CN102496400A - Preparation method of CsI(T1) X-ray scintillation conversion screen with microcolumn structure and application thereof - Google Patents

Preparation method of CsI(T1) X-ray scintillation conversion screen with microcolumn structure and application thereof Download PDF

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CN102496400A
CN102496400A CN2011104424555A CN201110442455A CN102496400A CN 102496400 A CN102496400 A CN 102496400A CN 2011104424555 A CN2011104424555 A CN 2011104424555A CN 201110442455 A CN201110442455 A CN 201110442455A CN 102496400 A CN102496400 A CN 102496400A
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conversion screen
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csi
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vapor deposition
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CN102496400B (en
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顾牡
姚达林
刘小林
刘波
黄世明
倪晨
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Tongji University
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Abstract

The invention relates to a preparation method of CsI(T1) X-ray scintillation conversion screen with a microcolumn structure and application thereof. The method for preparing a CsI(T1) X-ray scintillation conversion screen with a microcolumn structure is provided. According to the method, CsI(T1) is used as a raw material as well as quartz, a fiber faceplate and an optical taper and the like are used as a substrate; and a thermal evaporation technology is employed and adjustment on an evaporation temperature, a substrate temperature and preparation atmosphere and the like is carried out; therefore, effective control on morphology, a line width, a predominant crystal orientation and the like of a microcolumn of a conversion screen can be realized. The scintillation microcolumn that is approximately vertical to the screen surface and has a good crystallization performance can guide scintillating lights to be transmitted along the microcolumn direction, so that a spatial resolution of an X-ray image device can be improved and requirements on a high spatial resolution and high detection efficient can be met. The prepated CsI(T1) X-ray scintillation conversion screen with the microcolumn structure can be coupled with a photoelectric detector and then can be applied for X ray imaging with a high resolution ratio. According to the invention, the preparation method is suitable for industrialization production and the promotion application value is high.

Description

The preparation method and the application thereof of microtrabeculae structure C sI (Tl) X ray flicker conversion screen
Technical field
The invention belongs to high-resolution digital x-ray imaging technical field; Be specifically related to the preparation method and the application thereof of a kind of microtrabeculae structure cesium iodide (mixing thallium) [chemical formula: CsI (Tl)] X ray flicker conversion screen, prepared flicker conversion screen can satisfy the x-ray imaging requirement of high spatial resolution and high detection efficiency simultaneously.
Background technology
X-ray imaging has very at numerous areas such as crystallography, medical science and life science, plasma diagnostics, Non-Destructive Testing and astrophysicss to be used widely.Along with the particularly development of x-ray tomography imaging technique (X-ray CT) of x-ray imaging technology, the method for carrying out image recording through sensitive film far can not adapt to actual needs in recent years.For this reason, people have successively been developed X ray charge-coupled image sensor (X ray CCD) and X ray amorphous silicon photodiodes array (X ray a-Si:H), have realized the digitized record of radioscopic image.
The ultimate principle of X ray CCD and X ray a-Si:H is: convert radioscopic image to visible images by the flicker conversion screen, through optical taper etc. image is coupled on the common CCD or a-Si:H.Therefore under the prerequisite that visible light CCD and a-Si:H become better and approaching perfection day by day, the performance of the conversion screen that glimmers is the key that influences x-ray imaging sensitive detection parts index.CsI (Tl) is one of at present the most frequently used flicker conversion screen material, its emission peak :-540nm, photoyield :-64ph/keV, luminescence decay time :-0.8 μ s.With regard to the angle that improves the x-ray imaging spatial resolution (as: the breast X-ray imaging hopes that spatial resolution can reach tens μ m magnitudes); Usually the film thickness that needs restriction flicker conversion screen; But thin thickness is difficult to satisfy the needs that the flicker conversion screen is surveyed X ray (particularly hard X ray) again, and therefore common X ray conversion screen is difficult to satisfy simultaneously the requirement of high spatial resolution and high X ray detection efficiency.
C. W. Bates in 1969; Jr. with A. L. N. Stevels in 1974 etc. at first report adopt vacuum thermal evaporation can prepare CsI film with microtrabeculae structure; This special microtrabeculae structure can guide passage of scintillation light along post to propagation, thereby can effectively improve the spatial resolution of x-ray imaging; Play I. Fujieda, V. V. Nagarkar, Garnier etc. in 1991 and studied the influence to the output of conversion screen light, modulation transfer function, noise power, detective quantum efficiency etc. such as vapor deposition boat temperature, substrate and underlayer temperature, absorption and reflection horizon coating respectively; Polycrystalline structure in CsI (Tl) microtrabeculae can cause the absorption and the scattering of passage of scintillation light; To this phenomenon; Played A. Ananenko, A. Lebedinsky and A. Fedorov etc. in 2004 and studied the influence of substrate respectively the microtrabeculae crystal property; On LiF (100) crystal face prepare (110) and (112) two kinds CsI (Tl) the microtrabeculae film of high preferred orientations according to qualifications, but they are CsI (Tl) the microtrabeculae film that substrate has obtained to have (110) and (112) two kinds of high preferred orientations of selecting the superior at glass also simultaneously; A. Fedorov had studied the hydrophobic property of CsI film on LiF (100) crystal face in 2010, proposed the CsI particulate and was the surface energy difference that mainly comes from CsI and substrate perpendicular to < 110>preferred orientation of substrate surface.
Research for CsI (Tl) X ray flicker switching film; Domestic report is very limited; Cheng Feng in 2008 etc. have studied the influence of annealing temperature to CsI (T1) film microstructure and scintillation properties, find that annealing can influence the crystal property of CsI (T1) film, Tl distributes and the quantity of defective and size etc.; So far domesticly also do not see relevant microtrabeculae structure C sI (Tl) film preparation and study comparatively systematic account.
Make a general survey of domestic and international present Research; Although for the existing abroad report of the development with microtrabeculae structure C sI (Tl) X ray conversion screen; But its means relate generally to vapor deposition temperature, underlayer temperature etc., and the ability of regulation and control of microtrabeculae at aspects such as pattern, live width, crystal properties remained further to be strengthened; Domesticly do not see that also the comparatively expansion of system is arranged and study accordingly.
Summary of the invention
The object of the present invention is to provide the preparation method and the application thereof of a kind of microtrabeculae structure C sI (Tl) X ray flicker conversion screen.
The preparation method of microtrabeculae structure C sI (Tl) the X ray flicker conversion screen that the present invention proposes; With CsI (Tl) is raw material; With glass, fibre faceplate or optical taper etc. is substrate, adopts hot evaporation coating technique, through the adjusting of vapor deposition temperature, underlayer temperature, prepared atmosphere etc.; Realization is to effective control of conversion screen microtrabeculae pattern, live width, crystal property, thereby makes CsI (Tl) the X ray flicker conversion screen of being developed have good spatial resolution.Concrete steps are following:
(1) used substrate is cleaned up oven dry back kept dry with ultrasonic method;
(2) step (1) gained substrate is fixed on the work rest of deposited chamber top, then the CsI that takes by weighing (Tl) powder is placed in the vapor deposition boat, the distance between vapor deposition boat and substrate is provided with baffle plate between vapor deposition boat and the substrate between 10-30cm;
(3) open vacuum pump, the vacuum tightness of control deposited chamber is 1.0 * 10 -6-5.0 * 10 -3Pa;
(4) work rest is furnished with heating and slewing, in vacuum, can adjust underlayer temperature, and underlayer temperature is controlled between the room temperature to 350 ℃; Before the beginning evaporated film, work rest is at the uniform velocity rotated with the rotating speed of 45-75rpm;
(5) treat that vacuum tightness and underlayer temperature reach balance after, can regulate gas admittance valve as required, inject micro-argon gas, argon flow amount is controlled at: (or air pressure is controlled at≤60sccm :≤6 * 10 -1Pa); Open vapor deposition boat heating power supply, the vapor deposition boat is heated to 420-540 ℃, and keep temperature-resistant.
(6) after boat to be deposited reaches predetermined temperature, open baffle plate, start vaporizer, through the film thickness of the prepared conversion screen of thicknessmeter on-line measurement, treat that film thickness reaches predetermined the requirement after, close baffle plate, vapor deposition boat power supply and substrate heating power supply etc.
(7) vacuum environment is closed vacuum valve after naturally cooling to room temperature, takes out after charging into dry gas, and the CsI that obtains (Tl) flicker conversion screen places dry environment to store.It is CsI (Tl) the X ray flicker conversion screen pictorial diagram of substrate that Fig. 1 and Fig. 2 are respectively with quartz glass and fibre faceplate.
Among the present invention, the substrate described in the step (1) be in glass, fibre faceplate or the optical taper etc. any, substrate dimension can be adjusted according to actual needs.
Among the present invention; The consumption of the raw material of CsI (Tl) described in the step (2) confirmed by the conversion screen film thickness of required preparation, and and vapor deposition boat and substrate between distance dependent, if will prepare tens microns CsI (Tl) conversion screens to millimeter magnitude thickness; The raw material consumption is usually between several grams to several hectograms; The thicker conversion screen of preparation thickness can be through repeatedly vapor deposition completion, and 1g raw material consumption can prepare the film of 1-7 μ m thickness usually.
Among the present invention, firing equipment used in step (4) and the step (5) uses temperature-controlling system, can keep temperature stabilization constant, guarantees the stability of coating process; The pattern and the crystal property of vapor deposition temperature, underlayer temperature, prepared atmosphere is adjustable conversion screen microtrabeculae, the live width of microtrabeculae can be regulated between sub-micron to tens micron, and the crystal face preferred orientation is respectively (110) and (200) etc.
Among the present invention, dry gas is a nitrogen described in the step (7).
The microtrabeculae near vertical of utilizing the flicker conversion screen that the inventive method prepares is in panel, marshalling.
The flicker conversion screen and the application of photoelectric detector coupling back in high resolution X-ray imaging that utilize the inventive method to prepare.
The present invention relates to adopt hot vapour deposition method; CsI (Tl) the flicker conversion screen that has the microtrabeculae structure through special preparation technology preparation on quartz, fibre faceplate and optical taper etc.; The microtrabeculae that is obtained is not only regular, orderly, controlled; And good crystallinity; Near vertical can guide passage of scintillation light to propagate along the microtrabeculae direction in the flicker microtrabeculae of panel, thereby the spatial resolution of x-ray imaging device is effectively improved, and can satisfy the x-ray imaging requirement of high spatial resolution and high X ray detection efficiency simultaneously.The present invention is suitable for suitability for industrialized production, and application value is high.
Description of drawings
Fig. 1 is CsI (Tl) the X ray flicker conversion screen pictorial diagram of substrate with the quartz glass.
Fig. 2 is CsI (Tl) the X ray flicker conversion screen pictorial diagram of substrate with the fibre faceplate.
The stereoscan photograph of the flicker conversion screen section that records among Fig. 3 embodiment 1.
The flicker conversion screen X-ray diffraction spectrogram that records among Fig. 4 embodiment 1.
The stereoscan photograph of the flicker conversion screen section that records among Fig. 5 embodiment 2.
The flicker conversion screen X-ray diffraction spectrogram that records among Fig. 6 embodiment 2.
The stereoscan photograph of the flicker conversion screen section that records among Fig. 7 embodiment 3.
The flicker conversion screen X-ray diffraction spectrogram that records among Fig. 8 embodiment 3.
The flicker conversion screen modulation transfer function that records through the microfocus x-ray imaging system among Fig. 9 embodiment 3.
Embodiment
Embodiment below in conjunction with concrete further specifies the present invention.
Embodiment 1:
CsI (Tl) powder that takes by weighing 12.5g adds in the vapor deposition boat, and the substrate that cleans up (glass, fibre faceplate or optical taper) is fixed on the work rest, and the distance between vapor deposition boat and substrate is 15cm, begins to vacuumize.In the vacuum, underlayer temperature is controlled at 300 ℃, chamber to be deposited vacuum tightness reaches 1.0 * 10 -3During Pa, work rest is at the uniform velocity rotated with the rotating speed of 45rpm and begin to heat vapor deposition boat to 500 ℃, open the baffle plate of retaining above the vapor deposition boat then, the beginning evaporated film.Raw materials evaporate finishes, and closes vapor deposition boat heating power supply and substrate heating power supply.Conversion screen is closed vacuum valve after in vacuum environment, naturally cooling to room temperature, opens deposited chamber after charging into drying nitrogen, and CsI (Tl) powder that takes by weighing 12.5g again adds in the vapor deposition boat.Repeat above-mentioned steps, obtain CsI (Tl) the flicker conversion screen of twice vapor deposition.The stereoscan photograph of flicker conversion screen section is seen Fig. 3, and X-ray diffraction spectrum is seen Fig. 4.Experiment shows: conversion screen thickness is about 80 μ m, and repeatedly vapor deposition is to reach needed thickness; Microtrabeculae is arranged in order, and its average live width is about 15 μ m, and the crystal face preferred orientation is (110).
Embodiment 2:
CsI (Tl) powder that takes by weighing 4.0g adds in the vapor deposition boat, and the substrate that cleans up (glass, fibre faceplate or optical taper) is fixed on the work rest, and the distance between vapor deposition boat and substrate is 12cm, begins to vacuumize, and underlayer temperature keeps room temperature.Chamber to be deposited vacuum tightness reaches 2.0 * 10 -4During Pa, work rest is at the uniform velocity rotated with the rotating speed of 60rpm and open vapor deposition boat heating power supply, the vapor deposition boat is heated to 450 ℃, open the baffle plate of retaining above the vapor deposition boat then, the beginning evaporated film, raw materials evaporate finishes, and closes vapor deposition boat heating power supply.Conversion screen is closed vacuum valve after in vacuum environment, naturally cooling to room temperature, takes out after charging into drying nitrogen.Prepared flicker conversion screen profile scanning electromicroscopic photograph is seen Fig. 5, and X-ray diffraction spectrum is seen Fig. 6.Experiment shows: conversion screen thickness is about 23 μ m, and microtrabeculae is arranged in order, and its average live width is about about 2.6 μ m, and the crystal face preferred orientation is (200).
Embodiment 3:
CsI (Tl) powder that takes by weighing 4.0g adds in the vapor deposition boat; The substrate that cleans up (glass, fibre faceplate or optical taper) is fixed on the work rest, guarantees that substrate is placed on directly over the vapor deposition boat, the distance between vapor deposition boat and substrate is 12cm; Begin to vacuumize, underlayer temperature keeps room temperature.Chamber to be deposited vacuum tightness reaches 2.0 * 10 -4During Pa, inject micro-argon gas, argon flow amount is controlled at 50sccm; Open vapor deposition boat heating power supply, the vapor deposition boat is heated to 450 ℃, open the baffle plate of retaining above the vapor deposition boat then, the beginning evaporated film, raw materials evaporate finishes, and closes vapor deposition boat heating power supply etc.Conversion screen is closed vacuum valve after in vacuum environment, naturally cooling to room temperature, takes out after charging into drying nitrogen.Prepared flicker conversion screen profile scanning electromicroscopic photograph is seen Fig. 7, and X-ray diffraction spectrum is seen Fig. 8, and the modulation transfer function that records conversion screen through the microfocus x-ray imaging system is seen Fig. 9.Experiment shows: conversion screen thickness is about 23mm, and microtrabeculae is arranged in order, and its average live width is about about 1.4mm, and the crystal face preferred orientation is (200), and the spatial resolution of x-ray imaging can reach 23lp/mm.

Claims (7)

1. the preparation method of a microtrabeculae structure C sI (Tl) X ray flicker conversion screen is characterized in that concrete steps are following:
(1) used substrate is cleaned up oven dry back kept dry with ultrasonic method;
(2) step (1) gained substrate is fixed on the work rest of deposited chamber top, then the CsI that takes by weighing (Tl) powder is placed in the vapor deposition boat, the distance between vapor deposition boat and substrate is provided with baffle plate between vapor deposition boat and the substrate between 10-30cm;
(3) open vacuum pump, the vacuum tightness of control deposited chamber is 1.0 * 10 -6-5.0 * 10 -3Pa;
(4) work rest is furnished with heating and slewing, in vacuum, can adjust underlayer temperature, and underlayer temperature is controlled between the room temperature to 350 ℃; Before the beginning evaporated film, work rest is at the uniform velocity rotated with the rotating speed of 45-75rpm;
(5) treat that vacuum tightness and underlayer temperature reach balance after, can regulate gas admittance valve as required, inject micro-argon gas, argon flow amount is controlled at :≤60sccm, or air pressure is controlled at :≤6 * 10 -1Pa; Open vapor deposition boat heating power supply, the vapor deposition boat is heated to 420-540 ℃, and keep temperature-resistant;
(6) after boat to be deposited reaches predetermined temperature, open baffle plate, start vaporizer, through the film thickness of the prepared conversion screen of thicknessmeter on-line measurement, treat that film thickness reaches predetermined the requirement after, close baffle plate, vapor deposition boat power supply and substrate heating power supply;
(7) vacuum environment is closed vacuum valve after naturally cooling to room temperature, takes out after charging into dry gas, and the CsI that obtains (Tl) flicker conversion screen places dry environment to store.
2. preparation method according to claim 1, it is characterized in that the substrate described in the step (1) be in glass, fibre faceplate or the optical taper any.
3. preparation method according to claim 1, the consumption that it is characterized in that the raw material of CsI (Tl) described in the step (2) confirmed by the conversion screen film thickness of required preparation, and and vapor deposition boat and substrate between distance dependent.
4. preparation method according to claim 1 is characterized in that used firing equipment all uses temperature-controlling system in step (4) and the step (5).
5. preparation method according to claim 1, the live width that it is characterized in that gained microtrabeculae structure C sI (Tl) X ray flicker conversion screen are sub-micron to tens micron, and the crystal face preferred orientation is respectively (110) and (200).
6. preparation method according to claim 1, the microtrabeculae near vertical that it is characterized in that gained microtrabeculae structure C sI (Tl) X ray flicker conversion screen be in panel, marshalling.
7. microtrabeculae structure C sI (Tl) X ray flicker conversion screen and the photoelectric detector coupling application in high resolution X-ray imaging afterwards of obtaining of preparation method according to claim 1.
CN201110442455.5A 2011-12-27 2011-12-27 Preparation method of CsI(T1) X-ray scintillation conversion screen with microcolumn structure and application thereof Expired - Fee Related CN102496400B (en)

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Cited By (7)

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CN103060752A (en) * 2013-01-22 2013-04-24 同济大学 Pre-plating layer auxiliary preparation method of X-ray flash conversion screen with micro-column structure CsI (Tl) and application thereof
CN103614694A (en) * 2013-11-21 2014-03-05 同济大学 Preparation method of template auxiliary matrix-type micro-columnar CsI(Tl) scintillation conversion screen and application of scintillation conversion screen
CN103961115A (en) * 2013-01-29 2014-08-06 北京科实医学图像技术研究所 Intensifying screen
CN105609153A (en) * 2015-12-18 2016-05-25 深圳大学 High-resolution X-ray conversion screen fluorescent material filling method
CN108130512A (en) * 2017-11-21 2018-06-08 同济大学 ZnO:Ga monocrystal nano rods array X radiographic flicker conversion screen and its preparation method and application
CN109680247A (en) * 2019-01-04 2019-04-26 潍坊华鼎电子技术有限公司 A kind of booster cutout screen evaporation of aluminum technique
CN115818972A (en) * 2022-11-16 2023-03-21 曹掌歧 Glass scintillation substrate for detecting soft beta particle rays and preparation method thereof

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103060752A (en) * 2013-01-22 2013-04-24 同济大学 Pre-plating layer auxiliary preparation method of X-ray flash conversion screen with micro-column structure CsI (Tl) and application thereof
CN103961115A (en) * 2013-01-29 2014-08-06 北京科实医学图像技术研究所 Intensifying screen
CN103614694A (en) * 2013-11-21 2014-03-05 同济大学 Preparation method of template auxiliary matrix-type micro-columnar CsI(Tl) scintillation conversion screen and application of scintillation conversion screen
CN103614694B (en) * 2013-11-21 2016-01-20 同济大学 The template companion matrix rod structure CsI (Tl) that declines glimmers the preparation method of conversion screen and application thereof
CN105609153A (en) * 2015-12-18 2016-05-25 深圳大学 High-resolution X-ray conversion screen fluorescent material filling method
CN108130512A (en) * 2017-11-21 2018-06-08 同济大学 ZnO:Ga monocrystal nano rods array X radiographic flicker conversion screen and its preparation method and application
CN109680247A (en) * 2019-01-04 2019-04-26 潍坊华鼎电子技术有限公司 A kind of booster cutout screen evaporation of aluminum technique
CN115818972A (en) * 2022-11-16 2023-03-21 曹掌歧 Glass scintillation substrate for detecting soft beta particle rays and preparation method thereof

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