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CN-122017926-A - Manufacturing method of copper-based halide microstructure linear array type scintillator and detector

CN122017926ACN 122017926 ACN122017926 ACN 122017926ACN-122017926-A

Abstract

The invention discloses a copper-based halide microstructure linear array type scintillator and a manufacturing method of a detector. The detector sequentially comprises a high-reflection coating, a copper-based halide scintillator array and a photodiode array along the ray direction, wherein the scintillator is selected from Cs 3 Cu 2 I 5 、CsCu 2 I 3 and other doping systems of Zn, tl, ce and the like, a triangular, n-shaped or trapezoid periodic microstructure array is prepared on the crystal surface, and the microstructure linear array type scintillator can realize the spatial resolution of more than or equal to 6 lp/mm. The preparation of the linear array type scintillator adopts a rotary furnace to dynamically synthesize a precursor in a solid phase, the precursor is melt-grown in a graphite array die, a reflecting layer is sprayed by ultrasonic, and the precursor is coupled to a diode array in vacuum, so that the whole process is low-temperature, solvent-free and expandable. The detector has the advantages of high light output, low afterglow, high resolution and environmental friendliness, and meets the requirements of high speed and low dosage for security inspection, medical imaging and the like.

Inventors

  • YANG CHENGZHANG
  • WANG ZHICHENG
  • LI XIAOMING
  • WANG CHUJIE

Assignees

  • 杭州钛光科技有限公司

Dates

Publication Date
20260512
Application Date
20251230

Claims (9)

  1. 1. A copper-based halide microstructure linear array scintillator and a detector are characterized in that the scintillator comprises the following components in sequence along the incident direction of rays: The crystal has periodic microstructure bulges, the cross section of each bulge is triangular, n-shaped or trapezoid, the top end spacing is 100-300 mu m, the bottom end spacing is 10-300 mu m, the height is 100-2000 mu m, and the radius R of an n-shaped top arc is 5-25 mu m; The high-reflection titanium dioxide coating covers the upper surface and the four side surfaces of the scintillator array, the thickness is 5-50 mu m, and the coating is continuous on the inner wall of the groove and has no pinholes; The photodiode array is coupled with the lower surface of the scintillator array through low-stress transparent epoxy resin with the refractive index of 1.50-1.55 and the volume shrinkage rate of <1%, the thickness of the adhesive layer is 5-50 mu m, and the interface is bubble-free.
  2. 2. The detector of claim 1, wherein the copper-based halide scintillator array is composed of Cs 3 Cu 2 I 5 :tl single-phase crystals with a Tl doping concentration of 0.1mol% (Cs: tl=1000:1), the microstructure protrusions are isosceles triangles with a vertex angle of 15 °, a top pitch of 200 μm, a bottom pitch of 20 μm, and a height of 1.8mm.
  3. 3. The probe of claim 1, wherein the titanium dioxide coating is formed by ultrasonic spraying, ultrasonic atomization frequency is 80kHz, spraying temperature is 60-120 ℃ gradient temperature rise, annealing temperature is 200 ℃ and time is 2h.
  4. 4. A method of making the copper-based halide microstructure linear scintillator and detector of any one of claims 1-4, comprising the steps of: s1, accurately weighing a halide raw material containing Cs, cu and doping element M according to the stoichiometric ratio of a target copper-based halide scintillator, adding the halide raw material into a corundum rotary furnace, continuously rotating and reacting for 1-30 hours at 100-400 ℃ and 5-60rpm in an inert atmosphere, and obtaining single-phase or solid-solution copper-based halide precursor powder through solid-phase dynamic synthesis, wherein the doping element M is at least one of Zn, pb, mn, ag, in, sb, tl, tb, pr, ce, yb, gd, nd, lu, and the doping concentration is 0-10mol%; s2, preparing a microstructure die, namely pre-opening a groove on a high-purity graphite block, processing a periodic microstructure convex array on the bottom of the groove by using a diamond fly-cutting process, and then performing magnetron sputtering on a BN release layer with the thickness of 50-500 nm; S3, growing an array scintillator, namely filling the precursor obtained in the step S1 into a mould cleaned by plasma, vibrating repeatedly, vacuum and repressing, heating to 380 ℃ at 5 ℃ per min under nitrogen atmosphere, preserving heat for 12 hours, and cooling to room temperature at 1 ℃ per min; S4, preparing a reflecting layer, namely ultrasonically spraying 5-50 mu mTiO 2 coating on the upper surface and four sides of the scintillator array obtained in the S3, and annealing; and S5, coupling the detector, namely bonding the lower surface of the scintillator with the photodiode array by using low-stress transparent epoxy resin through a vacuum lamination process, and thermally curing the scintillator at 60 ℃ for 2 hours, wherein the thickness of the adhesive layer is 5-50 mu m.
  5. 5. The method according to claim 4, wherein the temperature of the rotary kiln in S1 is 200 ℃, the rotation speed is 20rpm, and the reaction time is 12 hours.
  6. 6. The method of claim 4, wherein the surface finish Ra of the graphite blocks in S2 is less than or equal to 0.1 μm, the release layer is a BN coating with a thickness of 200nm, and the surface energy is less than or equal to 25 mN.m -1 .
  7. 7. The method of claim 4, wherein the number of melt-polishing cycles in S3 is 3.
  8. 8. The method according to claim 4, wherein the TiO 2 slurry in S4 is sprayed to a thickness of 30 μm and the annealing condition is 200 ℃ for 2 hours.
  9. 9. The method according to claim 4, wherein the epoxy resin used in S5 has a refractive index of 1.53 and a volume shrinkage of 0.8%, and the transmittance of the cured interface at a wavelength of 550nm is not less than 90%.

Description

Manufacturing method of copper-based halide microstructure linear array type scintillator and detector Technical Field The invention relates to a manufacturing method of a copper-based halide microstructure linear array type scintillator and a detector. Background Although the traditional scintillators such as CsI: tl, GOS ceramics and the like have been commercialized on a large scale, the high light output and the mature technology of the scintillators lead the scintillators to be dominant in security inspection, petroleum well logging and medical imaging, and inherent defects still limit the requirements of a new generation system. CsI: tl has high light output but its long persistence problem, such as smear artifact generated by high speed baggage scanning in dynamic detection. GOS ceramic is not deliquescent, so that a micro-pixel array can be realized, but the sintering temperature of single crystals/ceramic is more than 1000 ℃ and above, and the problem of ultrahigh energy consumption is caused. With the evolution of security inspection and the like to ultra-high resolution and low dosage, the pursuit of real-time high frame rate in industrial online detection is urgent to need a novel scintillator material which is environment-friendly and can be patterned at low temperature so as to break through the bottleneck problem faced by the traditional scintillator and simplify the system link. At present, the copper-based halide material becomes an ideal candidate for replacing the traditional cesium iodide and gadolinium oxysulfide in the fields of X-ray radiation detection and the like due to the advantages of self-limiting exciton luminescence characteristic, low afterglow, milder melting temperature and the like. At present, a novel micro-nano structure array process of a copper-based halide material still belongs to the blank. Therefore, developing a solvent-free, lossless, scalable patterning process is of great importance to the push of new copper-based halide materials for use in industrial and security detection devices. Disclosure of Invention In view of the above, the invention provides a method for manufacturing a copper-based halide microstructure linear array scintillator and a detector. The first aspect of the present invention provides a copper-based halide microstructure linear array scintillator and a detector, comprising, in order along a radiation incident direction: The crystal has periodic microstructure bulges, the cross section of each bulge is triangular, n-shaped or trapezoid, the top end spacing is 100-300 mu m, the bottom end spacing is 10-300 mu m, the height is 100-2000 mu m, and the radius R of an n-shaped top arc is 5-25 mu m; The high-reflection titanium dioxide coating covers the upper surface and the four side surfaces of the scintillator array, the thickness is 5-50 mu m, and the coating is continuous on the inner wall of the groove and has no pinholes; The photodiode array is coupled with the lower surface of the scintillator array through low-stress transparent epoxy resin with the refractive index of 1.50-1.55 and the volume shrinkage rate of <1%, the thickness of the adhesive layer is 5-50 mu m, and the interface is bubble-free. According to the embodiment of the invention, the copper-based halide scintillator array consists of Cs 3Cu2I5:Tl single-phase crystals, the Tl doping concentration is 0.1mol%, the microstructure protrusions are isosceles triangles with the apex angle of 15 degrees, the top end spacing is 200 mu m, the bottom end spacing is 20 mu m, and the height is 1.8mm. According to the embodiment of the invention, the titanium dioxide coating is formed by an ultrasonic spraying method, the ultrasonic atomization frequency is 80kHz, the spraying temperature is increased in a gradient manner from 60 ℃ to 120 ℃, the annealing temperature is 200 ℃, and the time is 2 hours. In a second aspect, the invention provides a method for preparing the copper-based halide microstructure linear array scintillator and detector, comprising the following steps: S1, accurately weighing a halide raw material containing Cs, cu and doping element M according to the stoichiometric ratio of a target copper-based halide scintillator, adding the halide raw material into a corundum material rotary furnace tube, continuously rotating at 100-400 ℃ and 5-60rpm in an inert atmosphere for reaction for 1-30h, and obtaining single-phase or solid solution type copper-based halide precursor powder through solid-phase dynamic synthesis, wherein the doping element M is at least one of Zn, pb, mn, ag, in, sb, tl, tb, pr, ce, yb, gd, nd, lu, and the doping concentration is 0-10mol%; s2, preparing a microstructure die, namely pre-opening a groove on a high-purity graphite block, processing a periodic microstructure convex array on the bottom of the groove by using a diamond fly-cutting process, and then performing magnetron sputtering on a BN release layer with the thickness of 50-500 nm; S3, gr