CN111519165A - Deliquescent scintillator photonic crystal and preparation method thereof - Google Patents
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Abstract
The invention discloses a deliquescent scintillator photonic crystal and a preparation method thereof, which avoid the direct contact of the deliquescent scintillator and water in the preparation process by transferring a heat release adhesive tape; the photonic crystal prepared by the method has stable structural property and compact structure, can obviously enhance the light output of the scintillator and exerts the effect of photonic crystal enhancement; the method is economical and applicable, and can be used for mass production.
Description
Technical Field
The invention belongs to the field of nuclear radiation detection and devices, and particularly relates to a preparation method of a deliquescent scintillator photonic crystal.
Background
Halide inorganic scintillators (e.g., CsI (Na), CsI (Tl), NaI (Tl), SrI2(Eu), LaCl3(Ce), LaBr3 (Ce)) generally have excellent scintillation properties. For example, CsI (Na) crystals as alkali metal halide inorganic scintillators have high density, atomic number and high light yield, thereby showing good stopping power for heavy charged particles and gamma rays and extremely unique radiation response and detection properties. It is as an idealThe scintillation material is widely applied to the fields of radiation imaging, high-energy physics, neutron-atomic nucleus scattering detection, nuclear medicine, dark substance detection, space detection and the like.
The halide inorganic scintillator has a high refractive index (usually between 1.7 and 1.9), and under the excitation of the high-energy particles to be measured, a large number of photons are generated inside the scintillator, and when the photons with an incident angle larger than the critical angle are totally reflected by the interface, the photons cannot be emitted effectively. The larger the refractive index, the more scintillation photons that cannot exit. Thus reducing the effective light output of the scintillator and hence the signal-to-noise ratio, sensitivity, etc. related performance of the detector.
In order to overcome the problem that photons caused by total reflection are limited in a scintillator and cannot be emitted, the photonic crystal can be prepared on the surface of the scintillator, the photonic crystal is an array structure material with refractive indexes distributed in a space period, and when scintillation photons larger than a total reflection angle reach an interface and meet the photonic crystal, the originally totally reflected light can be effectively extracted through the coupling of evanescent waves, so that the effective light output is improved, and various performances of a detector can be improved.
The patent (zl201410496266. x) discloses a photonic crystal preparation method based on a self-assembly microsphere array structure, by adopting the method, the photonic crystal can be prepared on the surface of a scintillator, the effective light output of the scintillator is improved, and the method has the advantages of low cost, simple preparation process and large-area preparation. However, this method is only applicable to non-deliquescent scintillators because the scintillator must be immersed in water in a critical step in order to self-assemble the microspheres on its surface.
Since halide inorganic scintillators are all deliquescent scintillators, the deliquescent scintillators can be damaged if immersed in water, and therefore, photonic crystals cannot be prepared on the surfaces of the deliquescent scintillators by adopting the method.
Disclosure of Invention
In order to produce photonic crystals on deliquescent scintillator surfaces, a new method must be developed which avoids direct contact of the scintillator with water during the production of the photonic crystals. In order to solve the problems, the invention provides a preparation method of a deliquescent scintillator photonic crystal; the specific technical scheme is as follows:
a preparation method of a deliquescent scintillator photonic crystal comprises the following steps:
1) soaking the silicon wafer in a 10-15% lauryl sodium sulfate solution for not less than 24 hours;
2) preparing a suspension by using a PS microsphere colloidal particle solution and water, and slowly dripping the suspension on the surface of the silicon wafer to perform PS microsphere self-assembly;
3) after the solution on the silicon chip is dried, slowly putting the silicon chip into deionized water; obtaining a single-layer PS microsphere array which is closely arranged;
4) fishing out the PS microsphere array from the water surface by using a glass slide, and after the water is volatilized, keeping the PS microsphere array on the glass slide;
5) in a dry ultra-clean environment, the heat release adhesive tape is tightly attached to the PS microsphere array on the glass slide, and a stamping machine is used for applying uniform pressure to ensure that the PS microsphere array is completely attached to the heat release adhesive tape;
6) the heat release adhesive tape attached with the PS microsphere array is taken off, and a stamping machine is used for applying uniform pressure to attach the surface of the heat release adhesive tape adhered with the PS microsphere array to the target surface of the deliquescent scintillator sample;
7) heating the sample to a degumming temperature of 90-110 ℃, and preserving heat for 30-60 seconds to completely degum the heat-release adhesive tape, wherein the PS microsphere array is attached to the surface of the sample due to van der Waals force;
8) and plating a conformal layer covering the whole scintillator on the prepared scintillator by utilizing an Atomic Layer Deposition (ALD) technology.
Further, the silicon wafer soaking time in the step 1) is 24-48 hours.
Further, the diameter of the PS microspheres in the step 2) is 300-600 nm.
Further, the pressure range in step 5) is 0.1-0.3 MPa.
Further, the pressure range in step 6) is 0.1-0.3 MPa.
Further, step 8) Wherein the substance of the conformal layer is TiO2、SiO2、Ta2O5、Al2O3。
Further, the thickness of the conformal layer in the step 8) is 30-90 nm.
Further, the dropping speed of the suspension in the step 2) is 1-2s of interval between every two drops.
Further, the speed of putting the silicon chip into the deionized water in the step 3) is controlled to be 1.6-3 mm/s.
The invention also discloses the deliquescent scintillator photonic crystal prepared by the method, which comprises the deliquescent scintillator, wherein a single layer of PS microspheres which are closely arranged is arranged outside the scintillator; a conformal layer is arranged outside the PS microsphere layer.
The preparation method of the deliquescent scintillator photonic crystal avoids the direct contact between the deliquescent scintillator and water in the preparation process through the transfer of the heat release adhesive tape; the photonic crystal prepared by the method has stable structural property and compact structure, can obviously enhance the light output of the scintillator and exerts the effect of photonic crystal enhancement; the method is economical and applicable, and can be used for mass production.
Drawings
FIG. 1 is an electron micrograph of a photonic crystal structure in example 1;
FIG. 2 is a scintillation luminescence spectrum of the sample of example 1 under X-ray excitation;
FIG. 3 is an electron micrograph of a photonic crystal structure in example 2;
FIG. 4 is a scintillation luminescence spectrum of the sample under X-ray excitation in example 2.
Detailed Description
The present invention will now be more fully described with reference to the following examples. This invention may, however, be embodied in many different forms and should not be construed as limited to the exemplary embodiments set forth herein.
For ease of description, spatially relative terms, such as "upper," "lower," "left," "right," and the like, may be used herein to describe one element or feature's relationship to another element or feature as illustrated in the figures. It will be understood that the spatial terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "below" other elements or features would then be oriented "above" the other elements or features. Thus, the exemplary term "lower" can encompass both an upper and a lower orientation. The device may be otherwise oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
Example 1
The scintillator used in this example was csi (na), and the crystal had a diameter of 30 mm and a thickness of 2 mm.
In a dry clean room, the preparation steps are as follows:
1) soaking the silicon wafer in a lauryl sodium sulfate solution with the mass fraction of 10% for 24 hours to form a hydrophilic monomolecular layer on the surface of the silicon wafer.
2) The suspension with the mass fraction of 2.5 percent of PS microsphere colloidal particle solution is prepared by adding deionized water into the PS microsphere colloidal particle solution with the diameter of 300nm purchased from Wuhan Huake Microscience and technology Limited liability company. Taking out the silicon wafer; three drops (about 0.15 ml) are dropped on the surface of the silicon chip by a pipette, the interval between every two drops is 1-2s, and then the PS microspheres can be self-assembled on the silicon chip to form a hexagonal close-packed microsphere periodic array structure. The suspension of 2.5 percent of suspension is only convenient for preparation, and other suspensions of PS microsphere colloidal particle solution with mass fraction can also be used in use.
3) After the suspension on the silicon wafer is completely dried, slowly putting the silicon wafer into deionized water; the speed of putting the silicon chip into the deionized water is controlled between 1.6 mm/s and 3 mm/s. Since the density of PS microspheres is less than that of water, the PS microsphere array will float on the water surface.
4) And fishing out the PS microsphere array by using a glass slide, and after the water is volatilized, keeping the PS microsphere array on the glass slide.
5) In a dry ultra-clean room, the heat release adhesive tape is tightly attached to the PS microsphere array on the glass slide, and a nano-imprint press with the model of Inpullin (NIL-100) is used for applying pressure of 0.1MPa to completely attach the PS microsphere array to the heat release adhesive tape;
6) the heat release adhesive tape attached with the PS microsphere array is removed, a nano-imprint machine is used for applying pressure of 0.1MPa to attach one surface of the heat release adhesive tape, which is adhered with the PS microsphere array, to the target surface of the CsI (Na) scintillator sample; the pressure needs to be controlled within a certain range, otherwise the integrity of the PS microspheres is affected.
7) And heating the sample to a degumming temperature of 90 ℃, preserving heat for 60 seconds to completely degum the heat-release adhesive tape, wherein the PS microsphere array is attached to the surface of the sample due to van der Waals force, and then removing the heat-release adhesive tape to obtain the scintillator with the PS microsphere array on the surface.
8) An atomic layer deposition system with the model of SUNALE R-200 is adopted, a 30-nanometer TiO2 conformal layer is plated on a CsI (Na) scintillator with a PS microsphere array prepared on the surface, and the conformal layer needs to cover the whole scintillator to form a protective layer, so that a final sample is obtained.
FIG. 1 is an electron micrograph of the surface photonic crystal structure of the prepared CsI (Na) scintillator, and it can be seen that the photonic crystal has a perfect periodic structure, and the expected effect is achieved.
Fig. 2 shows the scintillation luminescence spectra of the prepared scintillator with a photonic crystal structure on the surface and a reference sample without a structure under the excitation of X-rays, and it can be seen that the prepared photonic crystal significantly enhances the luminescence of csi (na), the enhancement ratio reaches 2.45 times, and the expected effect is obtained.
Example 2
The scintillator used in this example was csi (na), and the crystal had a diameter of 30 mm and a thickness of 2 mm.
In a dry clean room, the preparation steps are as follows:
1) soaking a silicon wafer in 15% of lauryl sodium sulfate solution by mass for 48 hours to form a hydrophilic monomolecular layer on the surface of the silicon wafer;
2) selecting a PS microsphere colloidal particle solution which is purchased from Wuhan Huake Microscience and technology Limited liability company and has the diameter of 400nm, adding water to prepare a suspension liquid with the mass fraction of the PS microsphere colloidal particle solution of 2.5%, dripping three drops (about 0.15 ml) by a liquid-transferring gun, dripping the drops on the surface of a processed silicon wafer at the interval of 1-2s, and then carrying out self-assembly on the PS microspheres on the silicon wafer;
3) after the solution on the silicon chip is dried, slowly putting the silicon chip into deionized water; the speed of putting the silicon chip into the deionized water is controlled between 1.6 mm/s and 3 mm/s. Because the density of the PS microspheres is less than that of water, the PS microsphere array can float on the water surface;
4) fishing out the PS microsphere array by using a glass slide, and after the water is volatilized, keeping the PS microsphere array on the glass slide;
5) in a dry ultra-clean room, the heat release adhesive tape is tightly attached to the PS microsphere array on the glass slide, and a nano-imprint press with the model of Inpullin (NIL-100) is used for applying pressure of 0.3MPa to completely attach the PS microsphere array to the heat release adhesive tape;
6) the heat release adhesive tape attached with the PS microsphere array is removed, a nano-imprint machine is used for applying pressure of 0.3MPa to enable one surface of the heat release adhesive tape, which is adhered with the PS microsphere array, to be attached to the target surface of the CsI (Na) scintillator sample;
7) heating the sample to a degumming temperature of 110 ℃, preserving heat for 30 seconds to completely degum the heat-release adhesive tape, wherein the PS microsphere array is attached to the surface of the sample due to van der Waals force, and then removing the heat-release adhesive tape to obtain the scintillator with the PS microsphere array on the surface; the temperature can ensure the degumming effect and can not cause the PS microsphere array to deform due to overhigh temperature; the photonic crystal is completely transferred to the surface of the scintillator, and a better light extraction effect is achieved.
8) An atomic layer deposition system with the model of SUNALE R-200 is adopted, a 90-nanometer SiO2 conformal layer is plated on a CsI (Na) scintillator with a PS microsphere array prepared on the surface, and the scintillator is coated to form a protective layer, so that a final sample is obtained. After the protective layer is added, the sufficient mechanical stability and the air isolation effect can be kept, and the conformal characteristic on the surface of the microsphere array cannot be lost due to too thick protective layer.
FIG. 3 is an electron micrograph of the photonic crystal structure of the CsI (Na) scintillator surface, from which it can be seen that the photonic crystal has a more perfect periodic structure, which achieves the expected effect.
Fig. 4 shows the scintillation luminescence spectra of the prepared scintillator with a photonic crystal structure on the surface and a reference sample without a structure under the excitation of X-rays, and it can be seen that the prepared photonic crystal significantly enhances the luminescence of csi (na), the enhancement ratio reaches 2.27 times, and the expected effect is obtained.
Examples 3 to 9
Using the above procedure, examples 3 to 9 were carried out, wherein the selection of the main preparation parameters and the test gave scintillation luminescence enhancement ratios as shown in table 1, for example. The results show that the method can obtain photonic crystal results and play a role in enhancing scintillation luminescence for the involved deliquescent scintillators.
Table 1 specification of parameters from examples 3 to 9
The preparation method disclosed by the invention is not limited to the deliquescent halide inorganic scintillator; it is also applicable to other deliquescent scintillators.
The above examples are only for illustrating the present invention, and besides, there are many different embodiments, which can be conceived by those skilled in the art after understanding the idea of the present invention, and therefore, they are not listed here.
Claims (10)
1. A preparation method of a deliquescent scintillator photonic crystal is characterized by comprising the following steps:
1) soaking the silicon wafer in a 10-15% lauryl sodium sulfate solution for not less than 24 hours;
2) preparing a suspension by using a Polystyrene (PS) microsphere colloidal particle solution and water, and slowly dripping the suspension on the surface of the silicon wafer to perform PS microsphere self-assembly;
3) after the solution on the silicon chip is dried, slowly putting the silicon chip into deionized water; obtaining a single-layer PS microsphere array which is closely arranged;
4) fishing out the PS microsphere array from the water surface by using a glass slide, and after the water is volatilized, keeping the PS microsphere array on the glass slide;
5) in a dry ultra-clean environment, the heat release adhesive tape is tightly attached to the PS microsphere array on the glass slide, and a stamping machine is used for applying uniform pressure to ensure that the PS microsphere array is completely attached to the heat release adhesive tape;
6) the heat release adhesive tape attached with the PS microsphere array is taken off, and a stamping machine is used for applying uniform pressure to attach the surface of the heat release adhesive tape adhered with the PS microsphere array to the target surface of the deliquescent scintillator sample;
7) heating the sample to a degumming temperature of 90-110 ℃, and preserving heat for 30-60 seconds to completely degum the heat-release adhesive tape, wherein the PS microsphere array is attached to the surface of the sample due to van der Waals force;
8) and plating a conformal layer covering the whole scintillator on the prepared scintillator by utilizing an Atomic Layer Deposition (ALD) technology.
2. The method for preparing the deliquescent scintillator photonic crystal of claim 1, wherein the silicon wafer in step 1) is soaked for 24-48 hours.
3. The method for preparing the deliquescent scintillator photonic crystal as claimed in claim 1, wherein the diameter of the PS microsphere in the step 2) is 300-600 nm.
4. The method of preparing a deliquescent scintillator photonic crystal of claim 1, wherein the pressure in step 5) is in the range of 0.1 to 0.3 MPa.
5. The method for preparing a deliquescent scintillator photonic crystal of claim 1, wherein the pressure in step 6) is in the range of 0.1 to 0.3 MPa.
6. The method of preparing a deliquescent scintillator photonic crystal of claim 1, wherein the material of the conformal layer in step 8) is TiO2、SiO2、Ta2O5、Al2O3。
7. The method of preparing a deliquescent scintillator photonic crystal of claim 1, wherein the thickness of the conformal layer in step 8) is 30-90 nm.
8. The method for preparing a deliquescent scintillator photonic crystal according to claim 1, wherein the suspension is dropped at a speed of 1-2s per drop in step 2).
9. The method for preparing a deliquescent scintillator photonic crystal according to claim 1, wherein the speed of putting the silicon wafer into the deionized water in the step 3) is controlled to be 1.6-3 mm/s.
10. A deliquescent scintillator photonic crystal prepared by the method of any one of claims 1 to 9, comprising a deliquescent scintillator having a single layer of closely packed PS microspheres disposed outside the deliquescent scintillator; a conformal layer is arranged outside the PS microsphere layer.
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Cited By (1)
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CN112716511A (en) * | 2020-12-21 | 2021-04-30 | 华中科技大学 | Novel scintillation crystal detector and design method and application thereof |
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