WO2015118533A1 - Procédés de fabrication de scintillateurs tridimensionnels - Google Patents

Procédés de fabrication de scintillateurs tridimensionnels Download PDF

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Publication number
WO2015118533A1
WO2015118533A1 PCT/IL2015/050127 IL2015050127W WO2015118533A1 WO 2015118533 A1 WO2015118533 A1 WO 2015118533A1 IL 2015050127 W IL2015050127 W IL 2015050127W WO 2015118533 A1 WO2015118533 A1 WO 2015118533A1
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Prior art keywords
process according
scintillator
polymer
pattern
scintillators
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PCT/IL2015/050127
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English (en)
Inventor
Guy RON
Shlomo Magdassi
Ido COOPERSTEIN
Michael Layani
Yonatan MISHNAYOT
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Yissum Research Development Company Of The Hebrew University Of Jerusalem Ltd
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Publication of WO2015118533A1 publication Critical patent/WO2015118533A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/16—Measuring radiation intensity
    • G01T1/20—Measuring radiation intensity with scintillation detectors
    • G01T1/203—Measuring radiation intensity with scintillation detectors the detector being made of plastics
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/16—Measuring radiation intensity
    • G01T1/20—Measuring radiation intensity with scintillation detectors
    • G01T1/203—Measuring radiation intensity with scintillation detectors the detector being made of plastics
    • G01T1/2033—Selection of materials

Definitions

  • the invention generally contemplates methods for fabricating three-dimensional scintillating materials and objects and uses thereof.
  • Scintillating materials which emit light when a charged particle traverses through the material, are commonly used in many applications requiring particle detection, from particle and nuclear physics experiments, through medial applications, and homeland security applications and in the detection of sensitive and suspicious materials.
  • These scintillators are manufactured either by casting resins into pre-formed molds, or by machining (subtractive manufacturing) of large, extruded, scintillator blocks. Both of these techniques suffer from the inability to provide precise, small scale geometries, as well as from the relatively high cost and long lead-time.
  • Scintillators are typically made by either casting of a resin and a hardener combination, or by extrusion of a molten scintillator [1]. These cast or extruded scintillator bars are then machined to the required geometry using standard machining techniques.
  • the invention disclosed herein provides methods and techniques for three- dimensional printing of scintillating materials.
  • the methods of the invention may be carried out employing commercial 3D-printing materials, as base materials, to which selective and specific functional materials may be added to optimize the scintillation and optical properties of the printed materials; thus forming "Functional Scintillators" tailored for a specific application, as detection of radiation sources such as neutron, or gamma-ray radiations.
  • use of organic scintillators such as anthracene, stilbene and naphthalene has been determined ineffective or difficult as such materials cannot be easily machined, nor can they be grown in large sizes. Therefore, such materials, despite their unique properties, have not been often used.
  • fluors such as p-terphenyl, 2-(4-Biphenylyl)-5-phenyl- 1,3,4- oxadiazole (PBD), 2-(4-tert-Butylphenyl)-5-(4-phenylphenyl)-l,3,4-oxadiazole (butyl PBD), 2,5-diphenyloxazole (PPO) and wavelength shifter such as 5-Phenyl-2-[4-(5- phenyl-l,3-oxazol-2-yl)phenyl]-l,3-oxazole (POPOP) could not be typically used where UV-mediated polymerization reactions were involved due to their competitive light absorption.
  • the ability to incorporate different compounds into the polymer matrix is of great importance, since it may be used to introduce dopants that exhibit a strong neutron absorption cross section (for example 6 Li and 10 B), which allow printing of scintillators with increased efficiency for the detection of fissionable materials.
  • dopants that exhibit a strong neutron absorption cross section (for example 6 Li and 10 B), which allow printing of scintillators with increased efficiency for the detection of fissionable materials.
  • the invention overcomes the above hurdles by providing a printing method for directly manufacture scintillator designs that cannot be achieved using standard approaches (e.g., hollow, gas filled scintillators, or scintillator designs with features which are too small to be machined).
  • the 3D printing of the invention allows integrating in the scintillator material, during the printing process, additives and dopants with a desired activity, ranging from wavelength shifting, dopants with enhanced reactivity to various radiation types and nanoparticles.
  • the methods of the invention permit design modalities which are currently unavailable in the printing of such materials and objects, thereby significantly reducing difficulties associated with manufacture of such scintillating materials, decrease development time and associated costs.
  • the invention provides an ink formulation suitable for printing or otherwise forming the 3D-scintilators of the invention.
  • the ink formulation typically comprises a scintillator, a material which absorbs a radiation, such as gamma-ray or X- ray, and emits an electromagnetic wave with a wavelength of visible light or near visible light, a primary phosphor, e.g., an organic phosphor for absorbing energy from the scintillator material, and optionally a further phosphor, which too may be an organic phosphor to shift the wavelength of the photons received from the primary phosphor to photons which more closely match that detected by a photo multiplier.
  • a primary phosphor e.g., an organic phosphor for absorbing energy from the scintillator material
  • a further phosphor which too may be an organic phosphor to shift the wavelength of the photons received from the primary phosphor to photons which more closely match that detected by a photo multiplier.
  • the ink formulation comprises a polymerizable pre -polymer material, monomers or oligomers, which acts as a matrix for the scintillator material or as the scintillator material itself, and one or more phosphor materials such as 2,5-diphenyloxazole (PPO) which emits at 360-380 nm, 1,3,5- triphenyl-2-pyrazoline (TPP) which emits at 410 nm and l,4-bis(4-methyl-5- phenyloxazol-2-yl)benzene dimethyl (POPOP) which emits at 427 nm.
  • PPO 2,5-diphenyloxazole
  • TPP 1,3,5- triphenyl-2-pyrazoline
  • POPOP 1,3,5- triphenyl-2-pyrazoline
  • one of the phosphor materials may be used as the primary phosphor, e.g., PPO, to accept energy from the scintillator material, e.g., an aromatic material, and a further or secondary scintillator, also known as a wavelength shifter, such as POPOP, to shift the wavelength of the photons, as explained herein.
  • PPO primary phosphor
  • a further or secondary scintillator also known as a wavelength shifter, such as POPOP, to shift the wavelength of the photons, as explained herein.
  • the ink formulation may further comprise a photoinitiator.
  • a (bottom up) process for fabricating a three-dimensional scintillator material comprising:
  • a scintillator formulation comprising at least one pre-polymer e.g., monomers polymerizable into a desired polymer and at least one photoinitiator
  • the scintillator formulation comprises:
  • the scintillator formulation comprises at least one pre-polymer e.g., monomers, polymerizable into a desired polymer, e.g., an aromatic polymer (polymer containing aromatic rings), at least one photoinitiator and one or more phosphors.
  • the phosphors are selected amongst primary and secondary phosphors, wherein the primary phosphor e.g., an organic phosphor, is capable of absorbing energy from the scintillator material, and wherein the secondary phosphor, which may be an organic phosphor as well is selected as a wavelength shifter capable of shifting the wavelength of the photons received from the primary phosphor to photons which match that detected by a photo multiplier.
  • the primary phosphor e.g., an organic phosphor
  • the secondary phosphor which may be an organic phosphor as well is selected as a wavelength shifter capable of shifting the wavelength of the photons received from the primary phosphor to photons which match that detected by a photo multiplier.
  • the term " cintillator” or any lingual variation thereof refers to a material which has the ability to emit light when excited by ionizing radiation and/or incoming charged particle, or which has the ability to shift the wavelength of the light.
  • the materials which are used for fabricating the 3D-scintilator may be selected amongst plastic scintillators, organic scintillators, inorganic scintillators, ceramic scintillators, liquid scintillators, base scintillators and glass scintillators, in which wavelength shifting dopants as well as other functional additives may be embedded.
  • the polymerizable pre-polymers are typically said to adapt scintillation properties, namely become scintillator materials, as defined herein, or to adapt no scintillation properties once polymerized.
  • the expression "adapt scintillation properties” refers to a polymer formed from pre-polymers, e.g., monomers and/or oligomers, and which presents scintillator characteristics (has the ability to emit light when excited by ionizing radiation and/or incoming charged particle, or which has the ability to shift the wavelength of the light) when formed, irrespective of the scintillating properties of the pre-polymers.
  • a polymer said "not to adapt scintillation properties” is one which is incapable of emiting light when excited by ionizing radiation and/or incoming charged particle, or which has the ability to shift the wavelength of the light.
  • the scintillator material may be comprised of a single scintillation material or may be in the form of a composition comprising a carrier, which by itself does not exhibit scintillation, and at least one agent which renders the composition scintillating, or the carrier itself has a scintillation property or combinations thereof.
  • a carrier which by itself does not exhibit scintillation
  • at least one agent which renders the composition scintillating, or the carrier itself has a scintillation property or combinations thereof.
  • any of the scintillator materials recited herein may be used by themselves or in combination with at least a carrier or any one or more additive, as further disclosed herein below.
  • Scintillators may be selected from: (a) polyethylene naphthalate, polyvinyl naphthalene, polymethylmethacrylate (PMMA), polyvinyl xylene (PVX), polymethyl styrenes, 2,4-dimethyl styrene, 2,4,5- trimethyl styrene, polyvinyl diphenyl, ethoxylated trimethylolpropanetriacrylate (ethoxylated TMPTA), ethoxylated bisphenol A diacrylate, polyvinyl tetrahydronaphthalene ;
  • aromatic hydrocarbons such as anthracene (CMHJO), stilbene (C 1 4H 1 2), naphthalene (CioH 8 ), polyvinyltoluene (PVT);
  • organometallic compounds such as triphenylbismuth
  • alkali metal halides such as Nal(Tl) (sodium iodide doped with thallium);
  • inorganic alkali halides such as CsI(Na), Csl(pure), CsF, KI(T1), Lil(Eu);
  • non-alkali materials such as BaF 2 , CaF 2 (Eu), ZnS(Ag), CaW0 4 , CdW0 4 , YAG(Ce) (Y 3 Al 5 0 12 (Ce)), GSO, LSO;
  • inorganic scintillators such as LaCl 3 (Ce), LaBr 3 (Ce);
  • polyphenyl hydrocarbons such as oxazole and oxadiazole aryls, n-terphenyl (PPP), 2,5-diphenyloxazole (PPO), l,4-di-(5-phenyl-2-oxazolyl)-benzene (POPOP), 2- phenyl-5 -(4-biphenylyl) - 1 , 3 ,4-oxadiazole (PB D) , 1,3,3 -Trimethyl- 1 -phenylindan (TMPI) and 2-(4'-tert-butylphenyl)-5-(4"-biphenylyl)-l,3,4-oxadiazole (B-PBD);
  • PPP polyphenyl hydrocarbons
  • PPO 2,5-diphenyloxazole
  • POPOP l,4-di-(5-phenyl-2-oxazolyl)-benzene
  • PB D 1,3,3 -Trimethyl- 1
  • tungstate and gadolinium based materials such as radmium tungstate or terbium-doped gadolinium oxysulphide (Gd 2 (3 ⁇ 4S), cadmium tungstate (CdWC>4 or CWO), terbium activated gadolinium and calcium tungstate (CaWO/ t );
  • (k) ceramic scintillators such as (Y,Gd)2(3 ⁇ 4:Eu,Pr; Gd 2 (3 ⁇ 4S:Pr,Ce,F; and Gd 3 Ga 5 0 12 :Cr,Ce;
  • the scintillator formulation comprises primary and secondary phosphors, each independently being selected from polyphenyl hydrocarbons.
  • the polyphenyl hydrocarbons are selected from s oxazole and oxadiazole aryls, n-terphenyl (PPP), 2,5-diphenyloxazole (PPO), l,4-di-(5- phenyl-2-oxazolyl)-benzene (POPOP), 2-phenyl-5-(4-biphenylyl)-l,3,4-oxadiazole (PBD), 1,3,3-Trimethyl-l-phenylindan (TMPI) and 2-(4'-tert-butylphenyl)-5-(4"- biphenylyl)-l,3,4-oxadiazole (B-PBD).
  • the primary and secondary phosphors are selected from PPO and POPOP.
  • the primary and secondary phosphors are TMPI.
  • the scintillator formulation comprises a resin material of an aromatic polymer (a polymer containing at least one aromatic or aryl group), such polymers may be selected from polyethylene naphthalate, polyvinyl xylene (PVX), polymethyl styrenes, 2,4-dimethyl styrene, 2,4,5-trimethyl styrene, polyvinyl diphenyl, polyvinyl naphthalene, ethoxylated bisphenol A diacrylate, bisphenol A, polyvinyl tetrahydronaphthalene.
  • the resin material is of bisphenol A acrylate, e.g., ethoxylated bisphenol A diacrylate or dimethylacrylate.
  • the phosphor materials are selected from aromatic hydrocarbons such as anthracene (C 1 4H 10 ), stilbene (C 1 4H 1 2), naphthalene (CioHg) and polyvinyltoluene (PVT).
  • aromatic hydrocarbons such as anthracene (C 1 4H 10 ), stilbene (C 1 4H 1 2), naphthalene (CioHg) and polyvinyltoluene (PVT).
  • the phosphor materials are selected from polyphenyl hydrocarbons such as oxazole and oxadiazole aryls, n-terphenyl (PPP), 2,5- diphenyloxazole (PPO), l ,4-di-(5-phenyl-2-oxazolyl)-benzene (POPOP), 2-phenyl-5-(4- biphenylyl)-l ,3,4-oxadiazole (PBD), 1 ,3,3-Trimethyl-l-phenylindan (TMPI) and 2-(4'- tert-butylphenyl)-5-(4"-biphenylyl)-l ,3,4-oxadiazole (B-PBD).
  • polyphenyl hydrocarbons such as oxazole and oxadiazole aryls, n-terphenyl (PPP), 2,5- diphenyloxazole (PPO), l ,4-di-(5-pheny
  • the phosphor materials are selected from TMPI, p- terphenyl, PBD, butyl PBD, PPO and POPOP.
  • the scintillator formulation for forming a 3D-scintillator according to the invention is selected from
  • the scintillators are made of a resin material and a hardener or crosslinker, or polystyrene based materials.
  • a pre -polymer material is used as a carrier to the scintillator, or where the scintillator is composed of a pre- polymer material such as monomers and/or oligomers
  • the polymerization of the monomers and/or oligomers may be initiated by the use of at least one polymerization initiator which may be comprised and patterned with the scintillating material and optionally the carrier.
  • the initiator is a photoinitiator such as 2,4,6-Trimethylbenzoyl-diphenyl-phosphineoxide (TPO).
  • the scintillator materials fabricated according to the invention may be used in a variety of applications, and thus in order to render the materials suitable for various applications, the materials may be doped or treated with suitable wavelength shifting materials and functional scintillators.
  • the amount of the materials, as dopants, which may be introduced varies based on the final intended application, inter alia, on the type of material, the type of dopant material, the effect to be achieved, the strength of the effect, the end application, presence or absence of other materials and others.
  • the concentration of material in the scintillator material is at most 10% w/w. In some embodiments, the concentration of the material is at least 0.5%. In some embodiments, the concentration of the material is between at least 0.5% and 10%. In some embodiments, the concentration of the material is between at least 0.5% and 20%. In some embodiments, the concentration of the material is between at least 0.5% and 30%. In some embodiments, the concentration of the material is between at least 0.5% and 40%. In some embodiments, the concentration of the material is between at least 0.5% and 50%. In some embodiments, the concentration of the material is between at least 0.5% and 9%, 8%, 7%, 6%, 5%, 4%, 3%, 2% or 1%. In some embodiments, the concentration of the material is between at least 0.5% and 1%.
  • the wavelength shifter are selected amongst optically active materials, e.g., nano- or micro-particles which are active at any wavelength ranging from the near UV through the visible wavelengths and up to the near IR spectrum. Such may be selected from charged particles (which traverse the scintillator and excite the material, thereby causing the material to emit light upon recombination, organic or inorganic materials or in combination thereof.
  • optically active materials e.g., nano- or micro-particles which are active at any wavelength ranging from the near UV through the visible wavelengths and up to the near IR spectrum.
  • Such may be selected from charged particles (which traverse the scintillator and excite the material, thereby causing the material to emit light upon recombination, organic or inorganic materials or in combination thereof.
  • the scintillator material is the carrier itself.
  • the carrier may comprise of a pre-polymer material (monomers and oligomers) which contains functional groups that emit light when excited by ionizing radiation and/or incoming charged particle.
  • the carrier can contain also other dopants.
  • the dopants are semiconductor materials capable of shifting wavelength from short wavelengths to longer wavelengths.
  • the materials are selected amongst core/shell semiconductor nanocrystals such as CdSe/ZnSe, CdSe/CdS, CdSe/ZnS and InP/ZnS.
  • oxides having absorbance in UV and IR may be used. Such oxides may be selected from Si(3 ⁇ 4, Ti0 2 , ZnO and AI2O3.
  • nanoparticles such as Ag, Au, Al, Fe, Cu, and others may be utilized, each based on its characteristic absorbance (e.g., Au - 550 nm, Al - 700-800 nm, Ag - 400 nm).
  • nanoparticles may be embedded in the scintillator using chemical binding.
  • the nanoparticles may be embedded by forming covalent or hydrogen bonds with the material or by physical interactions within the material matrix.
  • the nanoparticles may be pre -coated with relevant surface ligands and linkers which assist their association with the scintillator material.
  • the "nanoparticles" which may be embedded in the scintillator material may be any type of nanoparticle, of a material or shape known in the art.
  • the nanoparticles typically have at least one dimension, such as length, width, height, and diameter, below 1,000 nm. In some embodiments, the nanoparticles have at least one dimension which is less than about 100 nm. In some embodiments, the nanoparticles have at least one dimension which is between about 10 nm and 300 nm.
  • the nanoparticles employed in accordance with the invention may have any shape and symmetry, and may display branched or net structures. Without being limited thereto, the nanoparticles may be symmetrical or unsymmetrical, may be elongated having rod-like shape, round (spherical), elliptical, pyramidal, disk-like, branch, network or have any irregular shape. It should be emphasized that for the purposes of products and application according to the invention, the term "particle" by no means suggests any one particular pre-defined shape.
  • the nanoparticles may be of a single material or a combination of at least one material(s).
  • the material may be a metal, a metal oxide, a metal alloy, an insulator, a semiconductor material or any combination thereof.
  • the nanoparticles are optically active at any wavelength ranging from the UV through the visible wavelengths and up to the near IR spectrum.
  • the nanoparticles may be defined by having a plurality of material regions which are defined by continuous segments of differing chemical compositions.
  • the regions may be confined by a region of a different material, e.g., a metallic region confined by a different metal/metal alloy regions, or may be at a terminal region defining the ends of the nanoparticles.
  • the nanoparticle may similarly have the form of a continuous surface of one material, having thereon spaced apart regions (islands) of at least one other, e.g., metal/metal alloy material.
  • the nanoparticles may preferably be selected amongst non-spherical nanoparticles, e.g., nanorods, having at least one elongated region and one or more end regions of the same or different material.
  • the nanoparticles may also be selected based on their optical or electronic properties.
  • the nanoparticles may be selected to have an absorption onset in the visible, the visible and the near infrared range or even at deeper infrared then 3 ⁇ (micron), or to have the ability to (also or only) absorb in the UV range.
  • the nanoparticles may, for example, be selected to actively transform the wavelength or to change one or more optical property associated with a product of the invention.
  • the presence of silicon particles in a product of the invention allows light absorption at the UV and emission at the blue-green, to thereby increase protection from UV irradiation and to enhance efficiency.
  • the nanoparticles are quantum dots (QD).
  • heavy metals such as europium and terbium are embedded in the scintillator material.
  • the dopants used in a scintillator material according to the invention may be selected to provide an enhancement of a specific feature of the scintillators response.
  • “Functional Scintillators” as described herein are scintillators that are tailored to provide an enhancement of a specific feature of the scintillators response.
  • Such scintillating materials may be doped with, e.g., 10 B.
  • Boron is known to have an unusually large cross section for the ( ⁇ , ⁇ ) reaction for the efficient detection of neutrons emitted from fissionable materials.
  • 10 B in powder form may be easily mixed into the base resin, together with the required scintillation dopants, to allow for printing of such scintillators.
  • Also contemplated for neutron detection are 6 Li-based materials.
  • PPGNAA Prompt Gamma-Ray Neutron Activation Analysis
  • the formulation for forming a scintillator according to the invention may be utilized in three-dimensional printing, which comprises:
  • each of said one or more patterns may or may not be of the same shape and size, and may or may not have the same contour as a previous pattern, to obtain a three- dimensional pattern.
  • process step (c) is repeated several times to obtain a three-dimensional pattern or object which may be detached from the substrate on which it has been prepared and utilized in a process of scintillation.
  • the patterning steps are repeated more than twice. In other embodiments, the patterning steps are repeated between 2 and several thousand times. In other embodiments, the patterning steps are repeated between 2 and several hundred times. In other embodiments, the patterning steps are repeated between 2 and 50,000 times. In other embodiments, the patterning steps are repeated between 2 and 50,000 times.
  • the patterning steps are repeated between 2 and 40,000 times. In other embodiments, the patterning steps are repeated between 2 and 30,000 times. In other embodiments, the patterning steps are repeated between 2 and 20,000 times. In other embodiments, the patterning steps are repeated between 2 and 10,000 times. In other embodiments, the patterning steps are repeated between 2 and 5,000 times. In other embodiments, the patterning steps are repeated between 2 and 4,000 times. In other embodiments, the patterning steps are repeated between 2 and 3,000 times. In other embodiments, the patterning steps are repeated between 2 and 2,000 times. In other embodiments, the patterning steps are repeated between 2 and 1,000 times. In other embodiments, the patterning steps are repeated between 2 and 900 times.
  • the patterning steps are repeated between 2 and 800 times. In other embodiments, the patterning steps are repeated between 2 and 700 times. In other embodiments, the patterning steps are repeated between 2 and 600 times. In other embodiments, the patterning steps are repeated between 2 and 500 times. In other embodiments, the patterning steps are repeated between 2 and 400 times. In other embodiments, the patterning steps are repeated between 2 and 300 times. In other embodiments, the patterning steps are repeated between 2 and 200 times. In other embodiments, the patterning steps are repeated between 2 and 100 times. In other embodiments, the patterning steps are repeated between 2 and 90 times. In other embodiments, the patterning steps are repeated between 2 and 80 times. In other embodiments, the patterning steps are repeated between 2 and 70 times.
  • the patterning steps are repeated between 2 and 60 times. In other embodiments, the patterning steps are repeated between 2 and 50 times. In other embodiments, the patterning steps are repeated between 2 and 40 times. In other embodiments, the patterning steps are repeated between 2 and 30 times. In other embodiments, the patterning steps are repeated between 2 and 20 times. In other embodiments, the patterning steps are repeated between 2 and 10 times.
  • the patterning steps are repeated between 10 and 90 times. In other embodiments, the patterning steps are repeated between 20 and 90 times. In other embodiments, the patterning steps are repeated between 30 and 90 times. In other embodiments, the patterning steps are repeated between 40 and 90 times. In other embodiments, the patterning steps are repeated between 50 and 90 times. In other embodiments, the patterning steps are repeated between 60 and 90 times. In other embodiments, the patterning steps are repeated between 70 and 90 times. In other embodiments, the patterning steps are repeated between 80 and 90 times.
  • the process of the invention may comprise a step of forming a pattern of a carrier material or of a first formulation of a scintillator material, followed by forming a further or subsequent pattern thereof with a scintillator material or a different scintillator material.
  • the process of the invention may comprise the following:
  • step (c) repeating steps (a) and (b); or repeating step (a); or repeating step (b) one or more times to obtain a three-dimensional pattern.
  • the process comprising:
  • step (c) repeating steps (a) and (b); or repeating step (a); or repeating step (b) one or more times to obtain a three-dimensional pattern.
  • each scintillator may be selected, independently to have a structural or functional parameter selected from size, shape, composition, scintillator material, scintillation capacity, and others.
  • the process further comprises a step of treating the pattern or object fabricated under conditions selected from aqueous or organic washing, UV radiation, thermal treatment, polymerization, photopolymerization, laser sintering and others as may be known in the art.
  • the 3D-pattern or object may be fabricated by any printing process known in the art.
  • printing technologies may include, ink-jet printing, digital light processing (DLP) and Fused Deposition Modeling (FDM via extrusion), and 3D powder printing.
  • the printing is achieved by ink-jet printing.
  • ink-jet printing refers to a non-impact method for producing a pattern by the deposition of ink droplets in a pixel-by-pixel manner onto the substrate.
  • the ink-jet technology may be any ink-jet technology known in the art, including thermal ink-jet printing, piezoelectric ink-jet printing and continuous ink-jet printing.
  • the printing method is FDM, wherein 3D printing is performed by the extrusion of a plastic filament through a thin nozzle, and constructing the pattern geometry layer by layer.
  • the technique relies on printing using pre-existing plastic and/or any scintillator material, doped or un-doped, in fiber form or in any other geometry, as a printing medium.
  • Photopolymerization (PP) approaches using UV light may be utilized to selectively polymerize a liquid, either inside a resin bath, or in a printed or sprayed layer, similar to the method used in inkjet printers.
  • 3D Powder printing relates to placing a layer of powder material onto which a liquid binder is printed.
  • the scintillator can be made by printing a binder on powder of the scintillator material, thus forming a 3D scintillator.
  • the printed binder itself contains the scintillation formulation.
  • three-dimensional scintillating materials in a form selected from hollow structures, net-like structures, wires, cone-like structures, cylindrical structures, porous structures, branched structures, gas filled structures, and scintillator designs with features with are too small to be machined or produced by methods of the art.
  • Fig. 1 shows the absorption (solid) and emission (dashed) spectra for both PPO (black) and POPOP (gray), note the overlap of the PPO emission with the POPOP absorption.
  • Figs. 2A-2B provide: Fig. 2A- a typical spectrum of a reference sample (EJ-204, sample 8 in Table 1), and one of the printed samples of the invention.
  • Fig. 2B- The printed sample achieved -30% efficiency as compared to a commercial scintillator material, proving the viability of the technique of the invention.
  • Fig. 3 shows a printed design according to the invention; note the mesh and the threaded top of the cylinder, which are almost impossible to create in a scintillator using standard production techniques.
  • Fig. 4 demonstrates the efficiency measured for the different samples listed in Table I, compared to a commercial scintillator (EJ-204, sample 8 in Table 1).
  • Scintillating materials are commonly used in charged particle detectors as detector elements due to their ease of manufacture, relatively low cost, and good timing resolution.
  • the most common type of scintillator is the plastic scintillator, in which wavelength shifting dopants are embedded in a polystyrene matrix.
  • PPO 2,5-diphenyloxazole
  • PPO 2,5-diphenyloxazole
  • a second wavelength shifting dopant typically l,4-di-(5-phenyl-2-oxazolyl)-benzene (POPOP), with an emission wavelength peak at 410 nm is used to further shift the emitted light to the visible range, while keeping the wavelength short enough to be effectively detected by the detection element (usually a photocathode).
  • POPOP l,4-di-(5-phenyl-2-oxazolyl)-benzene
  • the invention describes several technologies including laser sintering, Fused Deposition Modeling (FDM via extrusion), 3D powder printing and photopolymerization (PP).
  • FDM 3D printing may be performed by the extrusion of a plastic filament through a thin nozzle, constructing geometry layer by layer.
  • PP approaches use UV light to selectively polymerize a liquid, either inside a resin bath, or in a sprayed and/or patterned layer, similar to the method used in inkjet printers is herein described.
  • the invention discloses both FDM and PP printing to allow direct printing of scintillator materials.
  • FDM allows printing unclad scintillating fibers as the filament for the printing, while in the PP approach the doping of the base resin used in the printing with various wavelength shifting compounds.
  • the doped sample has shown significant florescence under UV exposure, indicating that the dopant may be incorporated into the polymer matrix. Additionally, the doped sample has shown increased response to a radioactive source (i.e. scintillation).
  • a radioactive source i.e. scintillation
  • the invention further provides a method for the manufacture of scintillator materials in the form of plastic filaments
  • a formulation which is UV- polymerizable, e.g., based on acrylic monomers, doped with different fractions of scintillating and wavelength shifting materials.
  • the scintillator materials may be printed from ink formulations comprising, for example:
  • Fig. 1 shows the absorption (solid) and emission (dashed) spectra for both PPO (black) and POPOP (gray), note the overlap of the PPO emission with the POPOP absorption.
  • Curable formulations were composed of 99.5 wt. % SR9035 (Sartomer, Arkema) as the monomer and 0.5 wt. % Lucirin TPO (BASF) as the photoinitiator.
  • the formulations were generally stirred (in some embodiments for a period of 30 min in a water bath at 60°C) until all components were added.
  • the formulations were treated with the scintillator components: PPO, POPOP and naphthalene, at various concentrations (see Table I).
  • the final formulations were further stirred for 1 h in a water bath at 60°C.
  • the formulations were printed into a pattern and polymerized into the required shape (a cylinder 6.3mm in height and 20mm diameter) using an Asiga Pico Plus 39 printer (Asiga, Australia). Two different layer thicknesses were tested, 25 ⁇ and 127 ⁇ , in order to test the effect of the interface between printed layers on the light collection efficiency. The printed output was compared to reference samples of clear PMMA (plexiglas) and EJ-204 scintillator (Eljen Ltd.) of the same dimensions.
  • Fig. 3 shows a printed design according to the invention; note the mesh and the threaded top of the cylinder, which are almost impossible to create in a scintillator using standard production techniques. FDM Printing of Scintillators
  • Methods of the invention as herein described utilized the Fused Deposition Modeling techniques for scintillator printing by using exiting scintillator plastics, in fiber form, as a printing medium.
  • the potential benefit of this technique is in that these fibers constructed from material, which is known to operate in the desired manner, the invention focuses on the ability to accurately print and utilize the available material.
  • the invention further describes the operating parameters (temperature, speed, etc.) changes required in the 3D printer that will allow for printing of these materials (since, for example, the softening/melting points of scintillators are widely different from those of ABS plastic). Further, using two different materials in the printing, where the second material is either an opaque plastic such as ABS (for segmentation of the final product) or a wavelength-shifting plastic (used as part of common detector configurations and typically glued in specially made grooves) is herein described.
  • the FDM material filament can be made by solution casting or extrusion as known in the plastic industry compounding processes.
  • various dopants and concentrations may be used in order to optimize the scintillation and light collection properties of the resin used in PP printers.
  • the use may involve various monomers and resins, provided by several companies, and dope them with varying concentrations of PPO and secondary wavelength shifters.
  • PPO and secondary wavelength shifters As the photopolymers strongly absorb in the UV and short visible wavelength, care must be taken to shift as much of the available light into the visible range, where absorption is less of a problem.
  • Suitable resin (monomers/oligomers/polymers-dopant combinations may be photopolymerized and each sample characterized for its optical and scintillation properties.
  • Quantum dots may also be used in order to tailor the emission wavelength to match both the optical properties of the polymer base and the quantum efficiency of typical detector, such as Photo Multplier Tubes.
  • the 3D fabrication can take place by various technologies in which exposure to radiation (UV, IR etc.) leads to localized polymerization.
  • exposure to radiation UV, IR etc.
  • DLP inkjet- UV and laser curing.
  • Scintillators doped with a 10 B may be utilized in a variety of applications. Boron is known to have an unusually large cross section for the ( ⁇ , ⁇ ) reaction [Boron Cite], making it a good dopant. 10 B in powder form may be easily mixed into the base resin, together with the required scintillation dopants, to allow for printing of such scintillators.
  • PGP photon interaction cross sections
  • PPGNAA Prompt Gamma-Ray Neutron Activation Analysis
  • Such measurements are also performed in the detection of explosive compounds (nitrogen content) in many airports and docks.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Molecular Biology (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Luminescent Compositions (AREA)
  • Measurement Of Radiation (AREA)

Abstract

Les procédés de l'invention rendent possibles des modalités de conception qui ne sont pas disponibles actuellement dans l'impression d'objets et de matériaux scintillants, ce qui permet de réduire considérablement les difficultés liées à la fabrication de matériaux scintillants et de diminuer le temps de développement et les coûts associés.
PCT/IL2015/050127 2014-02-04 2015-02-04 Procédés de fabrication de scintillateurs tridimensionnels WO2015118533A1 (fr)

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FR3075977A1 (fr) * 2017-12-24 2019-06-28 Commissariat A L'energie Atomique Et Aux Energies Alternatives Dispositif scintillateur plastique avec piece comprenant un materiau hybride scintillant, procede de fabrication et de mesure associes et appareillage.
FR3075805A1 (fr) * 2017-12-24 2019-06-28 Commissariat A L'energie Atomique Et Aux Energies Alternatives Materiau hybride scintillant et son procede de fabrication.
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