CN115677899A - Plastic scintillator doped with organic tin compound and preparation method thereof - Google Patents
Plastic scintillator doped with organic tin compound and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an organic tin compound doped plastic scintillator and a preparation method thereof. The organic tin compound-doped plastic scintillator includes: plastic matrix, initiator, cross-linking agent, fluorescent dye and organic tin compound; the content of the initiator in the organic tin compound doped plastic scintillator is 0-1 wt%; the content of the fluorescent dye is 0.01-30 wt%; the content of the cross-linking agent is 0-10 wt%; the content of the organic tin compound is 0.1-60 wt%.
Description
Technical Field
The invention relates to an organic tin compound doped plastic scintillator and a preparation method and application thereof, belonging to the field of radiation detection.
Background
A scintillator is a component of a scintillator detector that interacts with particles to convert high-energy rays or particles to visible or ultraviolet light by ionizing radiation. As an optical functional material, the material is widely applied to the fields of high-energy physics, medical imaging, security and protection, industrial exploration and the like. At present, inorganic scintillation crystals NaI: tl and CsI: tl are the most important scintillators for gamma ray energy spectrum detection, but have the defects of easy deliquescence, high cost, difficulty in large-size preparation and long decay time.
The plastic scintillator is generally prepared by taking a polymerizable monomer as a matrix and adding a fluorescent substance for polymerization, and has the advantages of good environmental stability, extremely low cost, easiness in large-size preparation, quick attenuation and the like. However, conventional plastic scintillators are limited by the low effective atomic number (Z) eff ) Only gamma ray counting detection can be realized, and the energy spectrum detection capability is lacked. And the high effective atomic number sensitized plastic scintillator increases Z eff The preparation method has the advantages that the stopping capacity of the plastic scintillator on gamma rays is improved, the gamma ray energy spectrum detection capacity is realized, in addition, the plastic scintillator has the fast neutron detection capacity, and the gamma/neutron discrimination can be realized, so the research and the development of the high atomic number sensitized plastic scintillator are greatly concerned. Although commercially available organic heavy metal compound-doped plastic scintillators have been prepared, limitations such as high-content doping of organic heavy metal compounds, heavy atom fluorescence quenching effect, etc. are still difficult to achieve, and energy resolution is still not shown and light yield is drastically reduced in EJ-256 products doped with 5wt% pb by Eljen, usa.
In conclusion, the organic heavy metal compound doped plastic scintillator with high effective atomic number, moderate light yield and gamma/neutron resolution capability has high practical value in the radiation detection field such as portal security inspection and the like.
Disclosure of Invention
In order to overcome the defect that the traditional plastic scintillator cannot carry out energy spectrum detection, the invention aims to provide an organic tin compound doped plastic scintillator and a preparation method and application thereof.
In a first aspect, the present invention provides an organotin compound-doped plastic scintillator comprising: plastic matrix, initiator, cross-linking agent, fluorescent dye and organic tin compound;
the content of the initiator in the organic tin compound doped plastic scintillator is 0 to 1 weight percent
The content of the fluorescent dye is 0.01-30 wt%;
the content of the cross-linking agent is 0-10 wt%;
the organotin compound is contained in an amount of 0.1 to 60wt% (may be 0.1 to 40wt%, and more preferably 40 to 60 wt%).
Preferably, the structural general formula of the organotin compound is (R) 1 ) x (R 2 ) 4-x Sn; wherein x is 0, 1, 2, 3, or 4; r 1 Is a straight or branched alkyl substituent, preferably at least one selected from the group consisting of methyl, ethyl, propyl, butyl, isopropyl and tert-butyl; r is 2 Is at least one of a straight chain or branched chain substituent containing an unsaturated bond, a substituent containing a benzene ring or an aromatic heterocyclic ring, a substituent containing halogen, a substituent containing an ester group or a carbonyl group.
Preferably, the unsaturated bond-containing linear or branched substituent is at least one selected from the group consisting of vinyl, propenyl, 3-methyl-2-butenyl, propynyl, alkynyl, 1-ethoxyvinyl, cistanyl, acrylate, methyl methacrylate, vinyl methacrylate, and furfuryl methacrylate;
the substituent containing the benzene ring or the aromatic heterocyclic ring is at least one selected from phenyl, benzyl, phenethyl, phenylpropyl, furyl, thienyl, thiazolyl, imidazolyl, pyridyl, oxazolyl, styryl, methyl styryl and the like;
the halogen-containing substituent is selected from at least one of fluorine, chlorine, bromine, iodine, iodomethyl and the like;
the substituent containing an ester group or a carbonyl group is at least one selected from the group consisting of a 2-ethyl-hexanoyl group, an ethyl ester group, a propyl ester group, a 2, 4-pentanedionyl group, a 2, 6-tetramethyl-3, 5-heptanedionyl group, and the like. Generally, the organotin compound can be uniformly doped at 0.1 to 40wt% without adding a crosslinking agent. When the content of the organic tin compound is more than 40 and less than or equal to 60 weight percent, the crosslinking agent is added to realize uniform doping. In particular cases, when R is an organotin compound 2 When the unsaturated bond is at least one of a linear or branched substituent containing an unsaturated bond, a styryl group, a methylstyrene group, and the like (for example, tin of a styrene group), the unsaturated bond can participate in copolymerization of the plastic matrix monomer, and high content (40 to 60 wt%) doping can be performed without adding a crosslinking agent.
Preferably, the plastic matrix is formed by polymerizing matrix monomers containing unsaturated bond active groups; preferably selected from the group consisting of polymers synthesized from vinyl group-containing monomers and/or polymers synthesized from terephthalate group-containing monomers, and more preferably at least one of polystyrene, polyvinyltoluene, poly (9-vinylcarbazole), polymethyl methacrylate, and polyethylene terephthalate.
Preferably, the initiator is at least one selected from azo initiators, peroxide initiators and photoinitiators, preferably at least one selected from azobisisobutyronitrile, azobisisovaleronitrile, azobisisoheptonitrile, benzoyl peroxide t-butyl peroxide, methyl ethyl ketone peroxide, photoinitiators 184, photoinitiators BAPO and the like.
Preferably, the crosslinking agent is at least one selected from the group consisting of a substance having a plurality of functional groups in a molecule and a compound having a plurality of unsaturated double bonds in a molecule. Preferably at least one selected from Divinylbenzene (DVB), ethylene glycol dimethacrylate, bisphenol a dimethacrylate, and the like.
Preferably, the fluorescent dye comprises a primary fluorescent dye and/or a wave-shifting agent;
the primary fluorescent dye is selected from at least one of 2, 5-diphenyl oxazole, p-terphenyl, 2- (4 '-tert-butylbenzene) -5- (4' -biphenyl) -1,3, 4-oxadiazole, 2- (4-biphenyl) -5-phenyl oxadiazole and the like;
the wave-shifting agent is at least one selected from 1, 4-bis (5-phenyl-2-oxazolyl) benzene (POPOPOP), 1, 4-bis (2-methylstyrene), 1, 4-bis (4-methylstyrene), 9, 10-diphenylanthracene, coumarin 6, 7-diethylamino-4-methylcoumarin, etc.
In a second aspect, the present invention provides a method for preparing an organotin compound-doped plastic scintillator, comprising:
(1) In an inert atmosphere, mixing a monomer, an initiator, a cross-linking agent, a fluorescent dye and an organic tin compound of a plastic substrate to obtain a mixed solution;
(2) And sealing the mixed solution, and polymerizing for 1-4 weeks at 40-120 ℃ to obtain the organic tin compound doped plastic scintillator. For example, in the process of preparing a plastic scintillator, an organotin compound is doped into a plastic monomer such as styrene, vinyl toluene, etc. in a corresponding mass ratio and sufficiently mixed.
In a third aspect, the present invention provides a method for preparing an organotin compound-doped plastic scintillator, comprising:
(1) In an inert atmosphere, mixing a monomer of a plastic substrate, an initiator, a cross-linking agent, a fluorescent dye and an organic tin compound, sealing the mixture, and heating and polymerizing the mixture to obtain a solid material of the plastic scintillator doped with the organic tin compound. Adding solid materials of the plastic scintillator doped with the organic tin compound into a hopper of an injection molding machine, and screwing a mold by using a mold closing device;
(2) Under the action of a heater, the solid materials in the machine barrel are fully heated under the action of the rotation of the screw and the shearing force to obtain the resin in a molten flow state;
(3) Conveying the molten resin to the front end of the machine barrel through the rotation of the screw, continuously conveying the molten resin under the action of pressure, and injecting the molten resin into a mold cavity from a pouring gate through a main runner and a branch runner;
(4) And (3) after the mold cavity is filled with the resin, maintaining the pressure for a certain time to cool and mold the organic tin compound doped plastic scintillator, and taking out the organic tin compound doped plastic scintillator through a demolding device and an ejection device.
In a fourth aspect, the present invention provides a method for preparing an organotin compound-doped plastic scintillator, comprising:
(1) In an inert atmosphere, mixing a monomer of a plastic substrate, an initiator, a cross-linking agent, a fluorescent dye and an organic tin compound, sealing the mixture, and heating and polymerizing the mixture to obtain a solid material of the plastic scintillator doped with the organic tin compound. Adding solid materials of the plastic scintillator doped with the organic tin compound into a hopper of an extruder, and installing an extrusion die with a certain shape at the end of an extrusion die;
(2) Under the action of a heater, the solid materials in the machine barrel are fully heated through the rotation of the screw and the action of shearing force, and the molten resin is obtained;
(3) The resin in a molten state is conveyed to the front end of a machine barrel through the rotation of a screw, and is extruded and molded continuously through an installed extrusion die under the extrusion action of a screw or a plunger of an extruder to obtain an organic tin compound doped plastic scintillator product.
In a fifth aspect, the present invention provides an application of an organotin compound-doped plastic scintillator in the radiation detection field, wherein the radiation detection field comprises: x-ray detection, gamma ray spectroscopy detection, and neutron/gamma pulse shape discrimination.
Has the advantages that:
the invention discloses a preparation method and an example of an organic tin compound-doped plastic scintillator, wherein the plastic scintillator consists of a matrix, an initiator, a cross-linking agent, a fluorescent dye and an organic tin compound, and the preparation method comprises a bulk polymerization method, an injection molding method and an extrusion molding method. Compared with the undoped plastic scintillator, the plastic scintillator doped with the organic tin compound prepared by the invention not only retains the advantage of nanosecond fast attenuation of the plastic scintillator, but also increases the capability of gamma ray energy spectrum detection;
in the invention, the plastic scintillator doped with the organic tin compound has high effective atomic number, fast decay time, moderate light yield and better energy resolution, can be applied to X-ray detection, gamma-ray energy spectrum detection and gamma/neutron discrimination, and has important application prospect in the radiation detection field such as portal security inspection and the like.
Drawings
FIG. 1 is a photograph of samples of different tributyl (1-ethoxyethylene) tin concentrations doped plastic scintillators of example 1 under natural light; the sample size is 10mm high and 15mm in diameter;
FIG. 2 is a scintillation performance test of tributyl (1-ethoxyethylene) tin-doped plastic scintillator in example 1. Wherein a is the X-ray excitation emission spectrum of the plastic scintillator doped with different tributyl (1-ethoxyethylene) tin concentrations, and b is 20wt% of the plastic scintillator doped with tributyl (1-ethoxyethylene) tin 137 The scintillation decay time under the excitation of a Cs source, c is the content of tributyl (1-ethoxyethylene) tin doped plastic scintillators with different concentrations 137 Multichannel energy spectrum under Cs source irradiation, d is 20wt% of tributyl (1-ethoxyethylene) tin doped plastic scintillator 137 Multichannel energy spectrum under Cs source irradiation (determination of light yield and energy resolution compared with commercial inorganic scintillator BGO);
FIG. 3 is a scintillation performance test of a 40wt% tributyl (1-ethoxyethylene) tin-doped plastic scintillator of example 1 (in this example the wave-shifting agent is coumarin 6). Wherein a is the X-ray excitation emission spectrum and b is 137 Decay time of scintillation under Cs source excitation, c is 137 A plurality of energy spectrograms under the irradiation of a Cs source;
FIG. 4 is a photograph of samples of various concentrations of tributylphenyl tin-doped plastic scintillator (a) and various concentrations of 2-tributylstannyl thiophene-doped plastic scintillator (b) provided in example 2 under natural illumination; the sample size is 10mm high and 15mm in diameter;
fig. 5 is a scintillation performance test of the tributylphenyl tin-doped plastic scintillator provided in example 2. Wherein a is X-ray excitation emission spectrum of tributyl phenyl tin doped plastic scintillator with different concentrations, and b is 20wt% of tributyl phenyl tin doped plastic scintillator 137 The scintillation decay time under the excitation of a Cs source, c is the content of tributyl phenyl tin doped plastic scintillators with different concentrations 137 A multichannel energy spectrum under the irradiation of a Cs source;
FIG. 6 is 2 provided in example 2-testing the scintillation performance of the tributylstannyl thiophene doped plastic scintillator. Wherein a is the X-ray excitation emission spectrum of 2-tributylstannyl thiophene-doped plastic scintillator with different concentrations, b is 20wt% 137 The scintillation decay time under the excitation of a Cs source, c is 2-tributylstannyl thiophene doped plastic scintillators with different concentrations 137 A plurality of energy spectrograms under the irradiation of a Cs source;
FIG. 7 is a scintillation performance test of 40wt% 2-tributylstannyl thiophene doped plastic scintillators provided in example 2 (the wave-shifting agent in this example is coumarin 6). Wherein a is an X-ray excitation emission spectrum and b is 137 Scintillation decay time under Cs source excitation;
FIG. 8 is a photograph of samples of different concentrations of dibutyltin diacetate doped plastic scintillators provided in example 4 under natural illumination; the sample size is 10mm high and 15mm in diameter;
FIG. 9 is a scintillation performance test for different concentrations of dibutyltin diacetate doped plastic scintillators provided in example 4. Wherein a is the X-ray excitation emission spectrum of the dibutyltin diacetate doped plastic scintillator, and b is 10wt% of the dibutyltin diacetate doped plastic scintillator 137 The scintillation decay time under the excitation of a Cs source, c is the ratio of dibutyl tin diacetate with different concentrations to a plastic scintillator 137 A plurality of energy spectrograms under the irradiation of a Cs source;
FIG. 10 is a photograph of a sample of the 10wt% different organotin compound-doped plastic scintillator provided in example 5 under natural illumination; the sample size is 15mm high and 15mm in diameter;
FIG. 11 is a scintillation performance test of 10wt% different organotin compound-doped plastic scintillator provided in example 5. Wherein a is an X-ray excitation emission spectrum and b is 137 And (4) multichannel energy spectrograms under irradiation of a Cs source.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
In the present disclosure, an organotin compound-doped plastic scintillator is composed of a plastic matrix, an initiator, a crosslinking agent, a fluorescent dye, and an organotin compound. Wherein, the content of the initiator can be 0 to 1 weight percent (weight percentage content); the content of the cross-linking agent can be 0 to 10 weight percent (weight percentage content); the content of the fluorescent dye can be 0.01-30 wt% (weight percentage content); the content of the organotin compound may be 0 to 40% by weight or more and 40 to 60% by weight or more.
In an alternative embodiment, the initiator or the cross-linking agent is added at a low doping level without adding the initiator or the cross-linking agent in order to shorten the polymerization time of the plastic scintillator doped with the high-content organotin compound.
In an alternative embodiment, the organotin compound may be of the structure: formula (R) 1 ) x (R 2 ) 4-x An organotin compound of Sn wherein R 1 Is a straight-chain or branched alkyl substituent, R 2 Is a straight or branched substituent containing an unsaturated bond, and x is an integer of 0 to 4. R is 1 Typical examples of (a) include, but are not limited to, methyl, ethyl, propyl, butyl, isopropyl, and tert-butyl. R 2 Typical examples of (a) include, but are not limited to, ethenyl, propenyl, 3-methyl-2-butenyl, propynyl, butynyl, 1-ethoxyethenyl, cisbutynyl, acrylate, methyl methacrylate, vinyl methacrylate, and furfuryl methacrylate. The organotin compound may be contained in an amount of 0.1 to 60wt%, preferably 3 to 40wt%, more preferably 10 to 30wt%.
Wherein, the gamma ray and the scintillator deposit the energy thereof on one or more electrons in the detector material through Compton scattering and photoelectric effect, and the electrons are de-excited to generate visible light. In which the photoelectric effect depends on the effective atomic number (Z) of the material eff ) And with Z eff Is proportional to the fourth power of (c). Plastic scintillator not doped with organic tin compound only contains light elements of carbon, hydrogen, oxygen, nitrogen and the like, Z of material eff Small, gamma rays can only interact with a plastic scintillator in a Compton scattering mode, can only realize gamma ray counting detection, and lack energy spectrum detection capability. And plastic flash doped with organic tin compoundScintillators having high Z eff Organic heavy metal compounds such as organic tin, lead, etc., increase the Z of the plastic scintillator eff The blocking capacity of the detector to gamma rays is improved, energy deposition in the form of photoelectric effect is increased, and therefore gamma ray energy spectrum detection can be achieved. In addition, since the introduction of the organotin compound only serves to increase the energy deposition and does not introduce a new slow luminescence center, the fast decay characteristic of the plastic scintillator is still maintained. If the amount of the organic tin compound added is insufficient, the effective atomic number Ze of the material is caused ff Low, difficult to deposit energy by photoelectric effect, unable to form photoelectric effect peak, resulting in poor gamma ray detection ability. If the addition amount of the organotin compound is too high, the following two cases result: (1) Exceeding the solubility limit results in the precipitation of the doping compound during plastic flash polymerization, rendering the plastic flash opaque; (2) The doped plastic flash is difficult to polymerize, and the prepared sample is difficult to mold or soft and cannot be subjected to subsequent processing.
In an alternative embodiment, the organotin compound may be of the structure: formula (R) 1 ) x (R 2 ) 4-x An organotin compound of Sn wherein R 1 Is a straight-chain or branched alkyl substituent, R 2 Is a substituent containing a benzene ring or an aromatic heterocyclic ring, and x is an integer of 0 to 4. R 1 Typical examples of (a) include, but are not limited to, methyl, ethyl, propyl, butyl, isopropyl, and tert-butyl. R is 2 Typical examples of (d) include, but are not limited to, phenyl, benzyl, phenethyl, phenylpropyl, furyl, thienyl, thiazolyl, imidazolyl, pyridyl, oxazolyl, styryl, or methylstyryl. The organotin compound may be contained in an amount of 0.1 to 60wt%, preferably 3 to 40wt%, more preferably 10 to 30wt%.
In an alternative embodiment, the organotin compound may be of the structure: formula (R) 1 ) x (R 2 ) 4-x An organotin compound of Sn wherein R 1 Is a straight-chain or branched alkyl substituent, R 2 Is a halogen-containing substituent, and x is an integer between 0 and 4. R 1 Typical examples of (A) include, but are not limited to, methyl, ethyl, propylButyl, isopropyl and tert-butyl. R 2 Typical examples of (a) include, but are not limited to, fluorine, chlorine, bromine, iodine, iodomethyl. The organotin compound may be contained in an amount of 0.1 to 40wt%, preferably 3 to 30wt%, more preferably 10 to 20wt%.
In an alternative embodiment, the organotin compound may be of the structure: formula (R) 1 ) x (R 2 ) 4-x An organotin compound of Sn wherein R 1 Is a straight-chain or branched alkyl substituent, R 2 Is a substituent containing an ester group or a carbonyl group, and x is an integer of 0 to 4. R 1 Typical examples of (a) include, but are not limited to, methyl, ethyl, propyl, butyl, isopropyl, and tert-butyl. R is 2 Typical examples of (B) include, but are not limited to, 2-ethyl-hexanoyl, ethyl, propyl, 2, 4-pentanedionyl, 2, 6-tetramethyl-3, 5-heptanedionyl. The organotin compound may be contained in an amount of 0.1 to 40% by weight, preferably 5 to 30% by weight, more preferably 10 to 20% by weight.
The following is an exemplary description of a method for preparing an organotin compound-doped plastic scintillator by a bulk polymerization method.
Step 1: sequentially passing through deionized water, ethanol and acetone respectively, cleaning the glass reaction vessel for three times, putting the glass reaction vessel into an oven, standing overnight, and heating and drying in vacuum.
Step 2: in an inert atmosphere, adding a matrix monomer, an initiator (0-1 wt%), a cross-linking agent (0-10 wt%), a fluorescent dye (0.01-30 wt%) and an organic tin compound into the glass reaction vessel cleaned in the step 1, and dissolving at normal temperature or by ultrasonic waves to obtain a uniform solution system.
And 3, step 3: after the glass reaction vessel equipped with the mixed solution in step 2 is sealed, it is put into an oven or added to a prescribed polymerization temperature using a heat transfer fluid (oil, water, etc.) and polymerization is carried out while maintaining the temperature for several days. The polymerization temperature and polymerization time are partially different according to the property and doping amount of the added organotin compound, the organotin compound with low boiling point and low doping content is generally selected to be polymerized at 40-100 ℃ for several weeks, and higher doping amount may require longer time; high boiling point, low doping level organotin compounds may be selected for polymerization at 60-120 deg.c for several weeks, with higher doping levels possibly requiring longer times.
And 4, step 4: after the polymerization is finished, the temperature is slowly reduced to room temperature so as to reduce internal stress. And taking the cured product out of the glass container, cutting and polishing to obtain the required organic tin compound doped plastic scintillator.
As a further preferable scheme, the matrix monomer is purified to remove the stabilizer and water, the purity of other raw materials is more than 95%, and the batching environment is an inert gas environment (a glove box filled with argon or nitrogen).
The following is an exemplary description of a method for preparing an organotin compound-doped plastic scintillator by an injection molding method.
Step 1: in an inert atmosphere, mixing a plastic substrate, an initiator, a cross-linking agent, a fluorescent dye and an organic tin compound, sealing the mixture, and heating and polymerizing the mixture to obtain the solid material of the plastic scintillator doped with the organic tin compound. And adding the prepared solid material into a hopper of an injection molding machine, and screwing the mold by using a mold closing device.
Step 2: and (3) under the action of a heater, fully heating the solid materials in the cylinder in the step 1 to be in a molten flowing state through the rotation of the screw and the action of shearing force, and further uniformly mixing.
And 3, step 3: the melted resin in the step 2 is conveyed to the front end of the cylinder by the rotation of the screw, is continuously conveyed by high pressure, and is injected into the die cavity from the pouring gate through the main runner and the branch runner.
And 4, step 4: and (3) after the mold cavity is filled with the resin, maintaining the pressure for a period of time to cool and mold the plastic scintillator product, and taking out the prepared plastic scintillator product through a demolding device and an ejecting device.
As a further preferred option, in order to improve the final optical quality of the plastic scintillator, the raw materials are susceptible to contamination during the cartridge mixing step, and it is important to keep them clean. The solid material doped with the plastic scintillator or the mixed pre-polymerized resin is purified to remove impurities and water, and the whole preparation process is an inert gas environment (argon or nitrogen) to eliminate the influence of humidity and oxygen.
The following exemplarily illustrates a method for preparing an organotin compound-doped plastic scintillator by an extrusion molding method.
Step 1: in an inert atmosphere, mixing a plastic substrate, an initiator, a cross-linking agent, a fluorescent dye and an organic tin compound, sealing the mixture, and heating and polymerizing the mixture to obtain a solid material of the plastic scintillator doped with the organic tin compound. Adding the prepared solid material into a hopper of an extruder, and installing an extrusion die with a certain shape at the end of an extrusion die.
Step 2: and (3) under the action of a heater, fully heating the solid materials in the cylinder in the step 1 to be in a molten flowing state through the rotation of the screw and the action of shearing force, and further uniformly mixing.
And 3, step 3: and (3) conveying the molten resin in the step (2) to the front end of the machine barrel through the rotation of the screw, and obtaining a plastic scintillator product formed by continuous extrusion through the extrusion die arranged in the step (1) under the extrusion action of the screw or the plunger of the extruder.
As a further preferred option, the raw materials are susceptible to contamination during the barrel mixing step, and it is important to keep them clean. The solid material doped with the plastic scintillator or the mixed pre-polymerized resin is purified to remove impurities and water, a complex drying procedure with a nitrogen purging system in the whole preparation process can eliminate the influence of humidity, reduce the problem of degradation of plastics due to the existence of oxygen and improve the final optical quality of the plastic scintillator.
The present invention will be described in further detail with reference to examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing description are intended to be included within the scope of the invention. The specific process parameters and the like of the following examples are also merely one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below. In the following examples, different organotin compounds are selected and doped at different concentrations to obtain plastic scintillators with different optical and scintillation properties.
Example 1
This example 1 selects the formula (R) 1 ) x (R 2 ) 4-x One or two of the organotin compounds of Sn are doped in different concentrations, wherein R 1 Is a straight-chain or branched alkyl substituent, R 2 Is a straight or branched substituent containing an unsaturated bond, and x is an integer of 0 to 4. Specifically, tributyl (1-ethoxyethylene) tin is contained in the tin-based coating.
The preparation method of the organic tin compound doped plastic scintillator comprises the following steps:
in an inert atmosphere, a matrix monomer (vinyl toluene, abbreviated as VT), a primary fluorescent dye (PPO), a wave-shifting agent (POPOPOP) and tributyl (1-ethoxyethylene) tin (0-60 wt%, for example, 0wt%, 3wt%, 10wt%, 20wt%, 30wt%, 40wt%, 50wt%, 60 wt%) with different doping amounts are added into a cleaned and dried glass reaction vessel to be dissolved at normal temperature or by ultrasound, so as to obtain a uniform solution system. After the glass reaction vessel was sealed, it was put into an oil bath to be heated to a prescribed polymerization temperature and polymerization was carried out while maintaining the temperature for several days. Plastic scintillators with doping levels of 10wt% and below are typically selected for polymerization at 40-70 ℃ for three weeks, with higher doping levels (< 30 wt%) possibly requiring one month. Due to the solubility limit of POPOP, the higher doping amount is 40-60wt%, and a more soluble wave shifter (coumarin 6) is selected; and because the doping amount is increased, the polymerization time is longer, and the prepared doped plastic is easy to soften and difficult to process, so that a crosslinking agent (divinyl benzene, abbreviated as DVB) is added in the formula to increase the polymerization speed and the hardness of the doped plastic. The high-doping-amount plastic scintillator after the process optimization can be polymerized and finished by generally selecting the polymerization for three weeks at 40-70 ℃. After the polymerization is finished, the temperature is slowly reduced to room temperature so as to reduce internal stress. And taking the cured product out of the glass container, cutting and polishing to obtain the doped plastic scintillator. Higher doping amounts, such as 50wt% and 60wt% of the plastic scintillator, cause the organotin compounds to be eluted due to excessive doping, and cause opacity due to too fast a crosslinking speed.
As shown in a in FIG. 2, the test result of X-ray excitation emission spectrumThe emission peaks in the XEL doped with tributyl (1-ethoxyethylene) tin plastic scintillator are all derived from the wave-shifting agent popp; and with the increase of the doping concentration of tributyl (1-ethoxyethylene) tin, the XEL intensity is obviously higher than that of an undoped plastic scintillator, wherein the XEL intensity is the highest at 10wt%; as shown in the representation b in figure 2, 137 the scintillation decay time test result under Cs excitation shows that the plastic scintillator doped with tributyl (1-ethoxyethylene) tin still retains the fast decay characteristic of the traditional plastic scintillator, and the decay time is about 4ns;
the light yield of the plastic scintillator of the present invention was measured by a relative method. As shown in fig. 2 c, by 137 The result of multi-channel energy spectrum test under Cs excitation shows that with the increase of the doping concentration of tributyl (1-ethoxyethylene) tin, the scintillation light yield is reduced compared with that of an undoped plastic scintillator, but the counting rate is increased by about two times, and a full energy peak appears. Specific light yield and energy resolution are obtained by comparison with commercial inorganic scintillator BGO (size: 14X 5 mm), which is illustrated in FIG. 2 by d, with a light yield of 7500 phos/MeV and an energy resolution of about 16.3% @662keV;
as shown in a in FIG. 3, the X-ray excitation emission spectrum test result shows that the emission peak in the XEL doped with 40wt% of tributyl (1-ethoxyethylene) tin plastic scintillator comes from the wave-shifting agent coumarin 6;
as shown in the representation b in figure 3, 137 the scintillation decay time test result under Cs excitation shows that the plastic scintillator doped with 40wt% of tributyl (1-ethoxyethylene) tin still retains the fast decay characteristic of the traditional plastic scintillator, and the decay time is about 6ns;
as shown in c in fig. 3, by 137 The result of multi-channel energy spectrum test under Cs excitation shows that the counting rate of the plastic scintillator is improved due to higher-concentration tin doping, but because the luminescent peak position of coumarin 6 deviates from the sensitive wave band of PMT (R2059) used for testing, an obvious full-energy peak does not appear under the influence of detection efficiency. The tributyl (1-ethoxyethylene) tin-doped plastic scintillator can be applied to the radiation detection fields of X-ray detection, gamma-ray energy spectrum detection, gamma/neutron discrimination and the like.
Example 2
This example 2 selects the formula (R) 1 ) x (R 2 ) 4-x One or two of Sn organic tin compounds are doped with different concentrations, wherein R 1 Is a straight-chain or branched alkyl substituent, R 2 Is a substituent containing a benzene ring or a heterocyclic ring, and x is an integer between 0 and 4. Particularly, tributylphenyl tin and 2-tributylstannyl thiophene contained in the composition are selected.
The preparation method of the two organic tin compounds doped plastic scintillators comprises the following steps:
matrix monomer (VT), initiator (AIBN), primary fluorescent dye (PPO), wave-shifting agent (POPOPOP) and tributylphenyl tin (0-20 wt%, such as 0wt%, 3wt%, 7wt%, 20 wt%) and 2-tributylstannyl thiophene (0-60 wt%, such as 0wt%, 3wt%, 10wt%, 20wt%, 30wt%, 40wt%, 60 wt%) with different doping amounts are added into a cleaned and dried glass reaction vessel to be dissolved at normal temperature or ultrasound in an inert atmosphere, so as to obtain a uniform solution system. After the glass reaction vessel was sealed, it was put into an oil bath to heat it to a prescribed polymerization temperature and polymerization was carried out with keeping the temperature for several days. Plastic scintillators with doping levels of 10wt% and below are typically selected for polymerization at 40-70 ℃ for three weeks, with higher doping levels (20 wt%) polymerized at 90 ℃ for one month. Due to the solubility limit of POPOP, higher doping amount such as 40-60wt%, and more soluble wave shifter (coumarin 6); and because the doping amount is increased, the polymerization time is longer, and the prepared doped plastic is easy to soften and difficult to process, a cross-linking agent (DVB) is added in the formula to increase the polymerization speed and the hardness of the doped plastic. The high-doping-amount plastic scintillator after the process optimization is polymerized for three weeks at 40-70 ℃ usually. After the polymerization is finished, the temperature is slowly reduced to room temperature so as to reduce internal stress. And taking the cured product out of the glass container, cutting and polishing to obtain the doped plastic scintillator. However, the plastic scintillators with higher doping amounts, such as 50wt% and 60wt%, are prepared, and the doping compound is precipitated due to excessive doping, and are opaque.
As shown in a in FIG. 5, the X-ray excitation emission spectrum test result shows that the emission peaks in the XEL of the plastic scintillator doped with tributyl phenyl tin are all derived from the wave-shifting agent POPOPOPOP; the 3wt% doping level of XEL is highest compared to undoped plastic scintillators;
as shown in the representation b in figure 5 of the drawings, 137 the scintillation decay time test result under Cs excitation shows that the tributyl phenyl organotin compound doped plastic scintillator still maintains the fast decay characteristic of the traditional plastic scintillator, and the decay time is 4.1ns;
as shown in fig. 5 c, by 137 The result of multi-channel energy spectrum test under Cs excitation shows that with the increase of the doping concentration of tributyl phenyl tin, the scintillation light yield is reduced to some extent compared with that of an undoped plastic scintillator, but the counting rate is increased, and a full energy peak appears;
as shown in a in FIG. 6, the test result of X-ray excitation emission spectrum indicates that the emission peaks in the XEL of the plastic scintillator doped with 2-tributylstannyl thiophene all originate from the wave-shifting agent POPOPOPOPOPOP; and with the increase of the doping concentration of the 2-tributylstannyl thiophene, the XEL intensity is obviously higher than that of the undoped plastic scintillator, wherein the XEL intensity doped by 3wt% is the highest;
as shown in b in figure 6 of the drawings, 137 the scintillation decay time test result under Cs excitation shows that the 2-tributylstannyl thiophene doped plastic scintillator still retains the fast decay characteristic of the traditional plastic scintillator, and the decay time is about 4.1ns;
as shown in c in fig. 6, by 137 The result of multi-channel energy spectrum test under Cs excitation shows that with the increase of the doping concentration of the 2-tributylstannyl thiophene, the scintillation light yield is reduced to some extent compared with that of an undoped plastic scintillator, but the counting rate is increased, and a full energy peak appears;
as shown in FIG. 7 a, the X-ray excitation emission spectrum test results indicate that the emission peak in the XEL doped with 40wt% 2-tributylstannyl thiophene plastic scintillator is derived from the wave-shifting agent coumarin 6;
as shown in b in figure 7 of the drawings, 137 the results of the scintillation decay time test with Cs excitation showed that the plastic scintillator doped with 40wt% 2-tributylstannyl thiophene still retained the fast decay characteristic of conventional plastic scintillators, with a decay time of about 6ns;
the plastic scintillator doped with tributylphenyl tin and 2-tributylstannyl thiophene can be applied to the radiation detection fields of X-ray detection, gamma-ray energy spectrum detection, gamma/neutron discrimination and the like.
Example 3
Example 3 selects the formula as (R) 1 ) x (R 2 ) 4-x One or two of Sn organic tin compounds are doped with different concentrations, wherein R 1 Is a straight-chain or branched alkyl substituent, R 2 Is a halogen-containing substituent and x is an integer between 0 and 4. The tributyl (iodomethyl) stannane contained in the above-mentioned solvent is selected.
The preparation method of the organic tin compound doped plastic scintillator comprises the following steps:
in an inert atmosphere, a matrix monomer (VT), an Initiator (AIBN), a primary fluorescent dye (PPO), a wave-shifting agent (popp), and tributyl (iodomethyl) stannane (0-20 wt%, for example, 0wt%, 10wt%, 20 wt%) with different doping amounts were added to a cleaned and dried glass reaction vessel and dissolved at normal temperature or by ultrasound to obtain a uniform solution system. After the glass reaction vessel was sealed, it was put into an oil bath to heat it to a prescribed polymerization temperature and polymerization was carried out with keeping the temperature for several days. The doping amount of less than 10wt% is usually selected to polymerize at 40-80 ℃ for three weeks, and high doping may take longer. After the polymerization is finished, the temperature is slowly reduced to room temperature so as to reduce internal stress. And taking the cured product out of the glass container, cutting and polishing to obtain the doped plastic scintillator. The tributyl (iodomethyl) stannane-doped plastic scintillator can be applied to the radiation detection fields of X-ray detection, gamma-ray energy spectrum detection, gamma/neutron discrimination and the like.
Example 4
This example 4 selects the formula (R) 1 ) x (R 2 ) 4-x One or two of Sn organic tin compounds are doped with different concentrations, wherein R 1 Is a straight-chain or branched alkyl substituent, R 2 Is a substituent containing an ester group or a carbonyl group, and x is an integer of 0 to 4. Specifically, dibutyltin diacetate contained in the catalyst is selected.
The preparation method of the organic tin compound doped plastic scintillator comprises the following steps:
in an inert atmosphere, a matrix monomer (VT), a primary fluorescent dye (PPO), a wave-shifting agent (popp) and dibutyltin diacetate (0-20 wt%, such as 0wt%, 6wt%, 10wt%, 20 wt%) with different doping amounts are added into a cleaned and dried glass reaction vessel to be dissolved at normal temperature or by ultrasound, so as to obtain a uniform solution system. After the glass reaction vessel was sealed, it was put into an oil bath to be heated to a prescribed polymerization temperature and polymerization was carried out while maintaining the temperature for several days. The amount of the polymer to be doped is 10wt% or less, and the polymer is usually polymerized at 40-70 ℃ for three weeks, while the amount of the polymer to be doped is high (20 wt%) and polymerized at 90 ℃ for one month. After the polymerization is finished, the temperature is slowly reduced to room temperature so as to reduce internal stress. And taking the cured product out of the glass container, cutting and polishing to obtain the doped plastic scintillator.
As shown in a in fig. 9, the X-ray excitation emission spectrum test result indicates that the emission peaks in XEL of the plastic scintillator doped with dibutyl organotin diacetate are all derived from the wave-shifting agent popp; wherein the XEL intensity of 6wt% dibutyltin diacetate doped plastic flash is obviously higher than that of an undoped plastic scintillator;
as shown in b in figure 9 of the drawings, 137 the scintillation decay time test result under Cs excitation shows that the dibutyl organotin diacetate doped plastic scintillator still maintains the fast decay characteristic of the traditional plastic scintillator, and the decay time is 3.6ns;
as shown in fig. 9 c, by 137 The result of multi-channel energy spectrum test under Cs excitation shows that with the increase of the doping concentration of dibutyltin diacetate, the scintillation light yield is reduced to a certain extent compared with that of an undoped plastic scintillator, but the counting rate is increased, and a full energy peak appears; the dibutyltin diacetate doped plastic scintillator can be applied to the radiation detection fields of X-ray detection, gamma-ray energy spectrum detection, gamma/neutron discrimination and the like.
Example 5
This example 5 selects the formula (R) 1 ) 3 (R 2 ) An organotin compound of Sn wherein R 1 Is butyl, R 2 Is one of a linear or branched substituent containing an unsaturated bond, a substituent containing a benzene ring or an aromatic heterocyclic ring, a substituent containing halogen, and a substituent containing an ester group or a carbonyl group. Specifically, the same doping amount is selected to be 10wt%,different structures of organotin compounds were used to prepare plastic scintillators and the differences in properties were compared.
The preparation method of the organic tin compound doped plastic scintillator comprises the following steps:
in an inert atmosphere, adding a matrix monomer (VT), a primary fluorescent dye (PPO), a wave-shifting agent (POPOPOP) and 10wt% of organic tin compounds (propenyl tributyltin, 2- (tributylstannyl pyridine), 2- (tributylstannyl) thiophene, 2- (tributylstannyl) furan and tributyl (iodomethyl) stannane) with doping amount into a cleaned and dried glass reaction container for normal temperature or ultrasonic dissolution to obtain a uniform solution system. After the glass reaction vessel was sealed, it was put into an oil bath to heat it to a prescribed polymerization temperature and polymerization was carried out with keeping the temperature for several days. Polymerization at 50-100 ℃ for ten days is usually selected under the condition of 10wt% doping amount without adding an initiator. After the polymerization is finished, the temperature is slowly reduced to room temperature so as to reduce internal stress. And taking the cured product out of the glass container, cutting and polishing to obtain the doped plastic scintillator.
As shown in a in fig. 11, the X-ray excitation emission spectrum test result shows that the emission peaks in XEL of different organic tin compound-doped plastic scintillators are all derived from the wave-shifting agent popp;
as shown in fig. 11 b, by 137 The multi-channel energy spectrum test result under Cs excitation shows that different organic tin compounds have different influences on the light yield, but the counting rate of the plastic scintillator is improved due to the doping of the tin compounds, and a full energy peak appears;
the doped plastic scintillator can be applied to the radiation detection fields of X-ray detection, gamma-ray energy spectrum detection, gamma/neutron discrimination and the like.
Example 6
In this embodiment 6, an organotin compound-doped plastic scintillator is prepared by an injection molding method, and any one of the organotin compound-doped plastic scintillators in the above structures may be selected as a solid material or a mixed pre-polymerized resin. Specifically, the tributyltin methacrylate doped plastic scintillator is selected.
The preparation of the organotin compound-doped plastic scintillator by the injection molding method comprises the following steps:
in an inert atmosphere, mixing a plastic substrate, an initiator, a cross-linking agent, a fluorescent dye and an organic tin compound, sealing the mixture, and heating and polymerizing the mixture to obtain the solid material of the tributyltin methacrylate-doped plastic scintillator. In an inert atmosphere, the prepared solid material is added into a hopper of an injection molding machine, and a mold is screwed by a mold closing device. Under the action of a heater at 150 ℃, the solid materials added into the machine barrel are fully heated to be in a molten state through the rotation of the screw, and are further uniformly mixed, then the mixture is conveyed to the front end of the machine barrel and is injected into the die cavity from a pouring gate through the main runner and the sub-runners. And (3) keeping the pressure for 5min after the molten resin is filled in the die cavity, cooling and forming the molten resin, and taking out the prepared tributyltin methacrylate plastic scintillator product through a demoulding device and an ejection device.
The tributyltin-doped methacrylate plastic scintillator can be applied to the radiation detection fields of X-ray detection, gamma-ray energy spectrum detection, gamma/neutron discrimination and the like.
Example 7
In this embodiment 7, the plastic scintillator doped with an organotin compound is prepared by an extrusion molding method, and any organotin compound in the above structures may be selected to dope the solid material of the plastic scintillator or the mixed pre-polymerized resin. Specifically, the tributyltin methacrylate doped plastic scintillator is selected.
The preparation of the organic tin compound-doped plastic scintillator by the extrusion method comprises the following steps:
in an inert atmosphere, mixing a plastic substrate, an initiator, a cross-linking agent, a fluorescent dye and an organic tin compound, sealing, heating and polymerizing to obtain a solid material of the tributyltin methacrylate-doped plastic scintillator. Adding the prepared solid material into a hopper of an extruder in an inert atmosphere, fully heating the solid material added into a machine barrel to be in a molten state under the action of a heater at 150 ℃, further uniformly mixing, conveying the solid material to the front end of the machine barrel, extruding plastic from a circular die with the diameter of 5mm under the extrusion action, and cooling for 5min to obtain a cylindrical plastic scintillator product with the diameter of 5mm, wherein the cylindrical plastic scintillator product is continuously extruded and molded.
The tributyltin-doped methacrylate plastic scintillator can be applied to the radiation detection fields of X-ray detection, gamma-ray energy spectrum detection, gamma/neutron discrimination and the like.
Claims (11)
1. An organotin compound-doped plastic scintillator, comprising: plastic matrix, initiator, cross-linking agent, fluorescent dye and organic tin compound;
the content of the initiator in the organic tin compound doped plastic scintillator is 0-1 wt%;
the content of the fluorescent dye is 0.01-30 wt%;
the content of the cross-linking agent is 0-10 wt%;
the content of the organic tin compound is 0.1-60 wt%.
2. The organotin compound-doped plastic scintillator as claimed in claim 1, wherein the organotin compound has the general structural formula (R) 1 ) x (R 2 ) 4-x Sn, wherein x is 0, 1, 2, 3, or 4;
R 1 is a straight or branched alkyl substituent, preferably at least one selected from the group consisting of methyl, ethyl, propyl, butyl, isopropyl and tert-butyl;
R 2 is at least one of a straight chain or branched chain substituent containing an unsaturated bond, a substituent containing a benzene ring or an aromatic heterocyclic ring, a substituent containing halogen, a substituent containing an ester group or a carbonyl group.
3. The organotin compound-doped plastic scintillator as claimed in claim 2, wherein the unsaturated bond-containing straight or branched substituent is at least one selected from the group consisting of vinyl group, propenyl group, 3-methyl-2-butenyl group, propynyl group, alkynyl group, 1-ethoxyvinyl group, cis-butyldiacetic group, acrylate ester, methyl methacrylate, vinyl methacrylate and furfuryl methacrylate;
the substituent containing the benzene ring or the aromatic heterocyclic ring is selected from at least one of phenyl, benzyl, phenethyl, phenylpropyl, furyl, thienyl, thiazolyl, imidazolyl, pyridyl, oxazolyl, styryl and methyl styryl;
the halogen-containing substituent is selected from at least one of fluorine, chlorine, bromine, iodine and iodomethyl;
the substituent containing the ester group or the carbonyl group is at least one selected from 2-ethyl-hexyl group, ethyl ester group, propyl ester group, 2, 4-pentanedionato, and 2, 6-tetramethyl-3, 5-heptanedionato.
4. The organotin compound-doped plastic scintillator as claimed in any one of claims 1 to 3, characterized in that the plastic matrix is polymerized from matrix monomers containing active groups having unsaturated bonds; preferably selected from polymers synthesized from monomers containing vinyl groups and/or polymers synthesized from monomers containing terephthalate groups; more preferably at least one of polystyrene, polyvinyltoluene, poly (9-vinylcarbazole), polymethyl methacrylate and polyethylene terephthalate.
5. The organotin compound-doped plastic scintillator as claimed in any one of claims 1 to 4, wherein the initiator is selected from at least one of azo-type initiators, peroxide-type initiators and photoinitiators, preferably from at least one of azobisisobutyronitrile, azobisisovaleronitrile, azobisisoheptonitrile, benzoyl peroxide tert-butyl peroxide, methyl ethyl ketone peroxide, photoinitiators 184, photoinitiator BAPO.
6. The organotin compound-doped plastic scintillator as claimed in any one of claims 1 to 5, wherein the crosslinking agent is at least one selected from a substance having a plurality of functional groups in a molecule and a compound having a plurality of unsaturated double bonds in a molecule; preferably at least one selected from divinylbenzene, ethylene glycol dimethacrylate and bisphenol A dimethacrylate.
7. The organotin compound-doped plastic scintillator as claimed in any one of claims 1 to 6, characterized in that the fluorescent dye comprises a primary fluorescent dye and/or a wave-shifting agent;
the primary fluorescent dye is selected from at least one of 2, 5-diphenyl oxazole, p-terphenyl, 2- (4 '-tert-butylbenzene) -5- (4' -biphenyl) -1,3, 4-oxadiazole and 2- (4-biphenyl) -5-phenyl oxadiazole;
the wave-shifting agent is at least one selected from 1, 4-bis (5-phenyl-2-oxazolyl) benzene, 1, 4-bis (2-methyl styryl) benzene, 1, 4-bis (4-methyl styrene) benzene, 9, 10-diphenyl anthracene, coumarin 6 and 7-diethylamino-4-methyl coumarin.
8. A method for producing an organotin compound-doped plastic scintillator described in any one of claims 1 to 7, which comprises:
(1) In an inert atmosphere, mixing a monomer, an initiator, a cross-linking agent, a fluorescent dye and an organic tin compound of a plastic substrate to obtain a mixed solution;
(2) And sealing the mixed solution, and polymerizing for 1-4 weeks at 40-120 ℃ to obtain the organic tin compound doped plastic scintillator.
9. A method for producing an organotin compound-doped plastic scintillator described in any one of claims 1 to 7, which comprises:
(1) In an inert atmosphere, mixing a monomer of a plastic substrate, an initiator, a cross-linking agent, a fluorescent dye and an organic tin compound, sealing the mixture, and heating for polymerization to obtain a solid material of the plastic scintillator doped with the organic tin compound; then adding the solid material of the plastic scintillator doped with the organic tin compound into a hopper of an injection molding machine, and screwing a mold by using a mold closing device;
(2) Under the action of a heater, the solid materials in the machine barrel are fully heated under the action of the rotation of the screw and the shearing force to obtain the resin in a molten flowing state;
(3) Conveying the molten resin to the front end of the machine barrel through the rotation of the screw, continuously conveying the molten resin under the action of pressure, and injecting the molten resin into a mold cavity from a pouring gate through a main runner and a branch runner;
(4) And (3) after the mold cavity is filled with the resin, maintaining the pressure for a certain time to cool and mold the organic tin compound doped plastic scintillator, and taking out the organic tin compound doped plastic scintillator through a demolding device and an ejection device.
10. A method for producing an organotin compound-doped plastic scintillator as defined in any one of claims 1 to 7, which comprises:
(1) In an inert atmosphere, mixing a monomer of a plastic substrate, an initiator, a cross-linking agent, a fluorescent dye and an organic tin compound, sealing the mixture, and heating and polymerizing the mixture to obtain a solid material of the plastic scintillator doped with the organic tin compound; then adding the solid material of the plastic scintillator doped with the organic tin compound into a hopper of an extruder, and installing an extrusion die with a certain shape at the end of an extrusion die;
(2) Under the action of a heater, the solid materials in the machine barrel are fully heated through the rotation of the screw and the action of shearing force, and the molten resin is obtained;
(3) The resin in a molten state is conveyed to the front end of a machine barrel through the rotation of a screw, and is extruded and molded continuously through an installed extrusion die under the extrusion action of a screw or a plunger of an extruder to obtain an organic tin compound doped plastic scintillator product.
11. Use of an organotin compound-doped plastic scintillator as claimed in any of claims 1 to 7 in the field of radiation detection, characterized in that the field of radiation detection comprises: x-ray detection, gamma ray spectroscopy detection, and neutron/gamma pulse shape discrimination.
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