CN103305925B - Cesium iodide,crystal film surface defects processing method - Google Patents
Cesium iodide,crystal film surface defects processing method Download PDFInfo
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- CN103305925B CN103305925B CN201310269684.0A CN201310269684A CN103305925B CN 103305925 B CN103305925 B CN 103305925B CN 201310269684 A CN201310269684 A CN 201310269684A CN 103305925 B CN103305925 B CN 103305925B
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- cesium iodide
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Abstract
The present invention relates to technology of thin film material preparation.The invention discloses a kind of cesium iodide,crystal film surface defects processing method.The technical scheme is that cesium iodide,crystal film surface defects processing method comprises the following steps: a, cesium iodide,crystal thin film is put into hot air circulation drying oven；B, in hot air circulation drying oven inflated with nitrogen, discharge gas in case, in making case, form clean environment；C, set the temperature inside the box as 20～50 DEG C, utilize nitrogen circulation in blower system driving box, it is ensured that the temperature inside the box is uniform；D, reach the setting time, take out cesium iodide,crystal thin film.Processing procedure of the present invention is easy, membrane structure is changed without other measures additional, the tiny flaws such as sample hole after process, gap disappear, the continuous compactness of thin film and surface texture substantially improve, and have very important significance performances such as improving the continuous compactness of cesium iodide,crystal thin film and spatial resolution.
Description
Technical field
The present invention relates to technology of thin film material preparation, particularly to cesium iodide,crystal (CsI:Tl) film surface structure optimization technology.
Background technology
X-ray detection technology scientific research, live, be used widely in the field such as production, such as military aspect, can be used for analyzing
Missile impact ripple；Medical treatment aspect, can make the medical procedure image digitazations such as intervention, perspective, radiography, for long-range Clinics and Practices
Offer condition；Scientific research aspect, can develop medicine to toy radiation research for biosystem.Additionally, this technology is at spacecraft
There is huge application in the fields such as Non-Destructive Testing, space flight telescope, safety detecting system, earth mine locating, night vision, image transmitting
Prospect.
CsI:Tl is the scintillator material of a kind of excellent performance, and not only photoyield is high but also irradiation intensity is good, it is easy to same to silicon photocell
Carrying out Spectral matching, and good mechanical performance, production cost is relatively low, can be excited as optical fibers simultaneously.Utilize
CCD is as in the X-ray detection system of image record, and the effect of scintillation material is that X-ray is converted to recordable visible ray,
Its properties directly affects processing result image below.Present stage, China's scintillator used in terms of X-ray detection
Material still based on bulk, Chinese patent 94112210.7 " descent method for growing large size cesium iodide (CsI) crystal new technique ",
Chinese patent 96116387.9 " Technology of antivacuum descent method for growing cesium iodide,crystal crystal ", Chinese patent
200310109480.7 " the cesium iodide,crystal crystal technique with elemental powders as deoxidizer " and Chinese patents
What 201110340816.5 " the Bridgman-Stockbarge method for growing techniques of cesium iodide and cesium iodide,crystal monocrystalline " etc. were introduced is all to prepare bulk iodine
Change the new technique of caesium crystal and new technology, due to CsI:Tl crystal exist in the application as bulk volume more greatly, the lightest, no
The defects such as the connection equipment (such as optical fibers) that easy of integrationization, the needs that are connected with detector are extra, institute is for X-ray detection
The CsI:Tl crystal volume of device and other field application is relatively big, has the biggest deficiency at integrated aspect.Therefore, by CsI:Tl
Crystal film has critically important meaning for the integrated of X-ray detector, and Chinese patent 200910060112.5 " mixes thallium iodine
Change a kind of preparation method of caesium (CsI:Tl) thin film " and Chinese patent 201110442455.5 " micro-column structure CsI (Tl) X-ray
The preparation method and applications of flicker conversion screen " the middle new technology preparing microtrabeculae shape CsI:Tl thin film exactly introduced, due to thermal evaporation
The limitation of coating process, in coating process, the increase thin film top layer along with film thickness there will be the tables such as hole, gap and crackle
Face fault of construction, can have a strong impact on the continuous compactness of thin film, thus reduce its performance such as light conversion efficiency and spatial resolution.
Therefore, improve the continuous compactness of microtrabeculae shape structural membrane, make it can keep excellent at the other light conversion properties of film-grade, right
The overall performance improving X-ray detector has very important significance.
Summary of the invention
It is an object of the invention to provide a kind of cesium iodide,crystal film surface defects processing method, it have simple to operate, effect is bright
The feature such as aobvious.
The present invention solves described technical problem and employed technical scheme comprise that, cesium iodide,crystal film surface defects processing method, including
Following steps:
A, cesium iodide,crystal thin film is put into hot air circulation drying oven；
B, in hot air circulation drying oven inflated with nitrogen, discharge gas in case, in making case, form clean environment；
C, set the temperature inside the box as 20～50 DEG C, utilize nitrogen circulation in blower system driving box, it is ensured that the temperature inside the box is uniform；
D, reach the setting time, take out cesium iodide,crystal thin film.
Further, described cesium iodide,crystal thin film uses thermal evaporation coating process to be produced on substrate, in step a, together with lining
Hot air circulation drying oven is put at the end together.
Concrete, described substrate is n type single crystal silicon.
Concrete, described substrate is p type single crystal silicon.
Concrete, described substrate is the p type single crystal silicon being coated with silica membrane.
Further, in step d, set the time according to cesium iodide,crystal film thickness.
Recommending, when cesium iodide,crystal film thickness is respectively 70 μm, 100 μm, 150 μm, it is little that the setting time is respectively 12
Time, 24 hours, 36 hours.
Preferably, in step c, set the temperature inside the box as 27 DEG C.
The invention has the beneficial effects as follows, processing procedure is easy, it is not necessary to other measures additional change membrane structure, the sample after process
The tiny flaw such as hole, gap disappears, and the continuous compactness of thin film and surface texture substantially improve, and overcome different experimental conditions
Lower occur when preparing thin film hole, the tiny area structure problem such as gap, to the continuous compactness improving cesium iodide,crystal thin film
Have very important significance with performances such as spatial resolution.
Accompanying drawing explanation
Fig. 1 be film sample thickness be 70 μm use the present invention process before and after film surface Structure Comparison schematic diagram；
Fig. 2 be film sample thickness be 100 μm use the present invention process before and after film surface Structure Comparison schematic diagram；
Fig. 3 be film sample thickness be 150 μm use the present invention process before and after film surface Structure Comparison schematic diagram；
Fig. 4 is the process chart of the present invention.
Detailed description of the invention
The essence of the present invention be by the physical method placed in specific environment overcome cesium iodide,crystal (CsI:Tl) thin film hole,
The tiny area result defects such as gap, it is achieved the continuous compactness of cesium iodide,crystal (CsI:Tl) film surface structure.
Embodiment
Selecting purity to be the CsI:Tl powder that CsI and the TlI crystal of 99.99% mixes, substrate selects common microscope slide；
Cesium iodide,crystal film thickness is: sample 1 (70 μm), sample 2 (100 μm), sample 3 (150 μm)；Prepare thin film
Vacuum be 7 × 10-3Pa, evaporation current is 130A, and substrate is room temperature.
Hot air circulation drying oven working condition is: temperature is set as 27 DEG C, and air blast power is 370W, horizontal blast, the time
It is set as 12 hours (sample 1), 24 hours (sample 2), 36 hours (sample 3)；Optical metallographic microscope viewing film
Surface texture.
This example cesium iodide,crystal film surface defects process flow as shown in Figure 4, including following key step:
A, cesium iodide,crystal thin film is put into hot air circulation drying oven together with substrate；
B, in hot air circulation drying oven inflated with nitrogen, discharge gas in case, in making case, form clean environment；
C, set the temperature inside the box as 27 DEG C, utilize nitrogen circulation in blower system driving box, it is ensured that the temperature inside the box is uniform；
D, reach the setting time, take out cesium iodide,crystal thin film.
This example substrate can also use n type single crystal silicon, or p type single crystal silicon, or is coated with the p type single crystal silicon of silica membrane.
Increase owing to usual cesium iodide,crystal film surface defects increases along with film thickness, in step d, can be according to mixing thallium
Cesium iodide film thickness sets the time.
In the present invention, as long as thin film effect of optimization would not be impacted in prescribed limit by temperature, typical temperature is at 20～50 DEG C
Just can meet process requirement, set the temperature inside the box as 27 DEG C, be a both economical selection, temperature controls fairly simple,
Easily realize.Then the longer the better to set the time, but would not change after being optimized to a certain degree due to film defects again,
So setting, although the longer the better the time, but also will as the case may be depending on, in order to avoid waste resource.Cesium iodide,crystal thin film is thick
When degree is 70 μm, 100 μm, 150 μm, the setting time be respectively 12 hours, 24 hours, 36 hours substantially just permissible
Reaching treatment effect, the time extends the most nonsensical again, can increase processing cost on the contrary.
Fig. 1,2,3, respectively illustrate cesium iodide,crystal film thickness when being 70 μm, 100 μm, 150 μm, set the time
It is respectively 12 hours, 24 hours, the surface defect result of 36 hours.In figure, the photo on the left side is that cesium iodide,crystal is thin
Film Metallograph before treatment, the photo on the right is the Metallograph after cesium iodide,crystal thin film processes.Optics metallographic
Microscope is observed it can be seen that after the present invention processes, surface defect is obviously improved.Process zero in front sample 1
A large amount of holes in star hole, sample 2 and the slight gap in sample 3 all disappear, and the substitute is seriality and cause
Close property all well surface texture, the scheme that the present invention provides improves the continuous compactness of cesium iodide,crystal thin film, improves and mix
The performances such as the light conversion efficiency of thallium cesium iodide thin film and spatial resolution.
Claims (9)
1. cesium iodide,crystal film surface defects processing method, comprises the following steps:
A, cesium iodide,crystal thin film is put into hot air circulation drying oven；
B, in hot air circulation drying oven inflated with nitrogen, discharge gas in case, in making case, form clean environment；
C, set the temperature inside the box as 27～50 DEG C, utilize nitrogen circulation in blower system driving box, it is ensured that the temperature inside the box is uniform；
D, reach the setting time, take out cesium iodide,crystal thin film.
Cesium iodide,crystal film surface defects processing method the most according to claim 1, it is characterised in that described in mix thallium iodine
Changing caesium thin film uses thermal evaporation coating process to be produced on substrate, in step a, puts into hot air circulation drying oven together with substrate.
Cesium iodide,crystal film surface defects processing method the most according to claim 2, it is characterised in that described substrate is
Common microscope slide.
Cesium iodide,crystal film surface defects processing method the most according to claim 2, it is characterised in that described substrate is
N type single crystal silicon.
Cesium iodide,crystal film surface defects processing method the most according to claim 2, it is characterised in that described substrate is
P type single crystal silicon.
Cesium iodide,crystal film surface defects processing method the most according to claim 2, it is characterised in that described substrate is
It is coated with the p type single crystal silicon of silica membrane.
Cesium iodide,crystal film surface defects processing method the most according to claim 1, it is characterised in that in step d,
The time is set according to cesium iodide,crystal film thickness.
Cesium iodide,crystal film surface defects processing method the most according to claim 7, it is characterised in that cesium iodide,crystal
When film thickness is respectively 70 μm, 100 μm, 150 μm, the setting time is respectively 12 hours, 24 hours, 36 hours.
9. according to the cesium iodide,crystal film surface defects processing method described in above-mentioned any one claim, it is characterised in that
In step c, set the temperature inside the box as 27 DEG C.
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Citations (5)
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| CN1550023A (en) * | 2001-08-29 | 2004-11-24 | ��ʽ���綫֥ | Production method and production device for x-ray image detector and x-ray image detector |
| CN101002110A (en) * | 2004-08-10 | 2007-07-18 | 佳能株式会社 | Radiation detecting apparatus, scintillator panel, their manufacturing method and radiation detecting system |
| CN101967678A (en) * | 2009-07-27 | 2011-02-09 | 电子科技大学 | Method for preparing thallium-doped caesium iodide (CsI:T1) film |
| CN102700027A (en) * | 2012-05-23 | 2012-10-03 | 中昊晨光化工研究院 | Teflon drying system and application thereof |
| CN202792877U (en) * | 2012-08-23 | 2013-03-13 | 吕江强 | Closed cycle baking oven |
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| JP4201933B2 (en) * | 1999-09-22 | 2008-12-24 | 株式会社東芝 | Radiation-excited phosphor screen processing method and processing apparatus, and image intensifier thereby |
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Patent Citations (5)
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| CN1550023A (en) * | 2001-08-29 | 2004-11-24 | ��ʽ���綫֥ | Production method and production device for x-ray image detector and x-ray image detector |
| CN101002110A (en) * | 2004-08-10 | 2007-07-18 | 佳能株式会社 | Radiation detecting apparatus, scintillator panel, their manufacturing method and radiation detecting system |
| CN101967678A (en) * | 2009-07-27 | 2011-02-09 | 电子科技大学 | Method for preparing thallium-doped caesium iodide (CsI:T1) film |
| CN102700027A (en) * | 2012-05-23 | 2012-10-03 | 中昊晨光化工研究院 | Teflon drying system and application thereof |
| CN202792877U (en) * | 2012-08-23 | 2013-03-13 | 吕江强 | Closed cycle baking oven |
Non-Patent Citations (4)
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| Heat enhancement of the photoyield from CsI, NaI and CuI photocathodes;A. Buzulutskov，等;《Nuclear Instruments and Methods in Physics Research A》;19951201;第366卷;410-412 * |
| Production technique and quality evaluation of CsI photocathodes for the ALICE/HMPID detector;H. Hoedlmoser，等;《Nuclear Instruments and Methods in Physics Research A》;20060814;第566卷;338-350 * |
| Properties of CsI and CsI-TMAE photocathodes;D.F. Anderson,等;《Nuclear Instruments and Methods in Physics Research A》;19921215;第323卷;626-634 * |
| The sensitivity and spatial resolution dependence on the microstructures of CsI:Tl scintillation layer for X-ray imaging detectors;Bo Kyung Cha，等;《Nuclear Instruments and Methods in Physics Research A》;20100620;第633卷;S297-S299 * |
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