • the substrate may also or alternatively comprise an attachment layer, such as a printing paper, and/or a base layer, such as a cardboard layer, or any other layer(s) where desired or needed.
  • the image detector may comprise further layers and/or components.
  • the image detector has the added utility of enabling the use of the material represented by formula (I) as a detector material for imaging purposes.
  • the image detector has a further added utility of making use of an optically active material being non-toxic and non-expensive compared to currently used materials such as Ba(F,Cl,Br,I)2:Eu and CsITi.
  • the image detector has still an added utility of being reusable and recyclable. Further, the image detector can be used for point- of-care analysis without the need of complicated analysis systems.
  • the present description further relates to a device, wherein the device comprises a material according to one or more embodiments described in this specification.
  • the device is an ultraviolet radiation sensor, an ultraviolet radiation detector, or an ultraviolet radiation indicator.
  • the device is an X-radiation sensor, an X-radiation detector, an X-radiation indicator, or an X-radiation dose indicator.
  • the present method of electron bombardment of the material has the effect of decreasing afterglow of the present materials.
  • the present description thus relates also to a method for decreasing afterglow of a material represented by formula (I) as defined above, by carrying out the electron bombardment described above.
  • the decreased afterglow is afterglow of optically stimulated luminescence.
  • the optical stimulation being carried out with a laser. The effect is obtained especially when the material is both electron bombarded and heat treated.
  • a further effect of the present invention is the increase of intensity of optically stimulated luminescence.
  • the present description also relates to a method for increasing intensity of optically stimulated luminescence of a material represented by formula (I) as defined above, by carrying out the electron bombardment as described above. The effect is obtained especially when the material is both electron bombarded and heat treated.
  • a still further aspect of this description is a method for increasing contrast of a computed radiography plate, by using a material represented by formula (I) and treated with ultraviolet (UV) irradiation, as explained above.
  • Example 1 Preparation of the materials
  • the materials tested had the formula Li Na 7 Al 6 Si 6 O 24 (Br,S) 2 :Sr, with various amounts of Sr.
  • One sample also had some Cu.
  • the amounts of Sr (and Cu) are given below in Table 1.
  • zeolite A was first dried at 500 °C for 1 h. Stoichiometric amounts of zeolite A, NaBr, Na 2 SO 4 and LiBr were used as the starting materials. The dopants were added as bromides (SrBr 2 , CuBr when used). The following conditions were used: first heating was carried out at 800 °C in air for 5 hours, then a second heating at 850 °C under an atmosphere of 12 % H 2 and 88 % N2 for 2 hours. For the material MT84, the first heating was done for 5 hours in 850 °C, removed from the oven at 850 °C and thus cooled down quickly. The second heating was as above.
  • the material was electron bombarded as described below, and thereafter tested as also described below.
  • the MTxxa is the reference material that was not electron bombarded
  • the MTxxb etc. is the electron bombarded sample.
  • the temperature and pressure in the laboratory was kept at 20 °C and 1 atm. Approximately 30 mg of sample powder was spread as a thin surface onto a glass sample holder which was then put into the vacuum chamber Nuclide Corp. ELM2B connected to a Franklin Electric model 1102685400 vacuum pump providing continuous suction. The control unit Nuclide Corp. ELM2EX was then used to control the voltage and current levels for the electron bombardment. The voltage was kept at 5 kV and the current was kept at 1.0 mA for samples other than MT82 and MT83, the conditions for MT82 and MT83 being given below in Table 2. When the equipment's pressure reading was below 13 Pa, the electron beam was visible and could be visually adjusted with magnets that were held on both sides of the vacuum chamber's window.
  • the visible beam was kept oval shaped, measuring 7 mm x 30 mm. This area of the sample was bombarded for 30 min (other samples than MT82b and MT83), after which a new, unexposed area was bombarded for the same time until the whole surface of the sample surface had been exposed to a same current, voltage and time product.
  • the time of electron bombardment of each portion was as indicated in Table 1, while the voltage and current as well as the measured pressure are given below in Table 2.
  • the samples MT82a and MT82b had been heat treated before electron bombardment. Table 2
  • the mixture was then cast onto a polyester projector transparency, and subjected to UV irradiation at 20 °C and normal air pressure (1 atm).
  • a 302 nm handheld UVP model UVM-57, 6 W lamp was placed directly on top of the sample and switched on, exposing the sample to UV radiation for 5-30 min with an irradiance of 4.25 mW/cm ⁇ .
  • the photochromism of the material had faded, the enhanced glow of the polymer was visible under 302 nm and 365 nm UV light.
  • the material of formula Na 8 Al 6 Si 6 O 24 ( Cl,S) 2 was suspended in the same polymer matrix as in Example 3a and subjected to 254 nm UV irradiation from a handheld UVP model UVLS-24 EL, 4 W 254/365 nm lamp, also at 20 °C and normal air pressure (1 atm).
  • the lamp was placed directly on top of the sample and switched on, exposing the sample to UV radiation for between 10 seconds and 30 minutes with an irradiance of 5.92 mW/cm ⁇ .
  • the photochromism of the material had faded, the enhanced glow of the polymer was visible under 302 nm and 365 nm UV light.
  • Example 3a The tape-cast polymer as well as the polyester projector transparency of Example 3a (i.e. without any material according to formula (I)) were exposed to UV irradiation by the same
  • the samples MT82a and MT82b were heat treated as described below. The below explained heat-treatment was thus a third heating of the material, since the beginning of its manufacturing.
  • each material was placed into a small thermogravimetric analysis crucible.
  • Each sample was then heated in a Nabertherm N3/C8 muffle furnace at the default heating rate of approximately 20 °C/min up to a temperature of 600 °C in air at normal pressure (1 atm).
  • the sample was kept for 1 h at the desired temperature before being allowed to cool freely inside the furnace. Once the sample had cooled down, it was collected and its optically stimulated luminescence (OSL) was measured (as explained in more detail below).
  • OSL optically stimulated luminescence
  • MT82a is the reference material that was not heat-treated, while the MT82b is the heat-treated sample. After heat-treatment, the samples were submitted to electron bombardment as described above.
  • OSL intensity and afterglow were measured as follows. The temperature and pressure in the laboratory were kept at 20 °C and 1 atm. First, the sample powder was put into a glass capillary tube measuring 75 x 2.0 mm (Marienfeld no. 29 402 02). The sample was then irradiated with a Hg discharge lamp providing 254 nm emission and put at a distance where the irradiance was 0.12 mW/cm 2 . The sample tube was spun at a rate of 70 revolutions per second and is irradiated for 60 s while spinning.
  • the sample tube was then put into the middle of a measuring chamber with a 44.4 mm inner diameter and kept there for 12 hours (MT57, MT80, MT85, MT80, MT84 and MT85 in Figures 1, 2, 3, 6, 7 and 8, respectively), for 24 hours (MT83 in Figures 9 and 10) or for 5 hours (MT82 in Figure 11) to eliminate the initial afterglow.
  • the OSL intensity was measured by irradiating the sample with a 635 nm laser supplying 96 mA power output for 0.1 s.
  • One measurement set was an average of 100 measurements with 1.0 s scan time per measurement or an average of 10 measurements with 10.0 s scan time per measurement using a sampling step of 1 ms or 10 ms, respectively (10 measurements with 10.0 s scan time per measurement using 10 ms sampling step for MT57, MT80, MT85, MT80, MT84 and MT85 in Figures 1, 2, 3, 6, 7 and 8, respectively; 100 measurements with 1.0 s scan time per measurement using 1 ms sampling step for MT83 and MT82 in Figures 9, 10 and 11).
  • the adjustment of the laser beam was carried out with a 600 nm long wave pass filter, and the emission side consists of Thorlabs LA1951-B F25.4 mm lens, short wave pass filter 550 nm, short wave pass filter 600 nm, Thorlabs LA1951-B F25.4 mm lens, and finally a photomultiplier tube, respectively.
  • the photomultiplier tube was connected to a Stanford Research Systems SR570 low noise current preamplifier (parameters: bias voltage POS, filter type: none, input offset: 1 pA, gain mode: low noise, sensitivity: 50 nA/V; (20 nA/V used for non-treated and 50 nA/V for treated MT57, MT80, MT85, MT80, MT84 and MT85 in Figures 1, 2, 3, 6, 7 and 8, respectively; 50 nA/V used for MT83 and MT82 in Figures 9, 10 and 11) and to a Stanford Research Systems PS325 high voltage power supply unit.
  • the preamplifier was connected to ports 7 and 8 in a National Instruments NI USB-6251 multifunction I/O device.
  • a wire loop from ports 4 and 5 to ports 15 and 16 was connected in parallel to a Tektronic TDS 420 oscilloscope and a Newport laser diode driver model 5060.
  • the laser diode driver was connected to a Thorlabs LDM9LD laser diode, which was connected to a TE Technology TL-48-20 temperature control unit.
  • the temperature of the laser diode was kept at 18.0 °C and controlled with a Wentronic DF17132SB DL PSV laboratory power supply set to 2.8 V.
  • the normal afterglow was measured with a luminance spectrometer setup: the sample was irradiated for 5 minutes under 254 nm UV light with UVC irradiance of 3.4 mW/cm 2 hitting the sample, after which the afterglow measurement was started immediately with a Hagner Evacuation Route Photometer ERP-105 coupled to a Hagner SD 27 detector.
  • the signal coming from the instrument was converted to volts with a Fluke multimeter. FlukeView Forms PC application reads the value of the multimeter every second, and the value with a certain multiplication factor (depending on the sensitivity setting on the ERP-
  • Figures 1 to 3 illustrate the decrease of optically stimulated luminescence afterglow in electron bombarded material compared to non-treated material.
  • x-axis stands for “time/s”
  • y-axis stands for “normalized intensity”.
  • Solid line and dashed line describe electron bombarded material and non-treated material correspondingly.
  • the material tested was MT57 in Figure 1, MT80 in Figure 2 and MT85 in Figure 3. In these Figures, as the results are normalised, only the shape of the curve is significant.
  • Figures 4 and 5 illustrate the decrease of normal afterglow in electron bombarded material compared to non-treated material.
  • x-axis stands for “time” in seconds
  • y-axis stands for “luminance” in mcd/m .
  • the lower line represents the electron bombarded material
  • the upper line represents the non-treated material.
  • the material tested was MT55 in Figure 4 and MT57 in Figure 5.
  • Figures 6-8 illustrate the increase of intensity of optically stimulated luminescence in electron bombarded material.
  • the tested materials were MT80 in Figure 6, MT84 in Figure 7 and MT85 in Figure 8.
  • the Figures show the OSL intensity on the y-axis (in arbitrary units, a.u.) and time (in seconds) on the x-axis.
  • the upper curve is from the electron bombarded sample of MT80, while the lower was from the non-treated sample of the same MT80.
  • Figures 7 and 8 the same order of the curves was observed, although the results were closer to one another.
  • the sensitivity was set higher in the reference sample (i.e. non-treated sample), thus the intensity of the electron-bombarded sample was in fact even higher with respect to the non-treated sample, than what is immediately apparent from the Figures. The difference was about 2.5 fold.
  • Figures 9 and 10 illustrate the effect of the time of electron bombardment on the intensity of OSL of the material MT83.
  • Figures 9 and 10 are the same results, but Figure 10 shows the results stacked, for better visual assessment.
  • the scale on y-axis in Figure 10 is thus not representative, only the differences in the different lines.
  • the times of bombardment from top line towards the lowest line were 30 minutes, 20 minutes, 10 minutes, 5 minutes, 1 minute, 30 seconds and no bombardment.
  • the Figure clearly illustrates that for this particular material, the optimum electron bombardment time in order to increase the OSL intensity is 1-10 minutes.
  • the same graphs are shown in Figure 9, where the different lines are best distinguished from one another at times 0-0.1 seconds. The line that raises the highest is for the bombardment time 10 minutes, the second highest for 1 minute, the third highest for 5 minutes, thereafter 20 minutes, while the others are approximately the same.
  • Figure 11 illustrates the effect of electron bombardment and heat treatment on the intensity of optically stimulated luminescence according to an embodiment.
  • the sample was MT82, heat-treated and then electron bombarded as explained above.
  • Figure 11 also shows the results stacked, for better visual assessment.
  • the scale on y-axis in Figure 11 is thus not representative, only the differences in the different lines.
  • the upper line shows the result for the heat-treated but not electron bombarded sample MT82a, while the lower line is for the sample treated at 600 °C, followed by electron bombardment for 20 minutes (sample MT82b).
  • the increase in OSL intensity is clearly higher for the sample MT82b.
  • Figures 12 and 13 illustrate the effect of an UV radiation on CR image.
  • the material used in Figure 12 was MT55 (Example 3a) and in Figure 13, the material was MT57 (Example 3a).
  • the left-most picture is the plate prior to UV treatment.
  • the lower half of both plates was treated with one UV treatment (302 nm/20 min/4.25 mW/cm 2 ), whereas the upper half was left untreated.
  • X- rays 80 kV, 25 mA were used to produce the image.
  • the different pictures show the image of the plate after different amounts of X-ray exposures.
  • the second plate was exposed to X-rays ten times (total dose 101 mGy), the third plate 8 times (total dose 80 mGy), the fourth plate 5 times (total dose 50 mGy) and the fifth plate 1 time (total dose 10 mGy), when reading from left to right.
  • Figures 14 to 16 illustrate ultraviolet enhancement of polymer emission, i.e. without any material according to formula (I), obtained according to Example 3c.
  • the tape-cast polymer as explained above was used in Figures 14 and 15, while the polyester projector transparency was used in Figure 16.
  • unexposed and UV-treated tape- cast polymers were compared. All the Figures represent intensity (a.u., on the y-axis) as a function of wavelength (nm, on the x-axis). The measurements were an average of 10 measurements, with 1 second integration time. From Figure 14, it can be seen that the UV-treated polymer, which is the upper curve between wavelengths of about 450-485 nm, thus has a more intense blue emission.
  • Figure 15 shows the excitation spectra for blue emission for unexposed (marked with squares) and UV-treated polymer (marked with spheres), wherein it can be seen that the UV-treated polymer has a broader excitation band, which is thought to be the reason for brighter blue emission.
  • Figure 16 shows emission spectra of unexposed and UV-treated polyester transparency. From the Figure it can be seen that two different emission bands of this polymer (420 nm and 480 nm) are both enhanced by UV treatment.

Abstract

La présente invention concerne un procédé de traitement d'un matériau représenté par (M')8(M''M''')6O24(X,X')2:M'''', par bombardement d'électrons dans une chambre à vide ayant une pression permettant la formation d'un faisceau d'électrons. De plus, l'invention concerne un procédé permettant d'augmenter l'intensité de la luminescence simulée optiquement d'un tel matériau, ainsi qu'un procédé pour réduire la post-luminescence d'un tel matériau. En outre, la présente invention concerne un procédé permettant d'augmenter le contraste d'une image sélectionnée à partir d'une radiographie calculée, d'une tomodensitométrie et d'une radiographie numérique.
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Citations (3)

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WO2017194825A1 (fr) 2016-05-09 2017-11-16 Turun Yliopisto Matériau luminescent
WO2019092309A1 (fr) 2017-11-07 2019-05-16 Turun Yliopisto Indication de l'intensité d'un type prédéterminé de rayonnement
WO2019092308A1 (fr) 2017-11-07 2019-05-16 Turun Yliopisto Détermination de la quantité d'un type de rayonnement prédéfini irradié sur un matériau de capteur

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WO2019092309A1 (fr) 2017-11-07 2019-05-16 Turun Yliopisto Indication de l'intensité d'un type prédéterminé de rayonnement
WO2019092308A1 (fr) 2017-11-07 2019-05-16 Turun Yliopisto Détermination de la quantité d'un type de rayonnement prédéfini irradié sur un matériau de capteur

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