CN106154302B - A kind of ray detection flat panel detector scintillator panel and preparation method thereof - Google Patents
A kind of ray detection flat panel detector scintillator panel and preparation method thereof Download PDFInfo
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- CN106154302B CN106154302B CN201510130764.7A CN201510130764A CN106154302B CN 106154302 B CN106154302 B CN 106154302B CN 201510130764 A CN201510130764 A CN 201510130764A CN 106154302 B CN106154302 B CN 106154302B
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Abstract
The present invention relates to a kind of ray detection flat panel detector scintillator panels and preparation method thereof, the scintillator panel includes substrate, scintillator layers and the reflecting layer being clipped between the substrate and scintillator layers, wherein, the constitutional chemistry formula of the scintillator layers is (Lu(1‑x‑y)CexAy)3Al5O12, the alternative ion of A case includes Ca2+、Mg2+、Sr2+、Ba2+、Li+、Na+、K+At least one of, 0.001≤x≤0.05,0.0005≤y≤0.05.(Lu, A) of the invention3Al5O12: Ce crystalline ceramics ray flat panel detector has the characteristics that the sharp keen spatial resolution of imaging is high, and have maintenance cost low, the advantages that long service life and maintenance cost, applied to medical diagnosis, non-destructive testing, public safety, dose of radiation detection and oil exploration etc. using in the device of ray detection.
Description
Technical field
The invention belongs to ray scintillator detector image-forming device fields, and in particular to a kind of plate for ray detection
Scintillator panel in detector and preparation method thereof.The detector is penetrated ray (or particle) such as gamma-rays, β using scintillator panel
Line or X-ray etc. are converted into visible light, it is seen that phot-luminescence power conversion device generates electric current, then imports and be converted into figure in computer
Shape information, to realize the digitized photography of ray spatial distribution.It can be applied to medicine using the detector of the scintillator panel to examine
Disconnected, non-destructive testing, public safety, dose of radiation detection and oil exploration etc. are using in the device of ray detection.
Background technique
X-ray detection X and imaging technique are widely used in medical image, industrial nondestructive testing and airport station safety inspection etc.
Many production and living fields.Most crucial component is detector in ray detection.In recent years, not with medical imaging technology
Disconnected development, proposes the demand of the quick real time imagery of high-resolution to detector.Radiographic real-time imaging based on flat panel detector
Detection technique (Digital Radiography, DR) with its Portable durable, high sensitivity and pattern distortion are small the advantages that become
Real time radiography of new generation.
Currently, ray detection flat panel detector is divided into direct energy conrersion and indirect energy converts two classes, it is based on scintillator
The indirect conversion type flat panel detector of detector image-forming is a kind of most common radiographic techniques.
In this flat panel detector device, in order to convert visible light for ray and use scintillator detector carry out at
Picture.Scintillator employed in commercial flat panel detector is mainly CsI at present.Due to CsI have fusing point it is low, it is easy deliquesce etc. spies
Different physicochemical property, commercial scintillators flat panel detector mostly uses epitaxy to grow CsI columnar fiber film at present.This method is raw
Although long CsI film can effectively improve light collecting efficiency, the CsI film transmission rate using this method preparation is lower,
Preparation process is complicated, higher cost.In addition, due to CsI unstable chemcial property, so that existing in epitaxy growth CsI film
The point defects such as vacancy or vacancy cluster, to influence material luminous efficiency.
The oxide scintillator (Lu, Ce) of cubic garnet structure3Al5O12(LuAG:Ce) have density it is high (ρ=
6.73g/cm3) and the big (Z of effective atomic numbereff=62.9) the advantages of, strong to ray absorption capacity, it is that ideal ray is visited
It measures and monitor the growth of standing timber material.Using crystalline ceramics technology of preparing, the ceramic scintillator excellent with high optical quality luminescent properties can be prepared.Mesh
Before, the alkaline-earth metal Me of our preparations2+(Lu, Ce, the Me) being co-doped with3Al5O12(LuAG:Ce, Me) scintillating ceramic is under 1 μ s gate-width
Photoyield is higher than 22,000ph/MeV, and it is a kind of very potential scintillator that die-away time, fast (~40ns) twilight sunset was low.Simultaneously
We prepare the scintillator panel of surface etch, improve light collection by carrying out microstructure design and processing to crystalline ceramics surface
Efficiency improves scintillator imaging resolution.
Using with high optical quality, (Lu, the A) that luminescent properties are excellent and chemical property is stable3Al5O12: Ce ceramics
As scintillator, to realize that the detection of high sharpness imaging clearly fast-response ray detection plate provides possibility.Chinese patent
It is flat that CN102934172A, CN 102820071A, CN 103563006A and CN 103675885A once reported ray detection
The Device Patent of plate, wherein using scintillator for commercial rare earth halide.Chinese patent CN 1034101C, CN1995274A
The patent about pomegranate feldspar or single crystal scintillator is all reported with CN 103380194A etc., but their deficiency is
The problems such as being matched by the scintillation properties and rear end correlation electronics of material, before not useful garnet ceramic scintillator preparation
The precedent of ray detection flat panel detector.In addition, before in relation to the report of flat panel detector, such as CN103675885A and CN
102820071A etc. largely prepares scintillator layers, also not in scintillator panel by the way of epitaxial growth columnar fiber
It is upper to etch array element to improve the report of detector detection performance.
Summary of the invention
The present invention is directed to further existing ray detection flat panel detectors, and the present invention provides a kind of spies of ray detection plate
Survey device scintillator panel and preparation method thereof.
The present invention provides a kind of ray detection flat panel detector scintillator panel, the scintillator panel includes substrate, dodges
Bright body layer and the reflecting layer being clipped between the substrate and scintillator layers, wherein the constitutional chemistry formula of the scintillator layers is
(Lu(1-x-y)CexAy)3Al5O12, the alternative ion of A case includes Ca2+、Mg2+、Sr2+、Ba2+、Li+、Na+、K+In at least
One kind can may be the mixing of several ions, 0.001≤x≤0.05,0.0005≤y≤0.05 for a kind of ion.
Preferably, A case ion is Mg2+;0.001≤x≤0.01, more preferable 0.002≤x≤0.005;0.0005≤y
≤ 0.01, more preferably 0.001≤y≤0.005.
Preferably, the substrate material includes graphite, resin, glass or metal, the reflecting layer material include silica gel or
Epoxy resin, reflecting layer shines with increase scintillator panel and the effect of fixed substrate and scintillator layers.
Preferably, containing 40~95wt% light diffusing particles SiO in reflector material2Particle.
Preferably, substrate with a thickness of 0.05mm~10mm, reflecting layer with a thickness of 0.01 μm~0.5 μm, scintillator layers
With a thickness of 50 μm~500 μm.
Preferably, substrate with a thickness of 0.05mm~4mm, more preferable 0.5mm~4mm, reflecting layer with a thickness of 0.01 μm
~0.2 μm, scintillator layers with a thickness of 50 μm~200 μm.
Preferably, there are the independent array unit formed by etching, the preferred rectangle of array element, rectangle in scintillator layers surface
The side length of array is 50 μm~200 μm, 10~20 μm of spacing range, 10~50 μm of etching depth.
Also, the present invention also provides a kind of preparation methods of above-mentioned scintillator panel, comprising:
1) solid reaction process or liquid phase method combination ceramic sintering technology, preparation are used according to the constitutional chemistry formula of scintillator layers
Scintillator layers material;
2) scintillator layers material prepared by step 1) is cut into the scintillator layers thin slice of predetermined size;
3) it after fixing scintillator layers thin slice and substrate by reflector material, is polishing to specific thickness and polishes.
Preferably, cross section is rectangle before the polishing of scintillator layers thin slice, 10~50mm of side size range, thickness range 1mm~
4mm;
Before substrate polishing, cross section is rectangle, 20~70mm of side size range, thickness range 1mm~8mm.
Preferably, the preparation method further include:
4) surface for etching the scintillator layers, forms it into array element, wherein the mode of etching include: wire cutting,
Laser cutting or inductively coupled plasma body.
In addition, the present invention also provides a kind of flat panel detector containing above-mentioned scintillator panel, the flat panel detector packet
Include scintillator panel, light cone and electrooptical device.
In addition, the present invention also provides a kind of crystalline ceramics that above-mentioned scintillator panel uses, the composition of the crystalline ceramics
Chemical formula is (Lu(1-x-y)CexAy)3Al5O12, the alternative ion of A case includes Ca2+、Mg2+、Sr2+、Ba2+、Li+、Na+、K+
At least one of, can for a kind of ion may be several ions mixing, 0.001≤x≤0.01,0.0005≤y≤
0.01。
The present invention also provides a kind of preparation methods of above-mentioned crystalline ceramics, comprising:
1) it prepares mixed uniformly comprising luteium oxide, aluminium oxide, cerium oxide and the raw material powder for being co-doped with ion-oxygen compound
Body;
2) biscuit of ceramics will be obtained after material powder molding;
3) by biscuit of ceramics, vacuum-sintering obtains the crystalline ceramics at 1700-1900 DEG C.
Preferably, molding uses dry-pressing formed or cold isostatic compaction, wherein dry-pressing formed done at 50~150MPa
Pressure 1~5 minute, isostatic cool pressing is isostatic cool pressing 1~10 minute at 200~400MPa.
Preferably, the vacuum-sintering is in pressure≤10-210 hours are kept the temperature in 1700~1820 DEG C under the vacuum degree of Pa
More than.
Beneficial effects of the present invention:
(Lu, A) of the invention3Al5O12: Ce crystalline ceramics ray flat panel detector, which has, is imaged sharp keen spatial resolution height
The characteristics of, and have many advantages, such as that maintenance cost is low, long service life and maintenance cost, be applied to medical diagnosis, non-destructive testing,
Public safety, dose of radiation detection and oil exploration etc. are using in the device of ray detection.Pass through the method pair of surface etch
Material microstructure is designed, and can effectively improve system imaging resolution ratio, is suitable for all block scintillator materials.
Detailed description of the invention
The image-forming principle that Fig. 1 shows the flat panel detector prepared using scintillator panel in one embodiment of the present invention is shown
It is intended to;
Fig. 2 shows use (Lu, A) in one embodiment of the present invention3Al5O12: the scintillator of Ce crystalline ceramics preparation
The structural schematic diagram of plate;
Fig. 3 shows (Lu, the A) prepared in one embodiment of the present invention3Al5O12: Ce transparent ceramic scintillator X-ray
The luminescent spectrum of excitation and the identical size BGO monocrystalline of Czochralski grown are the luminous light of the excitation of X-rays of reference sample
Spectrum;
Fig. 4 is shown after the surface etch prepared in one embodiment of the present invention (Lu, A)3Al5O12: Ce crystalline ceramics
The optical microscope photograph of scintillator.
Specific embodiment
The present invention is further illustrated below in conjunction with attached drawing and following embodiments, it should be appreciated that attached drawing and following embodiments
It is merely to illustrate the present invention, is not intended to limit the present invention.
The purpose of the present invention is to provide a kind of preparation methods of indirect conversion type ray detection flat panel detector.Utilize with
LuAG:Ce is the multicomponent garnet (Lu, A) of matrix3Al5O12: Ce crystalline ceramics high optical quality shines superior chemical property
Stable advantage prepares the ray detection flat panel detector with high spatial resolution.In addition, by the way of surface etch pair
Material microstructure is designed, to effectively improve the resolution ratio of the flat panel detector.
In order to achieve the above object, a kind of the technical solution adopted by the present invention are as follows: high spatial resolution ray detection plate
Detector.The ray detection flat panel detector includes scintillator panel, light cone, electrooptical device and computer data acquiring
System.
In the present invention, the device being imaged for ray is known as ray detection flat panel detector.Its feature is indirect
The ray detection flat panel detector of conversion regime.The ray includes gamma-rays, β ray or X-ray etc..
In the present invention, it absorbs ray and is converted into the component of visible light and be known as scintillator panel.It is characterized in that, it
It is made of scintillator layers, reflecting layer and substrate.
In the present invention, the scintillator panel core component is scintillator layers.It is characterized in that, used material can
Think the blocks scintillation materials such as monocrystalline, ceramics or organic matter high-molecular compound.The selection of material is mainly from the stable state of material
Luminous efficiency, transmitance and processing performance etc. consider.Scintillator layers thickness range: 50 μm~500 μm.To improve flashing
The visible light conversion efficiency of body layer, needs to perform etching surface.
In a preferred embodiment of the present invention, the scintillator layers thickness range: 50 μm~200 μm.
In the present invention, by scintillator layers surface etch array element, to optimize the performance of detector.The surface
Etching technics can be wire cutting, laser cutting and inductively coupled plasma body (ICP) etching etc., but be not limited to above-mentioned side
Method.The technique is suitble to carry out microstructure design to monocrystalline, ceramics or organic high molecular compound block scintillator material.
In the present invention, after the surface etch technique, scintillator surface is finally divided into multiple independent battle arrays
Column unit.Etching becomes array element, because the structure can make scintillator surface generate light guide transmission, reduces total reflection loss,
To improve the visible light collecting efficiency of device, increase System spatial resolution.
In the present invention, each independent array element can be designed to different shape according to actual needs.
In a preferred embodiment of the present invention, the etching surface is rectangular array.Array side size range 50 μm~200
μm, 10~20 μm of spacing range.
In a preferred embodiment of the present invention, the material of the scintillator layers is multicomponent garnet (Lu, A)3Al5O12:
Ce crystalline ceramics, chemical composition are (Lu(1-x-y)CexAy)3Al5O12, wherein A is alternative Lu3+The co-dopant ions of case,
Alternative ion has Ca2+、Mg2+、Li+Deng, choose co-dopant ions foundation be that can be made in material by charge compensation
Obtain a certain amount of Ce4+, can may be a variety of co-dopant ions for a kind of co-dopant ions;The value range of x is 0.001
The value range of≤x≤0.05, y are 0.0005≤y≤0.05, preferably 0.0005≤y≤0.01, more preferably 0.001≤y
≤0.005。
In a preferred embodiment of the present invention, (Lu, the A)3Al5O12: the substitutional ion A of Ce crystalline ceramics is Mg2+。
In a preferred embodiment of the present invention, (Lu, the A)3Al5O12: the x value range of Ce crystalline ceramics: 0.001
≤ x≤0.01, more preferable 0.002≤x≤0.005.
In the present invention, support scintillator layers are that the component that scintillator layers work normally is known as substrate.Substrate thicknesses range:
0.05mm~10mm.
In the present invention, the baseplate material can be with are as follows: the structural chemistry property such as graphite, resin, glass and metal
Stable material.
In a preferred embodiment of the present invention, the baseplate material is graphite.Use graphite as baseplate material, density
It is low few to radiation absorption, additionally have many advantages, such as processing performance it is excellent, be easy bonding and it is low in cost.
In a preferred embodiment of the present invention, the substrate thicknesses range: 0.05mm~4mm.
In the present invention, it is reduced visible between scintillator layers and substrate for improving scintillator detector luminous intensity
The component of optical scattering losses is known as reflecting layer.Reflecting layer, which has concurrently, to be increased scintillator panel and shines and fixed substrate and scintillator layers
Effect.Substrate is fixed with scintillator layers by the transparent adhesive in reflecting layer in scintillator panel.After high-energy ray sending, warp
Substrate and reflecting layer in the scintillator panel are crossed, the scintillator layers is reached and absorbs and be converted to visible light.
In the present invention, reflecting layer is dispersed in transparent adhesive by light diffusing particles and is constituted.Reflector thickness range:
0.01 μm~0.5 μm.Transparent adhesive can be silica gel or epoxy resin.
In a preferred embodiment of the present invention, the transparent adhesive that the reflecting layer is selected is silica gel.Made using silica gel
For transparent adhesive, because it has many advantages, such as that absorption property is high, thermal stability is good, chemical property is stable, mechanical strength is higher.
In a preferred embodiment of the present invention, the light diffusing particles that the reflecting layer is selected are SiO2Particle.Because of its tool
There is the higher feature of refractive index, improve reflecting layer reflectivity, reduces the luminous loss of scintillator layers, improve the resolution ratio of imaging.
In a preferred embodiment of the present invention, the reflector thickness range: 0.01 μm~0.2 μm.
In the present invention, the scintillator panel is obtained by scintillator layers, reflecting layer and substrate are fixed.
In the present invention, collect scintillator issue visible light and be conducted into electrooptical device can there are two types of design
Mode.First, design pattern is combined using traditional optical lens, completes light importing by being designed to optical path.Using this
Mode is in order to improve optical path anti-radiation performance, so that system structure complexity light transmissioning efficiency is low, system imaging resolution ratio is poor.The
Two, directlying adopt light cone as transmission intermediary then can effectively improve system imaging resolution ratio to avoid problem above.
In a preferred embodiment of the present invention, light cone used in the flat panel detector.Because its light collecting efficiency is high,
It is coupled with the photovoltaic converter of rear end, imaging resolution is high.
In the present invention, it will be seen that the device that light is converted into electric signal is known as electrooptical device.
In the present invention, electrooptical device can select photodiode, charge coupled cell (CCD), complementary metal
Oxide semiconductor (CMOS) or photomultiplier tube (PMT) etc., but it is not limited to above-mentioned device.
In a preferred embodiment of the present invention, electrooptical device used in the flat panel detector is CCD.
It utilizes (Lu, A)3Al5O12: the feature that Ce crystalline ceramics optical quality is good, luminous efficiency is high, the flat panel detector
Image quality is high under excitation of X-rays, and apparent is sharp keen.Use spongy lead to block-regulations test 10lp/mm under MTF 17.5% with
On.Use knife-edge method test selection criteria IEC62220-1 specified in RQA5 experiment condition carry out test MTF be 10% when, divide
Resolution is in 9lp/mm or more.Garnet crystalline ceramics chemical stability is good, can effectively improve detector service life, reduces
Device encapsulation and maintenance cost.The higher thermal conductivity of ceramics and heat-sinking capability can conveniently be applied to different use environments, especially
It is some environment for needing high-temperature operation, such as oil well exploration.
The present invention provides a kind of ray detection flat panel detector, structural schematic diagram and spatial resolution test philosophy
As shown in Figure 1.Referring to Fig. 1, the flat panel detector includes scintillator panel, light cone, CCD and subsequent data collecting card computer
Deng composition.Illustrate emergent ray after light source issues in Fig. 1, by (Lu, A)3Al5O12: Ce transparent ceramic scintillator plate is converted to
Visible light.Visible light enters CCD through light-cone QCD sum rules and is converted to electric signal, acquires analog imaging photo through computer.
In the present invention, the flat panel detector X-ray carries out imaging system test.Knife-edge method tests selection criteria
RQA5 experiment condition specified in IEC62220-1 carry out test MTF be 10% when, resolution ratio is in 9lp/mm or more.
To sum up, the present invention provides a kind of indirect conversion type ray inspection using scintillator as radiation absorption and conversion medium
The preparation method of master plate detector.Under ray excitation, (Lu, A)3Al5O12: Ce transparent ceramic scintillator issues central wavelength
For the visible light of 510nm.Such visible light is imaged after being detected by subsequent photoelectric converter through computer simulation show.The scintillator
For flat panel detector since used ceramic scintillator luminous intensity is high, twilight sunset is low, the sharp keen spatial resolution of system imaging is high.This
Outside, since ceramic machinery is had excellent performance, have the advantages that machinability is good, be easy to perform etching surface processing.Ceramics etching
Afterwards, ceramic surface generates waveguide transmission, reduces total reflection loss, to improve the visible light collecting efficiency of device, it is empty to increase system
Between resolution ratio.Therefore, the present invention can effectively solve to encounter in the development of current flat panel detector due to commercial at present non-oxide
The problems such as maintenance cost caused by object scintillator unstable chemcial property is high, preparation process is complicated.It is produced using with independent intellectual
Power, optical quality excellent (straight line transmittance > 73% at 2mm thickness ceramics 800nm) and luminous intensity height (more than 7.5 times BGO)
(Lu,A)3Al5O12: Ce crystalline ceramics is prepared for having the plate of high spatial resolution (> 9lp/mm) to detect as scintillator
Device.The flat panel detector has many advantages, such as that maintenance is simple simultaneously, and thermal stability is good.
On the other hand, the present invention also provides the preparation methods of the transparent ceramic scintillator plate, comprising: according to crystalline ceramics
The chemical composition of scintillator prepares transparent ceramic scintillator using solid reaction process or liquid phase method combination ceramic sintering technology;By institute
The crystalline ceramics block processing of preparation is cut into the scintillator of certain size;The transparent ceramic scintillator is led to baseplate material
Reflecting layer is crossed to fix;By the multi-layer compound structure sanding and polishing to certain thickness;And by scintillator in the composite construction
Layer is cut into rectangular array.
The preparation method of crystalline ceramics that scintillator layers use includes:
(1) preparation of raw material mixed powder body;
In one example, according to the chemical composition (Lu of transparent ceramic scintillator(1-x-y)CexAy)3Al5O12(wherein
0.001≤x≤0.01,0.0005≤y≤0.01) using solid reaction process preparation raw material mixed powder body.Specifically, using oxygen
Change lutetium (Lu2O3), aluminium oxide (Al2O3), cerium oxide (CeO2) and be co-doped with ionic oxide formation be raw material, two kinds of powder originals of accurate weighing
Expect 60g, carried out respectively using dehydrated alcohol or deionized water as decentralized medium wet ball grinding be uniformly mixed, rotational speed of ball-mill can be 80~
200rmp/min, Ball-milling Time can be 5~12 hours;Then mixed powder drying, sieving are obtained oxide and mixed respectively
Close powder.
In another example, raw material mixed powder body can be prepared using liquid phase method.Specifically, it selects and contains Lu3+、Al3 +、Ce3+And it is co-doped with the precursor solution of ion, according to (Lu(1-x-y)CexAy)3Al5O12(wherein 0.001≤x≤0.01,0.0005
≤ y≤0.01) in stoicheiometry precursor solution is mixed, instill to NH4HCO3Or NH3·H2In the precipitating reagents such as O, in order to mention
A certain amount of dispersing agent and surfactant can also be added in high powder dispersity, by being aged, washing, and gained sinks respectively
It forms sediment in 950~1200 DEG C of calcinings acquisition (Lu, A) in 4~8 hours3Al5O12: Ce powder.Wherein the precursor solution can be difference
Contain Lu3+、Al3+、Ce3+With the soluble-salt for being co-doped with ion, such as hydrochloride, nitrate, acetate, sulfate etc..
(2) molding of raw material mixed powder body.The oxide mixed powder and (Lu, A) that will be obtained in (1) respectively3Al5O12:
Ce powder carries out isostatic cool pressing later and improves biscuit density first through dry-pressing formed.It is described it is dry-pressing formed can be 50~
Dry-pressing 1~5 minute under 150MPa, the isostatic cool pressing can be isostatic cool pressing 1~10 minute at 200~400MPa.
(3) vacuum-sintering.Respectively by the biscuit obtained in (2) 10-2Pa~10-4Under the vacuum degree of Pa in 1700~
1900 DEG C (preferably 1700~1820 DEG C) heat preservations 10 hours or more are to carry out vacuum-sintering.The ceramics sample prepared is thrown respectively
Light can be obtained (Lu, A) with high optical quality3Al5O12: Ce crystalline ceramics.The ceramic polished polishing of sintering can be obtained
It obtains (Lu, A)3Al5O12: Ce transparent ceramic scintillator.
(4) preparation of transparent ceramic scintillator plate.Crystalline ceramics is consolidated with substrate by the transparent adhesive in reflecting layer
It is set to as shown in Figure 2.The bonding location of bonding agent is unlimited, as long as composite construction can be fixed to each other and guarantee that scintillator shines i.e.
It can.Optical scatter is filled in bonding agent to enhance reflecting effect.By the composite construction sanding and polishing, and to (Lu, A)3Al5O12: scintillator panel is obtained after Ce transparent ceramic scintillator layer surface etching.After etching, crystalline ceramics surface is finally separated
At multiple independent scintillator arrays units.Each independent array element can be designed to different shape according to actual needs.
It should be understood that the etching technics is also suitble to the microstructure design of other block scintillator materials.
In a preferred embodiment of the present invention, (Lu, the A) of the transparent ceramic scintillator layer use3Al5O12: Ce pottery
Tile has very excellent optical quality, and 2mm thickness sample straight line transmittance at 800nm is more than 73%.
Under the excitation of X-rays that X-ray source issues, (Lu, the A)3Al5O12: Ce transparent ceramic scintillator shines
For intensity up to 7.5 times or more of BGO, die-away time is less than 45ns.
In the present invention, before crystalline ceramics polishing, cross section is square side size range: 10~50mm, thickness
Range: 1mm~4mm.
In a preferred embodiment of the present invention, side length 20mm before the crystalline ceramics is polished, thickness range: 2mm~
4mm。
In the present invention, before substrate polishing, cross section is square side size range: 20~70mm, thickness range:
1mm~8mm.
In a preferred embodiment of the present invention, side length 25mm, thickness range: 1mm~4mm before the substrate is polished.
In the present invention, the transparent adhesive in reflecting layer fixes the crystalline ceramics and substrate.
In a preferred embodiment of the present invention, the transparent adhesive is silica gel.
In a preferred embodiment of the present invention, the scintillator panel is after sanding and polishing, substrate thicknesses range: 0.5mm
~4mm.
In a preferred embodiment of the present invention, the scintillator panel is after sanding and polishing, scintillator layers thickness range: 50
μm~200 μm.
In the present invention, to improve the scintillator layers light collecting efficiency in the scintillator panel, need to carry out surface etch.
After etching, crystalline ceramics surface is finally divided into multiple independent scintillator arrays units.Each independent array element can
To be designed to different shape according to actual needs.The etching technics is also suitble to other block scintillator materials.
Preparation method of the invention can obtain the crystalline ceramics excellent with high optical quality, luminescent properties, after fixed
Scintillator panel can effectively absorb ray and be converted to visible light.The simple process, controllability is high, reproducible, is suitble to
Large-scale production.
Fig. 2 shows the schematic diagrames of the scintillator panel of an example of the present invention.As seen from the figure, scintillator panel is by substrate, reflection
Layer and scintillator layers composition.Ray reaches scintillator layers through substrate reflecting layer, is converted to visible light by scintillator layers absorption.In
Show that upper layer is substrate, middle layer is structure that reflecting layer lower layer is scintillator layers in Fig. 1, it should be appreciated that in the present invention, not
The placement direction for limiting scintillator panel is also possible to left, center, right three-decker composition.But guarantee ray by substrate incident, by dodging
Bright body layer outgoing.
Wherein, substrate thicknesses range: 0.05mm~10mm, preferably: 0.05mm~4mm, more preferably 0.5mm-4mm;
Reflector thickness range: 0.01 μm~0.5 μm, preferably: 0.01 μm~0.2 μm;Scintillator layers thickness range: 50 μm~500 μ
M, preferably: 50 μm~200 μm.
Fig. 3 shows (Lu, the A) of an example of the present invention3Al5O12: Ce transparent ceramic scintillator excitation of X-rays shines
Spectrum, the identical size BGO monocrystalline of Czochralski grown are reference sample.As seen from the figure, under X-ray effect (Lu, A)3Al5O12:
Ce crystalline ceramics can effectively launch 510nm's as it can be seen that steady generation efficiency reaches 7.5 times of BGO.
Fig. 4 is shown in an example of the present invention after surface etch (Lu, A)3Al5O12: the light of Ce transparent ceramic scintillator
Learn microscope photo.As seen from the figure, surface etch transparent ceramic scintillator is used to be divided into side length for 50 μm of rectangular array, square
The spacing of shape array is 10 μm.Transparent ceramic scintillator after surface etch forms waveguide transmission on surface, reduces total reflection damage
It loses, to improve the visible light collecting efficiency of device, increases System spatial resolution.
Technical effect of the invention is as follows;
1, the present invention is using high optical quality, (Lu, the A) of high-luminous-efficiency3Al5O12: Ce crystalline ceramics as scintillator,
The ray flat panel detector system with high spatial resolution is developed.System image quality under excitation of X-rays is high,
Apparent is sharp keen.Using spongy lead to MTF under block-regulations test 10lp/mm 17.5% or more.Selection mark is tested using knife-edge method
RQA5 experiment condition specified in quasi- IEC62220-1 carry out test MTF be 10% when, resolution ratio is in 9lp/mm or more;
2, it can effectively improve detector as scintillator using the stable pomegranate feldspar of chemical property and use the longevity
Life reduces device encapsulation and maintenance cost;
3, the characteristics of being had excellent performance using Ceramic manufacturing after transparent ceramic scintillator is cut into rectangular array, makes ceramics
Surface forms waveguide transmission, reduces light loss caused by total reflection, to improve device collecting efficiency, increases system space and differentiates
Rate.
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary specific value.
Embodiment 1
Using luteium oxide (Lu2O3), aluminium oxide (Al2O3), magnesia (MgO), cerium oxide (CeO2) it is raw material, according to
(Lu0.995Ce0.003Mg0.002)3Al5O12Accurate weighing powder material 60g is formed, then is carried out using dehydrated alcohol as decentralized medium
Ball milling mixing, after a certain period of time, two kinds of powders are respectively through drying, sieving for ball milling;Tabletting is carried out to it afterwards, and it is cold to impose 200MPa
Equal static pressure become green body;It puts it into vacuum or hot-pressed sintering furnace and is sintered 20 hours at 1880 DEG C again, to obtain
(Lu(1-x-y)CexMgy)3Al5O12Ceramics polish obtained ceramic material, and final obtain has high optical quality
Crystalline ceramics.The crystalline ceramics sanding and polishing is cut to 20 × 20 × 2mm.Crystalline ceramics straight line at 800nm penetrates
For rate up to 73%, luminous intensity reaches 7.5 times of BGO monocrystalline.By the substrate of crystalline ceramics and 25 × 25 × 4mm by being mixed with dispersion
The silica gel of grain is adhesively fixed.Scintillator panel is by above-mentioned composite construction polishing grinding surface etch to rear acquisition.Scintillator after processing
Layer is with a thickness of 50 μm, and the rectangular array that its surface is 50 × 50 μm, and 10 μm of spacing.By incident light source, scintillator panel, light cone with
And the components such as CCD are as shown in Figure 1, connection prepares (Lu, A)3Al5O12: Ce transparent ceramic scintillator flat panel detector.The plate is visited
It surveys device spongy lead use to test MTF under 10lp/mm to block-regulations and tested in selection criteria IEC62220-1 using knife-edge method for 17.5%
Defined RQA5 experiment condition carry out test MTF be 10% when, resolution ratio 9lp/mm.
Embodiment 2
When prepared by scintillator panel, scintillator layers are not cut by laser with a thickness of 50 μm, and other conditions are the same as embodiment 1.
The flat panel detector flat panel detector is used spongy lead to test MTF under 10lp/mm to block-regulations and is tested using knife-edge method for 13.0%
RQA5 experiment condition specified in selection criteria IEC62220-1 carry out test MTF be 10% when, resolution ratio 6lp/mm.
Embodiment 3
By (Lu0.997Ce0.001Mg0.002)3Al5O12Chemical constituent accurate weighing 60g, other conditions, can with embodiment 1
With acquisition (Lu0.997Ce0.001Mg0.002)3Al5O12Crystalline ceramics.Straight line transmittance is up to 75% after the polished polishing of preparation ceramics,
Luminous intensity reaches 5 times of BGO monocrystalline.
Embodiment 4
By (Lu0.996Ce0.002Mg0.002)3Al5O12Chemical constituent accurate weighing 60g, other conditions, can with embodiment 1
With acquisition (Lu0.996Ce0.002Mg0.002)3Al5O12Crystalline ceramics.Straight line transmittance is up to 77% after the polished polishing of preparation ceramics,
Luminous intensity reaches 5 times of BGO monocrystalline.
Embodiment 5
By (Lu0.994Ce0.004Mg0.002)3Al5O12Chemical constituent accurate weighing 60g, other conditions, can with embodiment 1
With acquisition (Lu0.994Ce0.004Mg0.002)3Al5O12Crystalline ceramics.Straight line transmittance is up to 67% after the polished polishing of preparation ceramics,
Luminous intensity reaches 8.7 times of BGO monocrystalline.
Embodiment 6
By (Lu0.9968Ce0.002Mg0.0012Li0.0006)3Al5O12Chemical constituent accurate weighing 60g, co-dopant ions oxidation
Object selects LiOHH2O other conditions can obtain (Lu with embodiment 10.9968Ce0.002Mg0.0012Li0.0006)3Al5O12It is transparent
Ceramics.For straight line transmittance up to 71%, luminous intensity reaches 9.0 times of BGO monocrystalline after the polished polishing of preparation ceramics.
Industrial applicability: (Lu, A) of the invention3Al5O12: Ce crystalline ceramics ray flat panel detector has imaging sharp keen
The high feature of spatial resolution, and have many advantages, such as that maintenance cost is low, long service life and maintenance cost are examined applied to medicine
Disconnected, non-destructive testing, public safety, dose of radiation detection and oil exploration etc. are using in the device of ray detection.Pass through surface
The method of etching is designed material microstructure, can effectively improve system imaging resolution ratio, is suitable for all blocks and dodges
Bright body material.
Claims (17)
1. a kind of ray detection flat panel detector scintillator panel, which is characterized in that the scintillator panel includes substrate, scintillator
Layer and it is clipped in shining and fixed substrate and scintillator with increasing scintillator panel between the substrate and scintillator layers
The reflecting layer of the effect of layer, wherein the constitutional chemistry formula of the scintillator layers is (Lu(1-x-y)CexAy)3Al5O12, A case for
The ion of selection includes Ca2+、Mg2+、Sr2+、Ba2+、Li+、 Na+、K+At least one of, 0.001≤x≤0.05,0.0005≤
y≤0.05;
There is the independent array element formed by etching on the surface of the scintillator layers, and array element is rectangular array unit,
The side length of the rectangular array unit is 50 μm~200 μm, 10~20 μm of spacing range, 10~50 μm of etching depth.
2. scintillator panel according to claim 1, which is characterized in that A case ion is Mg2+;0.001≤x≤0.01;
0.0005≤y≤0.01。
3. scintillator panel according to claim 2, which is characterized in that 0.002≤x≤0.005.
4. scintillator panel according to claim 2, which is characterized in that 0.001≤y≤0.005.
5. scintillator panel according to claim 1, which is characterized in that the substrate material include graphite, resin, glass or
Metal, the reflecting layer material include silica gel or epoxy resin.
6. scintillator panel according to claim 1, which is characterized in that scattered in reflector material containing 40~95 wt% light
Particle SiO2Particle.
7. scintillator panel according to claim 1, which is characterized in that substrate with a thickness of the mm of 0.05 mm~10, reflection
Layer with a thickness of 0.01 μm~0.5 μm, scintillator layers with a thickness of 50 μm~500 μm.
8. any scintillator panel in -7 according to claim 1, which is characterized in that substrate with a thickness of 0.05 mm~4
Mm, reflecting layer with a thickness of 0.01 μm~0.2 μm, scintillator layers with a thickness of 50 μm~200 μm.
9. scintillator panel according to claim 8, which is characterized in that substrate with a thickness of the mm of 0.5 mm~4.
10. the preparation method of any scintillator panel in a kind of claim 1-9 characterized by comprising
1) solid reaction process or liquid phase method combination ceramic sintering technology, preparation flashing are used according to the constitutional chemistry formula of scintillator layers
Body layer material;
2) scintillator layers material prepared by step 1) is cut into the scintillator layers thin slice of predetermined size;
3) it after fixing scintillator layers thin slice and substrate by reflector material, is polishing to specific thickness and polishes.
11. preparation method according to claim 10, which is characterized in that before the polishing of scintillator layers thin slice, cross section is square
Shape, 10~50 mm of side size range, thickness range 1 mm~4 mm;
Before substrate polishing, cross section is rectangle, 20~70 mm of side size range, thickness range 1 mm~8 mm.
12. preparation method described in 0 or 11 according to claim 1, which is characterized in that the preparation method further include:
4) surface for etching the scintillator layers, forms it into array element, wherein the mode of etching includes: wire cutting, laser
Cutting or inductively coupled plasma body.
13. a kind of flat panel detector containing the scintillator panel any in claim 1-9, which is characterized in that the plate
Detector includes scintillator panel, light cone and electrooptical device.
14. the crystalline ceramics that any scintillator panel uses in a kind of claim 1-9, which is characterized in that the transparent pottery
The constitutional chemistry formula of porcelain is (Lu(1-x-y)CexAy)3Al5O12, the alternative ion of A case includes Ca2+、Mg2+、Sr2+、Ba2+、
Li+、 Na+、K+At least one of, 0.001≤x≤0.01,0.0005≤y≤0.01.
15. a kind of preparation method of crystalline ceramics described in claim 14 characterized by comprising
1) it prepares mixed uniformly comprising luteium oxide, aluminium oxide, cerium oxide and the material powder for being co-doped with ion-oxygen compound;
2) biscuit of ceramics will be obtained after material powder molding;
3) by biscuit of ceramics, vacuum-sintering obtains the crystalline ceramics at 1700-1900 DEG C.
16. preparation method according to claim 15, which is characterized in that molding using dry-pressing formed or isostatic cool pressing at
Type, wherein dry-pressing formed is dry-pressing 1~5 minute at 50~150 MPa, and isostatic cool pressing is cold etc. at 200~400 MPa
Static pressure 1~10 minute.
17. preparation method according to claim 15 or 16, which is characterized in that the vacuum-sintering is in pressure≤10-2
Keep the temperature 10 hours in 1700~1820 DEG C under the vacuum degree of Pa or more.
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