CN101738631A - Lithium iodide scintillation probe and preparation method thereof - Google Patents
Lithium iodide scintillation probe and preparation method thereof Download PDFInfo
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- CN101738631A CN101738631A CN200910247353A CN200910247353A CN101738631A CN 101738631 A CN101738631 A CN 101738631A CN 200910247353 A CN200910247353 A CN 200910247353A CN 200910247353 A CN200910247353 A CN 200910247353A CN 101738631 A CN101738631 A CN 101738631A
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Abstract
The invention discloses a lithium iodide scintillation probe and a preparation method thereof. The lithium iodide scintillation probe comprises a scintillation component, a metal box, an optical window, a light guide, a photodetector and a slowing-down body, wherein the top surface and the side face of the scintillation component are coated with a mixed layer of a reflecting material and a sealing material, and the thickness of the mixed layer is 200-800mum. The preparation method of the lithium iodide scintillation probe comprises the following steps of: forming the mixed layer by enabling a lithium iodide crystal which has diffusely reflecting surfaces at the top and sides and a polished light emitting face to contact the material of the mixed layer, then coupling the light emitting face of the crystal and the optical window, sealing in the metal box, coupling the optical window and the photodetector by the light guide and afterwards sealing in the slowing-down body. The method solves the problems of deliquescence and attenuation of the lithium iodide crystal, and the prepared lithium iodide scintillation probe has good humidity resistance, sensitive measurement, low detection lower limit, favorable signal-to-noise ratio, high attenuation prevention performance and long service life.
Description
Technical field
The present invention relates to a kind of lithium iodide scintillation probe and preparation method thereof.
Background technology
The number of neutron and the measurement of energy are had a wide range of applications at aspects such as modern industry, medical treatment, military affairs and securities.Yet the neutron neutral can not cause effects such as ionization, does not produce direct observable effects, and the detection of neutron can be surveyed the product of reaction by the interaction of neutron homoatomic nuclear.At present, utilize neutron usually and contain
3He,
6Li,
10B,
155Gd,
157Gd,
235U,
239The method of the material generation nuclear reaction of nucleic such as Pu is measured indirectly, for example:
n+
6Li→
4He+
3H??Q＝4.78Mev?σ＝940λ/1.8barns
Neutron detector commonly used have He-3 proportional counter tube, BF3 proportional counter tube, LiF thermoluminescence sheet,
6Li glass etc.Wherein, He-3 proportional counter tube and BF3 proportional counter tube all have defectives such as volume is big, detection efficiency is low.In recent years, the lithium iodide neutron detector because of have capture cross-section big (σ=940 λ/18barns), photoyield height (11000ph/Mev), detection efficiency height, counting rate height, volume be little, can with advantage such as photodiode coupling, be subjected to people's attention.
The lithium iodide neutron detector mainly comprises parts such as lithium iodide scintillation device, photoconduction, photo-detector and slow body, and its measuring principle is: neutron enters lithium iodate crystal after the slow body slowing down, in the crystal
6Li and neutron ray generation nuclear reaction, produce a particle carry energy and
3The H particle through exciting and de excitation, produces visible light, is converted to ultra-weak electronic signal through photo-detector then, amplify through prime amplifier again, thereby detect neutron ray, its detected neutron energy range from 0.025ev to hundreds of Mev.Usually recently represent the quality of LiI detector with the noise of prime amplifier output signal, qualified LiI detector signal to noise ratio (S/N ratio) is generally greater than 4: 1.
But, deliquescence and oxidation because lithium iodate crystal very easily absorbs water, this brings great difficulty to crystal processing and device package, and the moisture absorption of lithium iodate crystal can cause crystal property to descend, the signal to noise ratio (S/N ratio) variation, conventional processing environment and processing encapsulation means can't thoroughly be dealt with problems.
Summary of the invention
Technical matters to be solved by this invention is to have overcome lithium iodate crystal to descend because of very easily absorb water deliquescence and oxidation meeting cause crystal property, the signal to noise ratio (S/N ratio) variation, and the defective that conventional processing environment and processing encapsulation means can't thoroughly be dealt with problems provides a kind of preparation method and a kind of lithium iodide scintillation probe of lithium iodide scintillation probe.This method can solve lithium iodate crystal deliquescence attenuation problem, and the lithium iodide scintillation probe humidity resistance that makes is good, measurement is sensitive, the detection lower limit is low, signal to noise ratio (S/N ratio) good, the anti-performance that decays improves and long service life.
Lithium iodide scintillation probe of the present invention, it comprises a flicker device, a can, an optical window, a photoconduction, a photo-detector and a slow body, wherein, the end face of this flicker device and side are covered with the mixolimnion of reflecting material and encapsulant, and the thickness of this mixolimnion is 200-800 μ m.
Wherein, this mixed layer is for preventing too thin sealing and the reflex of not having, as if too thick then can be influential to device performance, be thought of as and reach better seal and reflectivity, its thickness is 200-800 μ m, preferable is about 600 μ m.This mixolimnion be overlying on the mode of this flicker device preferable be coating.
Wherein, the encapsulant that should mix in the layer draws through inventor's lot of experiments, on the one hand need prevent moisture air penetration from the outside, should have higher moisture resistance properties and lower moisture transmission, do not contain simultaneously any can deliquescence or infiltrate through the moisture or the solvent of crystal; On the other hand should and crystal between need have high adherence, help forming fast sealing and curing, and the sealing formation temperature can not produce deleterious effect to crystal.Therefore, the sealing material is preferable is in epoxy glue, polyurethane, silicon gel, silicones, polyester, phenolics, acryl resin, Parylene, polyethylene terephthalate, polycarbonate, vinyl chloride and the polyimide one or more.Wherein, when above-mentioned encapsulant is related to polymkeric substance, can uses with the molecular weight relation little, only relevant, general commonly used molecular weight ranges and all can use with the performance of material own.
Wherein, that the reflectivity of the reflecting material of this mixolimnion is preferable is 85-100%, then correspondingly this reflecting material preferable be in aluminium oxide, titanium dioxide, barium sulphate, magnesium oxide and the teflon one or more.What the particle diameter of this reflecting material was preferable is the powder of 30-100nm, and better is about 50nm.
Wherein, what the quality proportioning of encapsulant and reflecting material was preferable in this mixolimnion is 1: 0.1-1: 10, and better is about 1: 5.
Wherein, this flicker device preferable for mixing the europium lithium iodate crystal, can be
6The Li abundance is that 7-99% mixes the europium lithium iodate crystal, and better is
6The Li abundance is that 50-99% mixes the europium lithium iodate crystal, and best is
6The Li abundance is that 90-95% mixes the europium lithium iodate crystal.But the application number of mixing preparation method's REFERENCE TO RELATED people of europium lithium iodate crystal of the present invention is 200910050304.8, and the applying date is patented claim " preparation method of the preparation method of anhydrous lithium iodide and the doped lithium iodide scintillation crystal " preparation on April 30th, 2009.The geomery of described lithium iodate crystal is the conventional geomery that uses in this area, generally can adjust according to the size of whole sensitive detection parts, and it is square, circular or irregularly shaped that its shape can be.
Wherein, the unsealed can in miscellaneous part that lithium iodide scintillation probe of the present invention comprises such as bottom surface, optical window, photoconduction, photo-detector and slow body etc. are this area conventional components, and its connected mode is the conventional connected mode in this area.What lithium iodide scintillation probe connected mode of the present invention was preferable is: this flicker device is sealed in this can, the exiting surface of this flicker device is positioned at the bottom surface of this can, the exiting surface of this flicker device is coupled by optocoupler mixture and this optical window, this optical window is coupled by this photoconduction and this photo-detector, and aforementioned each parts all are sealed in slow body.
Preferably, this can and optical window melting welding sealing-in mutually.
Wherein, this can is the conventional aluminium box that uses in this area, and what the material of this aluminium box was preferable is anodised aluminium, and it stops the little and stable performance of ability to ray.
Wherein, this optocoupler mixture is the conventional kind of using in this area, preferable for epoxy resin optics with in glue, ultra-violet curing optics usefulness glue, silicon gel and the silicone oil one or more; The transmitance of this couplant generally should be greater than 85% (transmission peak wavelength 400-500nm).
Wherein, this optical window is the conventional materials used in this area, and preferable is quartz glass or ultraviolet optics glass; The transmitance of this optical window generally should be greater than 85% (transmission peak wavelength 400-500nm).
Wherein, this photoconduction is the conventional materials used in this area, one or more that preferable is in silicone oil, silicon rubber, organic glass, polystyrene and the glass fibre; The transmitance of this photoconduction generally should be greater than 85% (transmission peak wavelength 400-500nm).When general lithium iodide device size is more consistent with the photo-detector size, generally adopt silicone oil or silicone rubber plate to do photoconduction; And when lithium iodide device size and photo-detector size do not match, generally select for use silicon rubber, organic glass, polystyrene or glass fibre to make appropriate geometry and do photoconduction.
Wherein, this photo-detector is the conventional photo-detector in this area, and preferable is photomultiplier, photodiode, Charge Coupled Device (CCD) imageing sensor (CCD) or avalanche diode (APD).
Wherein, the material of this slow body is the conventional materials used in this area, and preferable is tygon and/or paraffin.This slow body material and thickness those skilled in the art all know adjusting according to concrete scintillation detector demand sensitivity.
The invention still further relates to the preparation method of lithium iodide scintillation probe of the present invention, it comprises the steps: that the lithium iodate crystal that crystal top and side has been formed diffuse surface and exiting surface polishing contacts the formation mixolimnion with the material of mixolimnion, exiting surface and optical window with crystal is coupled then, and be sealed in the can, again optical window is coupled with photo-detector by this photoconduction again, be sealed in afterwards in the slow body, get final product.
Wherein, preferably with optical window also with can melting welding sealing-in.
Wherein, the described preferable use fluid sealant sealing of sealing in being sealed in the can; Described fluid sealant has high moisture-proof, and bonding condition does not influence the performance of scintillator and optocoupler mixture.
Wherein, the material equalization that relates among the preparation method of described lithium iodide scintillation probe is with the described material of aforementioned lithium iodide scintillation probe parts.
Wherein, the lithium iodate crystal that described crystal top and side have formed the polishing of diffuse surface and exiting surface is that the crystal preprocess method of this area routine makes, preferable is made by following method: lithium iodate crystal is cut into target size, the cutting chip is removed in polishing then, polishing forms diffuse surface more afterwards, polishing at last forms exiting surface, gets final product.The equipment of described cutting is this area conventional equipment, and preferable is inner circle cutting machine or scroll saw.The environment of described cutting is the conventional cutting environment in this area, and is preferable for liquid water content is below the 5ppm, can be air, nitrogen, argon gas or vacuum.The liquid coolant of described cutting is the conventional liquid coolant in this area, the preferable mineral oil that is lower than 1ppm for liquid water content.It is this area routine operation that the cutting chip is removed in described polishing, and the preferable mineral oil for using liquid water content to be lower than 1ppm is polished on 2500-5000 purpose sand paper.It is this area routine operation that described polishing forms diffuse surface, and the preferable mineral oil for using liquid water content to be lower than 1ppm is polished on 400-800 purpose sand paper.It is this area routine operation that described polishing residue forms exiting surface, and preferable is to adopt liquid water content to be lower than mineral oil sanding and polishing on 2500-5000 purpose sand paper of 1ppm.
Agents useful for same of the present invention and raw material except that specified otherwise, all commercially available getting.
On the basis of general knowledge known in this field, above-mentioned each technical characterictic optimum condition can combination in any, promptly gets preferred embodiments of the present invention.
Positive progressive effect of the present invention is: preparation method and a kind of lithium iodide scintillation probe that a kind of lithium iodide scintillation probe is provided.This method solves lithium iodate crystal deliquescence attenuation problem, make the lithium iodide scintillation probe humidity resistance that makes good, measure sensitive, detect that lower limit is low, signal to noise ratio (S/N ratio) good, anti-decay performance improves and long service life.
Description of drawings
Fig. 1 is the structural representation of lithium iodide scintillation probe of the present invention; Mark among the figure is respectively: 1 lithium iodate crystal, the end face of 2 crystal, the side of 3 crystal, the mixolimnion of 4 reflecting materials and encapsulant, 5 cans, 6 optocoupler mixture, 7 optical windows, 8 exiting surfaces, 9 photoconductions, 10 photo-detectors, 11 slow bodies.
Fig. 2 measures the signal to noise ratio (S/N ratio) figure of lithium iodide scintillation probe placement after 1 year of embodiment 2 preparations for effect embodiment of the present invention.
Embodiment
Mode below by embodiment further specifies the present invention, but does not therefore limit the present invention among the described scope of embodiments.
As shown in Figure 1, the invention provides a kind of lithium iodide scintillation probe, it mainly comprises flicker device 1, can 5, optical window 7, photoconduction 9, photo-detector 10 and slow body 11, and this flicker device 1 is
6The abundance of Li be 90% mix the europium lithium iodate crystal, the end face 2 of flicker device 1 and the mixolimnion 4 that side 3 is covered with reflecting material and encapsulant, the thickness of mixolimnion 4 is 600 μ m; Wherein, encapsulant is an epoxy glue, and reflector material is a teflon, and particle size is 50nm, and encapsulant and reflecting material mass ratio are 1: 5; Flicker device 1 is sealed in the can aluminium box 5 that anodised aluminium makes, the exiting surface 8 of flicker device 1 is positioned at the bottom surface of can 5, the exiting surface 8 of flicker device 1 is coupled with glue 6 and optical window quartz glass 7 by optocoupler mixture epoxy resin optics, can 5 and optical window 7 melting welding sealing-in mutually, optical window 7 is coupled by photoconduction silicone rubber plate 9 and photo-detector photoelectricity multiplier tube 10, and each parts all is sealed in the slow body 11 that polythene material makes.
Prepare above-mentioned lithium iodide scintillation probe, its preparation method is as follows:
(1) in dry air and moisture are processing environment below the 5ppm, adopt the inner circle cutting machine will
6The abundance of Li is that (this preparation method's application reference of mixing the europium lithium iodate crystal number is 200910050304.8 for about 90% the europium lithium iodate crystal of mixing, the applying date is patented claim " preparation method of the preparation method of anhydrous lithium iodide and the doped lithium iodide scintillation crystal " preparation on April 30th, 2009), the cutting liquid coolant is the mineral oil that water cut is lower than 1ppm; The crystal by adopting water cut is lower than mineral oil frosted on 2500 purpose sand paper of 1ppm after will cutting afterwards, removes cutting damage and chip;
(2) mineral oil that crystal top and face is lower than 1ppm with water cut carries out frosted on 400 order sand paper, forms diffuse surface; The mineral oil that the exiting surface of lithium iodate crystal is lower than 1ppm with water cut polishes on 1200 order sand paper again, removes the polishing residue simultaneously;
(3) the mixture process formation thickness with crystal top and side employing coating encapsulant and reflecting material is the mixolimnion of the even compact of 600 μ m; Wherein, encapsulant is an epoxy glue, and reflector material is a teflon, and particle size is 50nm, and encapsulant and reflecting material mass ratio are 1: 5;
(4) the crystal exiting surface is coupled with glue and optical window quartz glass by optocoupler mixture epoxy resin optics; Then crystal is used fluid sealant to be sealed in the metallic aluminium box, and the fluid sealant bonding is used in the junction of can and optical window;
(5) and then with the optical window quartz glass be coupled by photoconduction silicone rubber plate and photo-detector photoelectricity multiplier tube, be sealed in the slow body that the polythene material of relative size makes, get final product.
Embodiment 2
A kind of lithium iodide scintillation probe, the annexation of its each parts and preparation method's step are all with embodiment 1, and specifically use the material of parts to be: lithium iodate crystal is
6The abundance of Li be about 7% mix the europium lithium iodate crystal, encapsulant is polyurethane and 1: 1 potpourri of polyethylene terephthalate mass ratio, reflecting material is the aluminium oxide of particle diameter 30nm, encapsulant and reflecting material mass ratio are 1: 0.1, mixolimnion thickness is 200 μ m, the optocoupler mixture is ultra-violet curing optics glue, optical window is a ultraviolet optics glass, photoconduction is a silicone oil, photo-detector is the Charge Coupled Device (CCD) imageing sensor, except that the material of above stated specification, other materials is also with embodiment 1.
A kind of lithium iodide scintillation probe, the annexation of its each parts and preparation method's step are all with embodiment 1, and specifically use the material of parts to be: the optocoupler mixture as silicon gel, lithium iodate crystal is
6The abundance of Li is about 7% to mix the europium lithium iodate crystal, encapsulant is silicones and 1: 1 potpourri of acryl resin mass ratio, reflecting material is the barium sulphate of particle diameter 100nm, encapsulant and reflecting material mass ratio are 1: 10, and mixolimnion thickness is 800 μ m, and photoconduction is a glass fibre, photo-detector is a photodiode, the slow body material is tygon and 1: 1 potpourri of paraffin mass ratio, and except that the material of above stated specification, other materials is also with embodiment 1.
A kind of lithium iodide scintillation probe, the annexation of its each parts and preparation method's step are all with embodiment 1, and specifically use the material of parts to be: encapsulant as silicon gel, lithium iodate crystal is
6The abundance of Li be about 95% mix the europium lithium iodate crystal, reflecting material is the titanium dioxide of particle diameter 50nm, encapsulant and reflecting material mass ratio are 1: 5, mixolimnion thickness is 600 μ m, and the optocoupler mixture is a silicone oil, and photoconduction is an organic glass, photo-detector is an avalanche diode, the slow body material is a paraffin, and except that the material of above stated specification, other materials is also with embodiment 1.
A kind of lithium iodide scintillation probe, the annexation of its each parts and preparation method's step are all with embodiment 1, and specifically use the material of parts to be: reflecting material is titanium oxide powder, and lithium iodate crystal is
6The abundance of Li be about 70% mix the europium lithium iodate crystal, encapsulant is Parylene, polyimide and 1: 1: 1 potpourri of polyester mass ratio, reflecting material is particle diameter 40nm, encapsulant and reflecting material mass ratio are 1: 4, and mixolimnion thickness is 400 μ m, and the optocoupler mixture is a silicone oil, photoconduction is a polystyrene, photo-detector is an avalanche diode, and except that the material of above stated specification, other materials is also with embodiment 1.
A kind of lithium iodide scintillation probe, the annexation of its each parts and preparation method's step are all with embodiment 1, and specifically use the material of parts to be: reflecting material is magnesia powder, and lithium iodate crystal is
6The abundance of Li be about 80% mix the europium lithium iodate crystal, encapsulant is polycarbonate, vinyl chloride and 1: 1: 1 potpourri of phenolics mass ratio, reflecting material is particle diameter 70nm, encapsulant and reflecting material mass ratio are 1: 8, and mixolimnion thickness is 700 μ m, and the optocoupler mixture is a silicone oil, photoconduction is a polystyrene, photo-detector is a photodiode, and except that the material of above stated specification, other materials is also with embodiment 1.
Effect embodiment detects the detector performance that embodiment 1～6 makes
Detector performance detects and uses equipment to be the ORTEC142A charge-sensitive preamplifier, and main putting is ORTEC-570, and enlargement factor is 15 times, is configured as 10 microseconds, and multichannel analyzer is ORTECTRUMP-PCI-8K, and neutron source is that activity is 1 microcurie
252Cf, signal to noise ratio (S/N ratio) is the ratio of neutron Feng Dao location and location, noise negative edge road, can be the test signal to noise ratio (S/N ratio) figure of lithium iodide scintillation probe placement after 1 year of embodiment 2 preparations referring to accompanying drawing 2, the lithium iodide scintillation probe test result that its result and other embodiment make together be recorded in the table 2.
The performance test results of the lithium iodide scintillation probe that table 2 embodiment 1～6 makes
| The embodiment numbering | ??1 | ??2 | ??3 | ??4 | ??5 | ??6 |
| Signal to noise ratio (S/N ratio) | ??6.8 | ??5.7 | ??5.5 | ??6.0 | ??5.8 | ??5.4 |
| Signal to noise ratio (S/N ratio) (after 1 year) | ??6.7 | ??5.7 | ??5.5 | ??5.8 | ??5.7 | ??5.2 |
By the signal to noise ratio (S/N ratio) determination data in the last table 2 as seen, the lithium iodide scintillation probe humidity resistance that the present invention makes is good, places 1 year later signal to noise ratio (S/N ratio) and still keeps good.
Claims (12)
1. lithium iodide scintillation probe, it comprises a flicker device, a can, an optical window, a photoconduction, a photo-detector and a slow body, it is characterized in that: the end face of this flicker device and side are covered with the mixolimnion of reflecting material and encapsulant, and the thickness of this mixolimnion is 200-800 μ m.
2. lithium iodide scintillation probe as claimed in claim 1 is characterized in that: the sealing material is one or more in epoxy glue, polyurethane, silicon gel, silicones, polyester, phenolics, acryl resin, Parylene, polyethylene terephthalate, polycarbonate, vinyl chloride and the polyimide.
3. lithium iodide scintillation probe as claimed in claim 1 or 2 is characterized in that: this reflecting material is one or more in aluminium oxide, titanium dioxide, barium sulphate, magnesium oxide and the teflon; The particle diameter of this reflecting material is 30-100nm.
4. as each described lithium iodide scintillation probe of claim 1～3, it is characterized in that: the quality proportioning of encapsulant and reflecting material is 1 in this mixolimnion: 0.1-1: 10.
5. as each described lithium iodide scintillation probe of claim 1～4, it is characterized in that: this flicker device is
6The Li abundance be 7-99% mix the europium lithium iodate crystal.
6. as each described lithium iodide scintillation probe of claim 1～5, it is characterized in that: the thickness of this mixolimnion is 600 μ m; The particle diameter of this reflecting material is 50nm; The quality proportioning of encapsulant and reflecting material is 1: 5 in this mixolimnion; This flicker device is
6The Li abundance is that 90-95% mixes the europium lithium iodate crystal.
7. as each described lithium iodide scintillation probe of claim 1～6, it is characterized in that: this can and the melting welding sealing-in mutually of this optical window.
8. as each described lithium iodide scintillation probe of claim 1～7, it is characterized in that: this can is the aluminium box, and the material of this aluminium box is an anodised aluminium; This optocoupler mixture for epoxy resin optics with glue, ultra-violet curing optics with in glue, silicon gel and the silicone oil one or more; This optical window is quartz glass or ultraviolet optics glass; This photoconduction is one or more in silicone oil, silicon rubber, organic glass, polystyrene and the glass fibre; This photo-detector is photomultiplier, photodiode, Charge Coupled Device (CCD) imageing sensor or avalanche diode; The material of this slow body is tygon and/or paraffin.
9. preparation method as each described lithium iodide scintillation probe of claim 1～8, it is characterized in that: it comprises the steps: that the lithium iodate crystal that crystal top and side has been formed diffuse surface and exiting surface polishing contacts the formation mixolimnion with the material of mixolimnion, exiting surface and optical window with crystal is coupled then, and be sealed in the can, again optical window is coupled with photo-detector by photoconduction again, be sealed in afterwards in the slow body, get final product.
10. preparation method as claimed in claim 9 is characterized in that: this optical window and can melting welding sealing-in, the fluid sealant sealing is used in described sealing in being sealed in the can.
11. as claim 9 or 10 described preparation methods, it is characterized in that: the lithium iodate crystal that described crystal top and side have formed diffuse surface and exiting surface polishing is made by following method: lithium iodate crystal is cut into target size, the cutting chip is removed in polishing then, polishing forms diffuse surface more afterwards, polishing at last forms exiting surface, gets final product.
12. preparation method as claimed in claim 11 is characterized in that: the equipment of described cutting is inner circle cutting machine or scroll saw; The environment of described cutting is that liquid water content is following air, nitrogen, argon gas or a vacuum of 5ppm; The liquid coolant of described cutting is the mineral oil that liquid water content is lower than 1ppm; Described polishing is removed the cutting chip and is polished on 2500-5000 purpose sand paper for the mineral oil that uses liquid water content to be lower than 1ppm; Described polishing forms diffuse surface and polishes on 400-800 purpose sand paper for the mineral oil that uses liquid water content to be lower than 1ppm; Described polishing residue forms exiting surface and is lower than mineral oil sanding and polishing on 2500-5000 purpose sand paper of 1ppm for adopting liquid water content.
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