CN107164734A - A kind of Deliquescence-resistant cesium iodide,crystal film and preparation method thereof - Google Patents
A kind of Deliquescence-resistant cesium iodide,crystal film and preparation method thereof Download PDFInfo
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- CN107164734A CN107164734A CN201710427438.1A CN201710427438A CN107164734A CN 107164734 A CN107164734 A CN 107164734A CN 201710427438 A CN201710427438 A CN 201710427438A CN 107164734 A CN107164734 A CN 107164734A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0694—Halides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
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Abstract
The invention discloses a kind of Deliquescence-resistant cesium iodide,crystal film and preparation method thereof, belong to scintillator detector technical field.The present invention is successively coated with the aluminium film of cesium iodide,crystal film and Nano grade by using vacuum thermal evaporation on substrate, because aluminium film can form the aluminum oxide of densification in humid air, moisture in air is effectively prevented to enter cesium iodide,crystal film, therefore the present invention can overcome cesium iodide,crystal film to hold deliquescent defect, it is to avoid influence of the deliquescence to performance indications such as the light conversion efficiencies and spatial resolution of cesium iodide,crystal film；Aluminium film has that adhesive ability is strong, the hard advantage such as wear-resisting of matter, can be effectively prevented from cesium iodide,crystal film and sustain damage；In addition, preparation technology of the present invention is simple controllable, with low cost, be conducive to industrialized production.
Description
Technical field
The invention belongs to scintillator detector technical field, more particularly to a kind of cesium iodide,crystal with moisture barrier properties is thin
Film and preparation method thereof.
Background technology
With the development of X-ray detection technology, scintillator detector turn into research at present it is most hot, using a best class X
Ray image detector.Scintillator detector is that have x-ray photon being converted into visible ray light by using scintillator material
The special performance of son, then be combined with highly developed visible images Detection Techniques, and then realize more satisfactory X ray picture
As detection.At present, scintillator detector is widely used in fields such as medical treatment, industry, security protections, such as in medical treatment side
The medical procedure image digitazations such as face enables to intervene, had an X-rayed, radiography；Non-Destructive Testing can be realized in industrial aspect, it is lossless
Flaw detection, expiloration of coal mines；It can be used in the safety inspection in many places such as subway, airport and customs in terms of security protection.So, dodge
The application of bright bulk detector is developing national economy, ensures that people's health is made that major contribution.
X-ray is mainly converted to recordable visible ray by the effect of scintillation material, therefore, the conversion efficiency of scintillation material
With light production capacity and other specification follow-up optical signal can be influenceed to read.In the prior art, mainly use with cesium iodide,crystal, mix
Thallium sodium iodide is used as scintillation material for the scintillation crystal of representative.And among a series of this scintillation crystal, cesium iodide,crystal is because of it
Photoyield is high, light conversion efficiency is good, easily carries out Spectral matching with CCD, with plasticity, and production cost is relatively low
Excellent properties, are most widely used in scintillator X-ray detector.Thus, relevant cesium iodide,crystal thin film preparation process
Research is also of increased attention.For example：Application No. CN 200910060112.5 Chinese patent《Mix thallium iodate
A kind of preparation method of caesium (CsI: Tl) film》, Application No. CN 201110442455.5 Chinese patent《Micro-column structure CsI
(Tl) preparation method and applications of X-ray scintillation conversion screen》, Application No. CN 201310269684.0 Chinese patent《Mix
Thallium cesium iodide film surface defects processing method》, Application No. CN 201310499469.X Chinese patent《A kind of thallium mixed
Cesium iodide laminated film and preparation method thereof》The preparation technology of cesium iodide,crystal film is disclosed Deng patent document, and is caused
Power is in its performance of raising.However, because traditional thermal evaporation coating process prepares the gained easy absorption air of cesium iodide,crystal film
In hydrone and occur deliquescence phenomenon, and deliquescence can further influence the pattern and shape of cesium iodide,crystal film surface crystal grain
Into the crystal orientation of crystal, the reduction of the performances such as the light conversion efficiency and spatial resolution of cesium iodide,crystal film is most caused at last.Cause
This, needs a kind of solution deliquescent method of cesium iodide,crystal film badly so that the other light conversion properties of its film-grade can keep excellent,
The indexs such as overall performance and service life of the solution of this technical problem for improving X-ray detector are significant.
The content of the invention
The technical problems to be solved by the invention are：There is provided a kind of cesium iodide,crystal film with moisture resistance characteristic and its
Preparation method, it is ensured that cesium iodide,crystal film light transformational can keep excellent, and then be conducive to improving the property of X-ray detector
Can index.
To achieve these goals, the present invention is adopted the following technical scheme that：
On the one hand, the invention provides a kind of Deliquescence-resistant cesium iodide,crystal film, it is characterised in that including：Mix thallium iodate
Caesium film and the aluminium film being deposited thereon, the aluminium film form fine and close damp-proof layer on cesium iodide,crystal film.
Further, the thickness of aluminium film is 200~300nm.
On the other hand, the invention provides a kind of preparation method of Deliquescence-resistant cesium iodide,crystal film, it is characterised in that adopts
With vacuum thermal evaporation cesium iodide,crystal film aluminum film again is first coated with substrate surface.
Further, the thickness of aluminium film is 200~300nm.
Further, the preparation method of presently disclosed Deliquescence-resistant cesium iodide,crystal film, specifically includes following steps：
Step A：Cesium iodide,crystal powder is placed on navicular evaporation source, the substrate of clean dried is then placed in the boat
Objective table above shape evaporation source, under vacuum conditions, heating navicular evaporation source cause cesium iodide,crystal powder to evaporate, and pass through rotation
Evaporation is coated with cesium iodide,crystal film in substrate surface；
Step B：Air pressure in reaction unit is recovered to normal pressure, using aluminium as evaporation source, plating then is made in step A
The substrate for having cesium iodide,crystal film is placed in objective table above aluminium, and so that is coated with the one side and aluminium of cesium iodide,crystal film
It is oppositely arranged, under vacuum conditions, heating evaporation source causes aluminium to evaporate, by rotating evaporation in cesium iodide,crystal film surface
Aluminum film.
Specifically, cesium iodide,crystal powder is mixed to form by CsI crystal and TlI crystal in the technical program.
Specifically, in the step A of the technical program the air pressure of vacuum environment 1 × 10-3To 3 × 10-3In the range of Pa.
Specifically, in the step A of the technical program mode of heating particular by evaporation source galvanization so that heat steam
Stimulating food matter, evaporation current value is 100A~120A.
Specifically, the vertical range of substrate distance navicular evaporation source is 15~30 centimetres in the step A of the technical program.
Specifically, the substrate speed of rotation is 25~35 revs/min when evaporation is rotated in the step A of the technical program.
Specifically, evaporation time is 90~120 minutes in the step A of the technical program.
Specifically, in the step B of the technical program the air pressure of vacuum environment 8 × 10-3To 3 × 10-3Pa。
Specifically, in the step B of the technical program mode of heating particular by evaporation source galvanization so that heat steam
Stimulating food matter, evaporation current value is 90A~120A.
Specifically, the substrate speed of rotation is 25~35 revs/min when evaporation is rotated in the step B of the technical program.
Specifically, evaporation time is 10~15 seconds in the step B of the technical program.
Specifically, the technical program also includes before step A：The cleaning of substrate, specifically using acetone soln, anhydrous second
Alcohol and deionized water are cleaned by ultrasonic respectively as cleaning fluid, are dried up after cleaning using nitrogen.
Preferably, the vacuum thermal evaporation deposition of cesium iodide,crystal film is fast in the step A of the technical program
Rate is 1 nanometer~1.5 nm/secs.
Compared with prior art, the present invention has the advantages that：
The present invention is coated with the aluminium film of Nano grade by using vacuum thermal evaporation on cesium iodide,crystal film, due to aluminium
Film can form the aluminum oxide of densification in humid air, effectively prevent moisture in air from entering cesium iodide,crystal film, because
This present invention can overcome cesium iodide,crystal film to hold deliquescent defect, it is to avoid deliquescence turns to the light of cesium iodide,crystal film
Change the influence of the performance indications such as efficiency and spatial resolution；Aluminium film has that adhesive ability is strong, the hard advantage such as wear-resisting of matter, can be effective
Ground avoids cesium iodide,crystal film from sustaining damage；In addition, preparation technology of the present invention is simple controllable, with low cost, be conducive to industry
Metaplasia is produced.
Brief description of the drawings
Fig. 1 is the structural representation and light path principle figure of Deliquescence-resistant cesium iodide,crystal film provided by the present invention；
Fig. 2 is the steady-state fluorescence of Deliquescence-resistant cesium iodide,crystal film provided by the present invention and traditional cesium iodide,crystal film
Spectrum comparison diagram.
Embodiment
Technical scheme is elaborated by the following examples and with reference to Figure of description, while to the present invention's
Principle and characteristic are described further.The present embodiment is served only for explaining the present invention, is not intended to limit the scope of the present invention.
Embodiment 1：
A kind of preparation method of Deliquescence-resistant cesium iodide,crystal film, specifically includes following steps：
Step A：
This implementation is that 99.99% CsI crystal and TlI crystal are mixed to form cesium iodide,crystal powder using purity, will
Above-mentioned cesium iodide,crystal powder is placed on molybdenum boat, and the substrate of clean dried then is placed in into the work rest above molybdenum boat at 30cm
On, close bell jar and cause system to turn into sealed environment, extraction system vacuum to 3 × 10-3, regulation substrate rotating speed is 30r/min, so
Afterwards using molybdenum boat as resistance heating source, by being passed through 120A electric current to molybdenum boat so that cesium iodide,crystal powder evaporates, substrate is protected
Normal temperature is held, evaporation time is 90 minutes；CsI molecules and TlI molecules are adsorbed rapidly in evaporation process by substrate, and aggregation forms brilliant
Core, nucleus formation crystal grain, crystal grain continued growth increasingly generates continuous cesium iodide,crystal film；Thallium iodate is mixed in the present embodiment
The thickness of caesium film is 7 microns；
Substrate selects simple glass slide in this implementation, and carries out cutting operation to substrate so that the size of substrate is
2.0cm×2.5cm.According to this area general knowledge, backing material can use any suitable material, it is not limited to this reality
Apply a material therefor；Because the surface adhesion of glass slide many pollutants, and these pollutants can be directly or indirectly
Consistency, mechanical characteristic and the combination between glass slide of the follow-up obtained cesium iodide,crystal film of influence.Therefore, it is
Film quality is reduced caused by reduction pollutant as far as possible, and the solution that this implementations is prepared using dichromic acid with sulfuric acid is to glass load glass
Piece is pre-processed, and then glass slide is sequentially placed into absolute ethyl alcohol, acetone and deionized water, set using ultrasonic cleaning
It is standby to be cleaned, it is placed in after the completion of cleaning in hot air circulation drying oven and processing is dried, it is final to obtain glass that is clean, drying
Slide.
The present embodiment uses molybdenum boat as the evaporation source in step A, in order to prevent the impurity in molybdenum boat to cesium iodide,crystal
Powder is polluted, and also molybdenum boat is polished before preparation manipulation, washing and drying treatment.
Step B：
Air pressure in reaction unit is recovered to normal pressure, using aluminium wire as evaporation source, and aluminium wire warm table electricity is suspended in
On extremely, the obtained substrates of cesium iodide,crystal film that are coated with of step A are then placed in work rest above aluminium wire, and to be coated with to mix thallium
The one side of cesium iodide film is oppositely arranged with aluminium, close bell jar cause system turn into sealed environment, extraction system vacuum to 5 ×
10-3, regulation substrate rotating speed is 30r/min, then makes molybdenum boat by the electric current that 100A is passed through to molybdenum boat as resistance heating source
The evaporation of cesium iodide,crystal powder is obtained, the temperature remains within the normal range for substrate, evaporation time is 10 seconds；Aluminium atom is rapid by substrate in evaporation process
Absorption, aggregation forms nucleus, and nucleus formation crystal grain, crystal grain continued growth is increasingly generated continuously in cesium iodide,crystal film surface
Aluminium film；The thickness of aluminium film is 240nm in the present embodiment；
The structural representation of Deliquescence-resistant cesium iodide,crystal film is made as shown in figure 1, because aluminium film is to visible in the present embodiment
The transmitance of light is essentially 0, and very superior to the through performance of X-ray, therefore Deliquescence-resistant cesium iodide,crystal film of the present invention exists
With when, X-ray should be caused to be projected after aluminium film injection from substrate, can so ensure the overall photopermeability of device,
And do not influence the light conversion efficiency of device.
Embodiment 2：
The preparation method of traditional cesium iodide,crystal film, specifically includes following steps：
This implementation is that 99.99% CsI crystal and TlI crystal are mixed to form cesium iodide,crystal powder using purity, will
Above-mentioned cesium iodide,crystal powder is placed on molybdenum boat, and the substrate of clean dried then is placed in into the work rest above molybdenum boat at 30cm
On, close bell jar and cause system to turn into sealed environment, extraction system vacuum to 3 × 10-3, regulation substrate rotating speed is 30r/min, so
Afterwards using molybdenum boat as resistance heating source, by being passed through 120A electric current to molybdenum boat so that cesium iodide,crystal powder evaporates, substrate is protected
Normal temperature is held, evaporation time is 90 minutes；CsI molecules and TlI molecules are adsorbed rapidly in evaporation process by substrate, and aggregation forms brilliant
Core, nucleus formation crystal grain, crystal grain continued growth increasingly generates continuous cesium iodide,crystal film；Thallium iodate is mixed in the present embodiment
The thickness of caesium film is 7 microns；
Substrate selects simple glass slide in this implementation, and carries out cutting operation to substrate so that the size of substrate is
2.0cm×2.5cm.According to this area general knowledge, backing material can use any suitable material, it is not limited to this reality
Apply a material therefor；Because the surface adhesion of glass slide many pollutants, and these pollutants can be directly or indirectly
Consistency, mechanical characteristic and the combination between glass slide of the follow-up obtained cesium iodide,crystal film of influence.Therefore, it is
Film quality is reduced caused by reduction pollutant as far as possible, and the solution that this implementations is prepared using dichromic acid with sulfuric acid is to glass load glass
Piece is pre-processed, and then glass slide is sequentially placed into absolute ethyl alcohol, acetone and deionized water, set using ultrasonic cleaning
It is standby to be cleaned, it is placed in after the completion of cleaning in hot air circulation drying oven and processing is dried, it is final to obtain glass that is clean, drying
Slide.
The present embodiment uses molybdenum boat as the evaporation source in step A, in order to prevent the impurity in molybdenum boat to cesium iodide,crystal
Powder is polluted, and also molybdenum boat is polished before preparation manipulation, washing and drying treatment.
Cesium iodide,crystal film is made to embodiment 2 first and carries out steady-state fluorescence spectrum test, testing process is by swashing
Light emitting source is exposed to after film sample, then passes through the steady-state fluorescence spectrum test result that subsequent optical path obtains correspondence output light.So
Deliquescence-resistant cesium iodide,crystal film is made in embodiment 1 afterwards cesium iodide,crystal film is made with embodiment 2 and be in humidity respectively
Placed in 76% humid air 48 hours, steady-state fluorescence spectrum test then is carried out to above-mentioned two sample again.
The steady-state fluorescence spectrum test result of above-mentioned three is as shown in Fig. 2 as can be seen from Figure 2：Tradition mixes thallium iodate
Caesium film is placed after 48 hours in humid air, and the light conversion efficiency generation to X-ray due to deliquescence declines to a great extent,
Light conversion efficiency is reduced to 16% or so of the cesium iodide,crystal film that also non-deliquescence is just made；And cesium iodide,crystal of the present invention is thin
Film is placed after 48 hours in humid air, thin for the cesium iodide,crystal that also non-deliquescence is just made to the light conversion efficiency of X-ray
95% or so of film.Above-mentioned comparing result can be drawn：After the influence reflected in view of aluminium film light absorbs, prepared by the present invention
Deliquescence-resistant cesium iodide,crystal film due to Deliquescence-resistant layer addition, restrained effectively cesium iodide,crystal film deliquescence phenomenon
Occur, it is to avoid the defect present in cesium iodide,crystal film deliquescence.
Above-mentioned embodiment is only schematical, rather than restricted, and one of ordinary skill in the art exists
Under the enlightenment of the present invention, in the case of present inventive concept and scope of the claimed protection is not departed from, many shapes can be also made
Formula, these are belonged within the protection of the present invention.
Claims (10)
1. a kind of Deliquescence-resistant cesium iodide,crystal film, it is characterised in that including：Cesium iodide,crystal film and the aluminium being deposited thereon
Film, the aluminium film forms fine and close damp-proof layer on cesium iodide,crystal film.
2. a kind of Deliquescence-resistant cesium iodide,crystal film according to claim 1, it is characterised in that the thickness of the aluminium film is
200~300nm.
3. a kind of preparation method of Deliquescence-resistant cesium iodide,crystal film, specifically includes following steps：
Step A：Cesium iodide,crystal powder is placed on navicular evaporation source, the substrate of clean dried then is placed in into the navicular steams
Rise top objective table, under vacuum conditions, and heating navicular evaporation source causes cesium iodide,crystal powder to evaporate, and is deposited by rotating
Cesium iodide,crystal film is coated with substrate surface；
Step B：Air pressure in reaction unit is recovered to normal pressure, evaporation source, under vacuum conditions, heating evaporation are used as using aluminium
Source causes aluminium to evaporate, by rotating evaporation in cesium iodide,crystal film surface aluminum film, and finally obtained Deliquescence-resistant mixes thallium iodine
Change caesium film.
4. a kind of preparation method of Deliquescence-resistant cesium iodide,crystal film according to claim 3, it is characterised in that the step
The air pressure of vacuum environment is 1 × 10 in rapid A-3~3 × 10-3In the range of Pa.
5. a kind of preparation method of Deliquescence-resistant cesium iodide,crystal film according to claim 3, it is characterised in that the step
Heating evaporation source is that design parameter is specific as follows by being heated to evaporation source galvanization in rapid A：Evaporation current value is 100A
~120A, evaporation time is 90~120 minutes；The vertical range of substrate distance navicular evaporation source is 15~30 in the step A
Centimetre.
6. a kind of preparation method of Deliquescence-resistant cesium iodide,crystal film according to claim 4 or 5, it is characterised in that institute
The vacuum thermal evaporation sedimentation rate for stating cesium iodide,crystal film in step A is 1 nanometer~1.5 nm/secs.
7. a kind of preparation method of Deliquescence-resistant cesium iodide,crystal film according to claim 3, it is characterised in that the step
The air pressure of vacuum environment is 8 × 10 in rapid B-3To 3 × 10-3Pa。
8. a kind of preparation method of Deliquescence-resistant cesium iodide,crystal film according to claim 3, it is characterised in that the step
Evaporation current value is 90A~120A in rapid B, and evaporation time is 10~15 seconds.
9. the preparation method of a kind of Deliquescence-resistant cesium iodide,crystal film according to claim 3, it is characterised in that rotation is steamed
The substrate speed of rotation is 25~35 revs/min during plating.
10. a kind of preparation method of Deliquescence-resistant cesium iodide,crystal film according to any one of claim 3 to 9, its feature
It is, the thickness of the aluminium film is 200~300nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342688A (en) * | 2018-03-19 | 2018-07-31 | 电子科技大学 | A kind of cesium iodide,crystal laminated film and preparation method thereof |
| CN110359023A (en) * | 2019-07-26 | 2019-10-22 | 同济大学 | Pixellated structure ZnO:Ga monocrystal nano rod array α particle scintillation conversion screen and its preparation method and application |
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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 |
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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 |
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| 张红柳: "CsI:TI闪烁薄膜的工艺制备和光学特性的研究", 《中国优秀硕士学位论文全文数据库》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342688A (en) * | 2018-03-19 | 2018-07-31 | 电子科技大学 | A kind of cesium iodide,crystal laminated film and preparation method thereof |
| CN110359023A (en) * | 2019-07-26 | 2019-10-22 | 同济大学 | Pixellated structure ZnO:Ga monocrystal nano rod array α particle scintillation conversion screen and its preparation method and application |
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