CN106054235B - A kind of fast scintillator of composite surface phasmon regulation - Google Patents
A kind of fast scintillator of composite surface phasmon regulation Download PDFInfo
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- CN106054235B CN106054235B CN201610341842.2A CN201610341842A CN106054235B CN 106054235 B CN106054235 B CN 106054235B CN 201610341842 A CN201610341842 A CN 201610341842A CN 106054235 B CN106054235 B CN 106054235B
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- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
- G01T1/16—Measuring radiation intensity
- G01T1/20—Measuring radiation intensity with scintillation detectors
- G01T1/202—Measuring radiation intensity with scintillation detectors the detector being a crystal
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Abstract
The present invention relates to a kind of fast scintillators of composite surface phasmon regulation, including basal layer, arrangement scintillator layers on the base layer, the metallic particles being arranged in scintillator layers and the oxide skin(coating) for being deposited on surface of metal particles, the metallic particles is gold and silver composite particles.Compared with prior art, the surface phasmon that the metallic particles that the present invention is constituted using gold and silver composition metal is formed can effectively realize broadband couple device, the application especially suitable for BGO and CsI:Tl scintillator.
Description
Technical field
The invention belongs to nuclear radiation detection fields, more particularly, to a kind of fast flashing of composite surface phasmon regulation
Body.
Background technique
Scintillation detecter system has important use in fields such as nuclear medicine, weapon physical study, nuclear physics experiments.It dodges
The characteristics of luminescence of bright body determines its ability and usage range of flash detection, is the core devices in detection system.Scintillator
It absorbs the energy of nuclear radiation particle and converts thereof into visible light or black light, the latter is by photodetector such as photomultiplier tube
Or optical diode receives to realize the detection to nuclear radiation.However as detection system further chasing after to time resolution
It asks, fast scintillator becomes the hot spot that people explore New Scintillators.Scintillator development has had more than 100 years history, from point
It is more difficult that son composition and crystal structure angle explore New Scintillators.Regulate and control existing scintillator using micro-nano photonics principle
Die-away time obtains the shorter blinking characteristics time as new developing direction.
Bo Liu et al. people (Applied Physics Letters, 104,061902,2014), which reports, utilizes metallic silver
Particle shape at surface phasmon regulate and control Lu2SiO5: Ce scintillator shines, and obtains the significant regulating and controlling effect of die-away time.Gold
Belong to the resonant wavelength range of the surface phasmon of Argent grain according to its particle size and property, is typically distributed about 350-
450nm range, with Lu2SiO5: the emission wavelength matching of Ce scintillator can play good regulating effect.But for broadband
Scintillator, such as BGO (Bi4Ge3O12) (luminescent spectrum range 400-750nm) and CsI:Tl (luminescent spectrum range 350-
750nm), the resonance bandwidth of the surface phasmon of Argent grain then can not play regulating and controlling effect in the whole bandwidth of scintillator,
The simple fast decay of luminescence adjusting function that cannot achieve BGO and CsI:Tl full bandwidth using silver metal particles.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of composite surface etc. from
The fast scintillator of excimer regulation.The composite construction realizes the extension of regulation bandwidth using gold and silver composite construction.The table of gold particle
The resonant wavelength of face phasmon is generally in the range of 450-1000nm, therefore the composite construction of two kinds of metals of gold and silver can be expanded altogether
Vibration wave-length coverage, meets the fast decaying goal of regulation and control of broadband scintillator BGO and CsI:Tl.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of fast scintillator of composite surface phasmon regulation, including basal layer, the scintillator of arrangement on the base layer
Layer, the metallic particles being arranged in scintillator layers and the oxide skin(coating) for being deposited on surface of metal particles, the metallic particles are
Gold and silver composite particles.
The volume ratio control of gold and silver is 1:1 in the metallic particles, and the width of particle is 80-100nm, and average height is
50nm。
The metallic particles is prepared using following methods: golden film and silverskin alternately are coated with to form period composite membrane
Then layer anneals period composite film by vacuum annealing or nitrogen protection atmosphere, control annealing temperature is 350 DEG C, the time
It is 10 minutes, so that metallic particles is reunited, gold and silver composite particles are prepared.Above-mentioned temperature and time is obtained by many experiments
, it is too high or too low for temperature all to cannot get required particle size, it was advisable within the time 10 minutes, too short, particle is formed not exclusively, mistake
Risk long then that silver oxidation can be generated.
The golden film and silverskin is alternately coated with shape using magnetically controlled sputter method, thermal evaporation method or electron beam evaporation method
At period composite film.
The golden film is identical with the thickness of silverskin, is 3-5nm, and the overall thickness of period composite film is 40nm, then
Heat treatment process will be so that metal agglomeration be at graininess, the height of particle will be above 40nm, reach the 50nm of requirement.
The scintillator layers are BGO scintillation crystal or CsI:Tl scintillation crystal.
The scintillator layers with a thickness of 60-80nm, the range of surface phasmon coupling meets exponential damping law,
Scintillator only within its coupling range will be adjusted, thus the thickness of sample must control this efficient coupling range it
It is interior.The penetration depth Z of metal surface phasmon can be determined using following formula.
Here ε 'sWith ε 'mIt is the real part of the dielectric constant of scintillator layers and metal respectively, λ is the launch wavelength of scintillator.
By calculating, average dielectric constant is used for two kinds of materials of gold and silver, considers further that the bandwidth of launch wavelength, obtains efficient coupling model
Enclose with a thickness of 60-80nm.
The oxide skin(coating) is deposited on surface of metal particles through atomic layer deposition mode, and main function is enhancing metal
Grain sample surfaces adhesive force, can also to avoid silver with air contact when oxidation, acquisition can stablize the sample used.
The material of the oxide skin(coating) is TiO2、Al2O3Or ZnO, these types of material are completely saturating in scintillator luminous spectrum
It is bright, the absorption to scintillator will not be generated.
The oxide skin(coating) with a thickness of 30-50nm.
Compared with prior art, the invention has the following advantages that
(1) surface phasmon that the metallic particles constituted using gold and silver composition metal is formed can effectively realize broadband
Coupling, the application especially suitable for BGO and CsI:Tl scintillator.
(2) while the preparation method of metallic particles used by allows two kinds of metals to merge very well, keep its respective
Phasmon feature obtains significant broadening bandwidth.
(3) structure of conformal oxide greatly reinforces the stability of sample mechanically and chemically.
(4) this method can prepare large-area high-quality sample, be conducive to it in the practical application in radiation detection field.
Detailed description of the invention
Fig. 1 is the atomic force microscopy for preparing sample of embodiment 1.
Fig. 2 is the luminescence decay time curve of the excitation of X-rays of embodiment 1.
Fig. 3 is the luminescence decay time curve of the excitation of X-rays of embodiment 2.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
BGO scintillator film is prepared using the impulse laser deposition system of SURFACE company, Germany production.It will clean up
Quartz substrate be put into and prepare chamber, be evacuated down to 1x10-5Torr is then adjusted oxygen pressure to 200m Torr, oxygen stream
It is maintained at 30sccm level.BGO ceramic target is used to prepare raw material.Laser pulse power and sedimentation time are adjusted, it is final to obtain
With a thickness of the BGO scintillator layers of 80nm.The preparation of gold and silverskin is carried out using LLTRP-450 type dual chamber magnetic control sputtering system.Target
Material be purity 99.9% silver plate and 99.9% golden plate.Vacuum degree is 1.5x10-5Torr pours argon gas in coating process, protects
It is horizontal to hold 500m Torr.Discharge voltage is 600V, electric current 500mA when preparing golden film, and discharge voltage is 500V when preparing silverskin,
Electric current 400mA.The time for preparing single layer of gold is 10 seconds, and with a thickness of 5nm, the time for preparing single silver is 15 seconds for acquisition, is obtained thick
Degree is 5nm.Golden film and the alternate periodicity of silverskin are 4, the final thickness for obtaining 40nm.By the film layer sample prepared in nitrogen
The lower annealing of protection obtains the reunion of metallic particles.Annealing temperature is 350 DEG C, and the time is 10 minutes.Utilize model SUNALE R-
200 atomic layer deposition system selects Three-dimensional atom layer depositional mode, in surface of metal particles depositing Ti O2Layer, deposition thickness
For 30nm, operating temperature when deposition is 75 DEG C.
Fig. 1 is the atomic force microscopy for preparing sample, the results showed that the pattern and scale and design of particle coincide.X
The result of the luminescence decay time regulation of ray excitation is as shown in Figure 2.The die-away time for the BGO sample for not having metal structure to regulate and control
Constant is 300ns, and when there is metal structure, we have monitored the luminescence decay time at 400nm and 650nm wavelength respectively, they
Damping time constant be respectively 28ns and 21ns, they have respectively corresponded the surface phasmon that silver and gold generate in particle and have produced
Raw regulating effect.Acquired results and imagination are consistent, have reached desired effect.
Embodiment 2
CsI:Tl scintillator film is prepared using thermal evaporation method system.The silicon wafer cleaned up is put into and prepares chamber,
It is evacuated down to 1x10-5Torr.Raw material is prepared using CsI powder and being mixed into for TlI powder, heating power 300W, it is heavy to adjust
Product time, the final BGO scintillator layers obtained with a thickness of 60nm.Gold is carried out using LLTRP-450 type dual chamber magnetic control sputtering system
With the preparation of silverskin.Target be purity 99.9% silver plate and 99.9% golden plate.Vacuum degree is 1.5x10-5Torr, plated film mistake
Argon gas is poured in journey, keeps 500m Torr horizontal.Discharge voltage is 600V, electric current 500mA, when preparing silverskin when preparing golden film
Discharge voltage is 500V, electric current 400mA.The time for preparing single layer of gold is 8 seconds, obtains with a thickness of 4nm, prepares the time of single silver
It is 8 seconds, obtains with a thickness of 4nm.Golden film and the alternate periodicity of silverskin are 5, the final thickness for obtaining 40nm.The film that will be prepared
Layer sample is annealed under nitrogen protection obtains the reunion of metallic particles.Annealing temperature is 350 DEG C, and the time is 10 minutes.Utilize type
Number be SUNALE R-200 atomic layer deposition system, select Three-dimensional atom layer depositional mode, surface of metal particles deposit
TiO2Layer, deposition thickness 50nm, operating temperature when deposition are 75 DEG C.
The result of the luminescence decay time regulation of excitation of X-rays is as shown in Figure 3.The CsI:Tl sample for not having metal structure to regulate and control
The damping time constant of product is 1000ns, and when there is metal structure, we have monitored shining at 450nm and 600nm wavelength respectively
Die-away time, their damping time constant are respectively 80ns and 63ns, they have respectively corresponded what silver and gold in particle generated
The regulating effect that surface phasmon generates.Acquired results and imagination are consistent, have reached desired effect.
Embodiment 3
A kind of fast scintillator of composite surface phasmon regulation, including basal layer, the scintillator of arrangement on the base layer
Layer, the metallic particles being arranged in scintillator layers and the oxide skin(coating) for being deposited on surface of metal particles.
Wherein, metallic particles is gold and silver composite particles, and the volume ratio control of gold and silver is 1:1, and the width of particle is 80nm, is put down
Height is 50nm.
Metallic particles is prepared using following methods: the golden film and silverskin for being 3nm for thickness are using magnetron sputtering side
Method alternately is coated with to form the period composite film that overall thickness is about 40nm, then by period composite film by vacuum annealing or
Nitrogen protection atmosphere annealing, control annealing temperature are 350 DEG C, and the time is 10 minutes, so that metallic particles is reunited, thickness is prepared
In 50nm or so gold and silver composite particles.Above-mentioned temperature and time is obtained by many experiments, too high or too low for temperature all to obtain
Less than required particle size, it was advisable within the time 10 minutes, too short, particle is formed not exclusively, and it is too long, the wind of silver oxidation can be generated
Danger.
The scintillator layers used are BGO scintillation crystal, and with a thickness of 60nm, the range of surface phasmon coupling meets index
Attenuation law, the only scintillator within its coupling range will be adjusted, therefore the thickness of sample must control herein effectively
Within coupling range.The penetration depth Z of metal surface phasmon can be determined using following formula.
Here ε 'sWith ε 'mIt is the real part of the dielectric constant of scintillator layers and metal respectively, λ is the launch wavelength of scintillator.
By calculating, average dielectric constant is used for two kinds of materials of gold and silver, considers further that the bandwidth of launch wavelength, obtains efficient coupling model
Enclose with a thickness of 60nm.
Oxide skin(coating) is deposited on surface of metal particles, material TiO through atomic layer deposition mode2, with a thickness of 30nm.Oxidation
The main function of nitride layer is the oxygen for enhancing metallic particles in the adhesive force of sample surfaces, when can also contact to avoid silver with air
Change, acquisition can stablize the sample used.The material of oxide skin(coating) is that these types of material is fully transparent in scintillator luminous spectrum, no
The absorption to scintillator can be generated.
Embodiment 4
A kind of fast scintillator of composite surface phasmon regulation, including basal layer, the scintillator of arrangement on the base layer
Layer, the metallic particles being arranged in scintillator layers and the oxide skin(coating) for being deposited on surface of metal particles.
Wherein, metallic particles is gold and silver composite particles, and the volume ratio control of gold and silver is 1:1, and the width of particle is 100nm,
Average height is 50nm.
Metallic particles is prepared using following methods: the golden film and silverskin for being 5nm for thickness are using thermal evaporation method
Alternating is coated with to form the period composite film that overall thickness is about 40nm, and period composite film is then passed through vacuum annealing or nitrogen
Gas shielded ambient anneal, control annealing temperature are 350 DEG C, and the time is 10 minutes, so that metallic particles is reunited, thickness, which is prepared, is in
50nm or so gold and silver composite particles.Above-mentioned temperature and time is obtained by many experiments, it is too high or too low for temperature all no
To required particle size, it was advisable within the time 10 minutes, too short, particle is formed not exclusively, and it is too long, the risk of silver oxidation can be generated.
The scintillator layers used are CsI:Tl scintillation crystal, and with a thickness of 80nm, the range of surface phasmon coupling meets
Exponential damping law, the only scintillator within its coupling range will be adjusted, therefore the thickness of sample must control herein
Within the scope of efficient coupling.The penetration depth Z of metal surface phasmon can be determined using following formula.
Here ε 'sWith ε 'mIt is the real part of the dielectric constant of scintillator layers and metal respectively, λ is the launch wavelength of scintillator.
By calculating, average dielectric constant is used for two kinds of materials of gold and silver, considers further that the bandwidth of launch wavelength, obtains efficient coupling model
Enclose with a thickness of 80nm.
Oxide skin(coating) is deposited on surface of metal particles, material ZnO, with a thickness of 50nm through atomic layer deposition mode.Oxidation
The main function of nitride layer is the oxygen for enhancing metallic particles in the adhesive force of sample surfaces, when can also contact to avoid silver with air
Change, acquisition can stablize the sample used.The material of oxide skin(coating) is that these types of material is fully transparent in scintillator luminous spectrum, no
The absorption to scintillator can be generated.
Claims (6)
1. a kind of fast scintillator of composite surface phasmon regulation, which is characterized in that
The metal that the scintillation component includes basal layer, arrangement scintillator layers on the base layer, is arranged in scintillator layers
Grain and the oxide skin(coating) for being deposited on surface of metal particles, the metallic particles are gold and silver composite particles；
The volume ratio control of gold and silver is 1:1 in the metallic particles, and the width of particle is 80-100nm, and average height is
50nm, the metallic particles are prepared using following methods: golden film and silverskin alternately be coated with to form period composite film,
Then period composite film is annealed by vacuum annealing or nitrogen protection atmosphere, control annealing temperature is 350 DEG C, the time 10
Minute, so that metallic particles is reunited, gold and silver composite particles are prepared；
The golden film and silverskin alternately is coated with to form week using magnetically controlled sputter method, thermal evaporation method or electron beam evaporation method
Phase composite film, the golden film is identical with the thickness of silverskin, is 3-5nm, and the overall thickness of period composite film is 40nm.
2. a kind of fast scintillator of composite surface phasmon regulation according to claim 1, which is characterized in that described
Scintillator layers are BGO scintillation crystal or CsI:Tl scintillation crystal.
3. a kind of fast scintillator of composite surface phasmon regulation according to claim 1, which is characterized in that described
Scintillator layers with a thickness of 60-80nm.
4. a kind of fast scintillator of composite surface phasmon regulation according to claim 1, which is characterized in that described
Oxide skin(coating) is deposited on surface of metal particles through atomic layer deposition mode.
5. a kind of fast scintillator of composite surface phasmon regulation according to claim 1, which is characterized in that described
The material of oxide skin(coating) is TiO2、Al2O3Or ZnO.
6. a kind of fast scintillator of composite surface phasmon regulation according to claim 1, which is characterized in that described
Oxide skin(coating) with a thickness of 30-50nm.
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Citations (3)
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| CN103311395A (en) * | 2013-05-08 | 2013-09-18 | 北京大学 | Laser stripping film LED (Light-Emitting Diode) and preparation method thereof |
| CN103869391A (en) * | 2014-03-28 | 2014-06-18 | 明天 | Color reinforcing film, and utilization structure, utilization method and manufacturing method of the color reinforcing film |
| CN104280761A (en) * | 2014-09-25 | 2015-01-14 | 同济大学 | High-light-extraction-efficiency scintillator realized by utilizing surface photon structure |
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2016
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103311395A (en) * | 2013-05-08 | 2013-09-18 | 北京大学 | Laser stripping film LED (Light-Emitting Diode) and preparation method thereof |
| CN103869391A (en) * | 2014-03-28 | 2014-06-18 | 明天 | Color reinforcing film, and utilization structure, utilization method and manufacturing method of the color reinforcing film |
| CN104280761A (en) * | 2014-09-25 | 2015-01-14 | 同济大学 | High-light-extraction-efficiency scintillator realized by utilizing surface photon structure |
Non-Patent Citations (1)
| Title |
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| an approach to achieve significantly faster luminescence decay of thin-film scintillator by surface plasmons;BO LIU et al.;《APPLIED PHYSICS LETTERS》;20140210;第104卷(第6期);1-6页 |
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