CN104164649A - Preparation method for large-area lead iodide thick film and implementation equipment thereof - Google Patents
Preparation method for large-area lead iodide thick film and implementation equipment thereof Download PDFInfo
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- CN104164649A CN104164649A CN201310181516.6A CN201310181516A CN104164649A CN 104164649 A CN104164649 A CN 104164649A CN 201310181516 A CN201310181516 A CN 201310181516A CN 104164649 A CN104164649 A CN 104164649A
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Abstract
The invention discloses a preparation method for a large-area lead iodide thick film and implementation equipment thereof. According to the invention, in a vacuum cavity of the equipment, the raw material high purity lead iodide powder is spread on a raw material carrier graphite sheet, which is placed on a flat heater, a directional heat dissipation plate equipped with a substrate at the bottom is supported by a quartz block over the raw material, in an environment with a vacuum degree of 10<-1>Pa-10<-5>Pa, starting the flat heater to heat the raw material to gasify it, and the raw material gas condenses and deposits at the low temperature substrate, thus forming the dense lead iodide polycrystal film. With the method and equipment provided by the invention, the lead iodide polycrystal thick film with a thickness of 50-1000 micrometers, an area of 5*5cm<2>-50*50cm<2>, uniform thickness and excellent properties can be prepared on the substrate. Also, the preparation process is simple and low in cost, thus being suitable for industrial mass production.
Description
Technical field
The present invention relates to the technology of preparing of large-area compound semiconductor polycrystalline film, particularly relate to preparation method and the equipment of preparation big area lead iodide polycrystalline thick film.
Background technology
Lead iodide (PbI
2) there is very important application prospect as a kind of room temperature ionizing rays detection and the direct transition material of digital flat panel x-ray imaging, the large (Z of ordination number of lead iodide material
pb=82, Z
i=53), energetic ray (as X ray, gamma-rays) is had to very high stopping power and large optical density, the large (E of energy gap
g=2.3-2.5eV), intrinsic resistivity is high, and the device creepage of being made up of it is little, and noise is low, and can normally work in room temperature to a 110 DEG C temperature range.Detect the injury to human body owing to needing to reduce as much as possible ray energy and dosage in human medical radial imaging to reduce medical science, therefore high resistivity, the lead iodide material of low-leakage current and low device noise is highly suitable for the application in this field.In view of above feature, large-area lead iodide polycrystalline thick-film material has become in recent years directly one of novel focus research material of conversion hysteria digital flat panel X-ray detector.
Large-area lead iodide polycrystalline thick film generally refers to that area is at 5 × 5cm
2above, thickness reaches 50 microns of above lead iodide polycrystalline film.The method of preparing lead iodide thick film mainly contains thermal evaporation, solution method and silk screen print method at present.Thermal evaporation can be prepared the polycrystalline thick film of excellent performance, but prior art is to adopt small area point-like evaporation source to prepare lead iodide thick film, cause prepared large-area polycrystalline thick film homogeneity poor, and along with the variation of underlayer temperature, the crystalline orientation of thick film and grain-size will occur obviously to change, cause density and the conversion performance of polycrystalline film greatly to reduce (M. Schieber, N. Zamoshchik, O. Khakhan, Journal of Crystal Growth 310 (2008) 3168 – 3173).The lead iodide polycrystalline film that adopts solution method to prepare, be difficult to obtain big area thick films more than hundred micron thickness, and easily introduce various impurity, the various defects that produced by impurity have seriously reduced the detection performance of material, the necessary annealed processing of the polycrystalline film of growth in addition, and different annealing processs has considerable influence to the performance of polycrystalline film, in solution, carry out crystallization and produce polycrystalline film, solution can cause corrosion in various degree to crystalline substrate, thereby affect performance (the J.P. Ponpon of device, M. Amann, Thin Solid Films 394 (2001), 277-283).Adopt silk screen print method to prepare lead iodide thick film by coating processes, can realize the preparation of hundred microns of thick films, but in preparation process, adopt and organic solvent and lead iodide powder are prepared to certain density coating raw material be coated on substrate, prepare lead iodide thick film by low-temperature heat treatment again, prepared lead iodide thick film crystalline-granular texture is imperfect, size is little, grain orientation is poor, and crystal grain gap is large, it between gap, is residual organic matter filling, that greatly reduces current carrier transports efficiency (as document Min-seok Yun, Sung-ho Cho, Rena Lee, Japanese Journal of Applied Physics 49 (2010) 041801).Above method and technology are not the Perfected process of the big area lead iodide thick film of preparation Stability Analysis of Structures, excellent performance, industrial production is badly in need of the new method of preparing big area lead iodide thick-film material of exploitation, to meet the needs of manufacturing the direct conversion layer of big area energetic ray flat panel detector.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, a kind of preparation method and facilities and equipments thereof of new big area lead iodide thick film be provided, for stability and high efficiency on substrate prepare big area, good uniformity, high performance lead iodide thick-film material.
The present invention is the one improvement of being prepared by thermal evaporation to lead iodide polycrystalline film, with respect to traditional thermal evaporation, the present invention is improving polycrystalline film thickness and homogeneity, increase mould material deposition area coverage, the crystalline orientation suppressing in polycrystalline film process of growth changes and grain-size change, and the aspect of the density of raising polycrystalline thick film, preparation process condition and the method for lead iodide polycrystalline thick film are innovated.
Foregoing invention object of the present invention can realize by the big area lead iodide thick film preparation method of following technical proposals.Big area lead iodide thick film preparation method mainly comprises following preparation process:
(1) high-purity raw material iodate lead powder end (3) is laid in to raw material supporting body graphite plate (4) above, it is upper that raw material supporting body graphite plate is placed on panel heater (5), is placed in vacuum cavity (8);
(2) substrate (2) is closely arranged on to oriented heat dissipating plate (1) upper, and faces raw water level land and be placed in the top of raw material with quartz wedge (6) support oriented heat dissipating plate with substrate;
(3) apparatus body vacuum cavity is evacuated to 10
-1pa～10
-5pa, closing vacuum cavity valve makes vacuum cavity in air-tight state, then open panel heater heating raw materials is made it to the gasification that heats up, unstripped gas is being positioned at the lower substrate coagulating sedimentation of temperature above raw material, form fine and close lead iodide polycrystalline film, heating raw materials gasification temperature is 200 DEG C～500 DEG C;
(4) the lead iodide polycrystalline film that substrate coagulating sedimentation forms reaches after design thickness, closes heating system and makes the temperature of the lead iodide polycrystalline film in vacuum cavity be down to room temperature, obtains the lead iodide polycrystalline thick film of high quality, big area, densification.
In order to realize better object of the present invention, the present invention further takes following technical measures on the basis of technique scheme.
In technique scheme, described heating raw materials gasification temperature rise rate preferentially heats up with the speed that is not more than 5 DEG C/min.
In technique scheme, the temperature of described heating raw materials gasification, top-priority temperature range is 220 DEG C～300 DEG C.
In technique scheme, in vacuum cavity, adopt mechanical pump and molecular pump to be evacuated to 10
-1pa～10
-5pa, first vacuumizes with mechanical pump, then vacuumizes with molecular pump afterwards, and vacuum cavity is evacuated to 10
-1pa～10
-5pa.
In technique scheme, lead iodide polycrystalline film reaches after design thickness at vacuum state borehole cooling to room temperature, normally adopts the mode that continues to vacuumize to make the temperature of the lead iodide polycrystalline film in vacuum cavity be down to room temperature.
In technique scheme, conventionally needed before using as the glass of substrate to clean, be generally to adopt glass to be placed on and in ethanol or acetone, then to apply ultrasonic wave and clean, after having cleaned, put into vacuum drying oven and dry.First carry out ethanol ultrasonic cleaning, then carry out afterwards acetone ultrasonic cleaning, after twice ultrasonic cleaning is complete, put into vacuum drying oven and dry.
The above-mentioned big area lead iodide of the present invention thick film is preparation method can implement by equipment by the following technical programs: the structure of facilities and equipments mainly comprises: vacuum cavity (8), be positioned at the thermal baffle (7) of vacuum cavity, panel heater (5), raw material supporting body graphite plate (4), substrate (2), oriented heat dissipating plate (1) and quartzy back-up block (6), the vacuum-pumping system (9) being communicated with vacuum cavity (8), and temperature-measuring element is positioned at temperature survey and the Controlling System (10) at vacuum cavity temperature point place, on panel heater is placed at the bottom of vacuum chamber body cavity by thermal baffle, raw material supporting body graphite plate is positioned on panel heater, oriented heat dissipating plate by quartzy back-up block be placed in raw material carrier graphite plate directly over, substrate and oriented heat dissipating plate fit tightly, face the raw material on the supporting body graphite plate of below.
In above-mentioned facilities and equipments, the distance between oriented heat dissipating plate and the raw material carrier graphite plate of its below is preferably controlled at and can makes the lower surface of substrate and the upper surface at the high-purity iodate lead powder of raw material end keep the distance of 1 to 50 millimeter.
In above-mentioned facilities and equipments, panel heater, raw material carrier graphite plate and the substrate being positioned on oriented heat dissipating plate are preferably positioned at the cavity being surrounded by thermal baffle, quartzy back-up block and oriented heat dissipating plate, be that quartzy back-up block surrounds tubular, panel heater is placed in the cylindrical shell that quartzy back-up block surrounds.
In above-mentioned facilities and equipments, the temperature element of temperature survey and Controlling System is preferably placed on the edge of raw material, and is close to raw material carrier graphite plate.
Preparation method and the facilities and equipments thereof of big area lead iodide thick film provided by the invention, taking panel heater as thermal source, the high-purity iodate lead powder of raw material end is laid on raw material supporting body graphite plate, raw material supporting body graphite plate is placed on panel heater, panel heater makes to be laid in high-purity iodate lead powder end on graphite plate by thermal conduction and thermal radiation, and to obtain heating evaporation be equably gas phase, effectively overcome prior art small area point-like evaporation source and prepared the ununiformity that big area lead iodide thick film exists.Because fitting tightly, substrate is placed on oriented heat dissipating plate again, oriented heat dissipating plate is by upwards heat loss through radiation of its upper surface, make the substrate that is positioned at its below realize heat directional transmissions, substrate temperature field distribution is even, in the time that phase feed is transported to substrate in a vacuum and deposition growing goes out polycrystalline film on substrate, crystallization preferred orientation has obtained greatly improving, and then has improved the consistence of thick film crystallization homogeneity, bulk structure and performance.
The present invention takes the upper surface at the lower surface of substrate and the high-purity iodate lead powder of raw material end to keep the distance of 1 to 50 millimeter, it is the close together of raw material and substrate, it is short that gas phase atom or molecule arrive the absolute distance of substrate, therefore effectively reduce collision in the gas gas-phase objects transport process power loss to gas phase atom or molecule, make gas phase atom or molecule arrive substrate and make to there is higher energy, be conducive to nucleation and the growth of gas gas-phase objects on substrate, improved the density of polycrystalline film and the sticking power with substrate.Meanwhile, raw material and substrate distance are short, and thermograde is little, and temperature field is stable, can effectively overcome the change of crystalline orientation, improve the consistence of grain-size and crystalline orientation.
It is thermal source that the present invention adopts panel heater, and thermal source is single, greatly reduces complicacy and the equipment cost of system control.
Adopt the present invention can prepare area and reach 5 × 5cm
2to 50 × 50cm
2, thickness reaches the lead iodide polycrystalline film of 50～1000 microns, can be used for manufacturing the direct conversion layer of big area energetic ray flat panel detector.
Of the present invention open, greatly promote the progress of lead iodide polycrystalline film technology of preparing.
Brief description of the drawings
Fig. 1 is device structure schematic diagram of the present invention.
Fig. 2 is that the thickness of preparing on employing method and apparatus substrate of the present invention is the cross section stereoscan photograph of the big area lead iodide thick film of 659 microns.
Drawing is described as follows:
1-oriented heat dissipating plate; 2-substrate; The high-purity iodate lead powder of 3-raw material end; 4-raw material carrier graphite plate; 5-panel heater; 6-quartz back-up block; 7-thermal baffle; 8-vacuum cavity; 9-air-bleed system; 10-heating and temperature controlling system.
Embodiment
Provide embodiments of the invention below, and by embodiment, the present invention is further described specifically.Be necessary to be pointed out that at this; embodiment is only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention; the person skilled in the art in this field can make some nonessential improvement and adjustment is implemented according to the content of the invention described above, but this still belongs to protection scope of the present invention.
embodiment 1
The present embodiment is that to prepare area be 5 × 5cm
2, thickness is the lead iodide polycrystalline thick film of 700 microns.
The processing step of this example is as follows:
1, substrate 2 is placed in to ethanol ultrasonic cleaning 30 minutes, then puts into acetone ultrasonic cleaning 30 minutes, then put into vacuum drying oven and dry;
2, cleaned substrate is arranged on oriented graphite heat radiation plate 1, ensures that the upper surface of substrate and graphite radiating plate lower surface fit tightly to be conducive to heat radiation and temperature uniformity of substrates;
3,, by high-purity raw material iodate lead powder end (99.99%) 3 and be laid on the raw material carrier graphite plate 4 being positioned on panel heater 5, the area of raw material is about 6 × 6cm
2, thickness is between 0.5-1.3 millimeter; Temperature sensor being placed on to raw edges all contacts with graphite flake with raw material again;
4, support the radiating module that substrate is installed at four direction with quartzy back-up block 6, substrate is just to raw material, and the distance of the maintenance lower surface of substrate and the upper surface of raw material is 5 millimeters;
5, with mechanical pump and turbomolecular pump, vacuum cavity 8 is evacuated to 1.0 × 10 respectively
-4pa, closes and connects all valves of vacuum cavity, open panel heater with the temperature rise rate of 1 DEG C/min to heating raw materials to 250 DEG C, and keep 30 minutes, then naturally cool in a vacuum room temperature and can take out sample.
embodiment 2
The present embodiment is that to prepare area be 50 × 50cm
2, thickness is the lead iodide polycrystalline thick film of 500 microns.
The technique of the technique of the present embodiment and embodiment 1 is basic identical, and difference is that the area that raw material is laid on raw material carrier graphite plate 4 is about 52 × 52cm
2, thickness is between 0.5-1.0 millimeter, and the distance of the lower surface of substrate and the upper surface of raw material is 50 millimeters, and the vacuum tightness of vacuum cavity 8 is 5.0 × 10
-2pa, the temperature rise rate of panel heater is 5 DEG C/min, heating raw materials to 300 DEG C, and keep 60 minutes.
embodiment 3
The present embodiment is that to prepare area be 20 × 20cm
2, thickness is the lead iodide polycrystalline thick film of 1000 microns.
The technique of the technique of the present embodiment and embodiment 1 is basic identical, and difference is that the area that raw material is laid on raw material carrier graphite plate 4 is about 22 × 22cm
2, thickness is between 1.1-2.0 millimeter, and the distance of the lower surface of substrate and the upper surface of raw material is 30 millimeters, and the vacuum tightness of vacuum cavity 8 is 1.0 × 10
-5pa, the temperature rise rate of panel heater is 3 DEG C/min, heating raw materials to 220 DEG C, and keep 40 minutes.
Claims (10)
1. a preparation method for big area lead iodide thick film, is characterized in that comprising following preparation process:
High-purity raw material iodate lead powder end is laid on raw material supporting body graphite plate, and raw material supporting body graphite plate is placed on panel heater, is placed in vacuum cavity; Substrate is closely arranged on oriented heat dissipating plate, and supports oriented heat dissipating plate and face raw water level land and be placed in substrate the top of raw material with quartz wedge; Vacuum cavity is evacuated to 10
-1pa～10
-5pa, closing vacuum cavity valve makes vacuum cavity in air-tight state, then open panel heater heating raw materials is made it to the gasification that heats up, unstripped gas is being positioned at the lower substrate coagulating sedimentation of temperature above raw material, form fine and close lead iodide polycrystalline film, heating raw materials gasification temperature is 200 DEG C～500 DEG C; The lead iodide polycrystalline film that substrate coagulating sedimentation forms reaches after design thickness, closes heating system and makes the temperature of the lead iodide polycrystalline film in vacuum cavity be down to room temperature, obtains the lead iodide polycrystalline thick film of high quality, big area, densification.
2. the preparation method of big area lead iodide thick film according to claim 1, is characterized in that the temperature rise rate of heating raw materials gasification is not more than 5 DEG C/min.
3. the preparation method of big area lead iodide thick film according to claim 1, is characterized in that heating raw materials gasification temperature is 200 DEG C～500 DEG C.
4. the preparation method of big area lead iodide thick film according to claim 1, is characterized in that vacuum cavity adopts mechanical pump and molecular pump to be evacuated to 10
-1pa～10
-5pa.
5. the preparation method of big area lead iodide thick film according to claim 1, is characterized in that substrate is of a size of 5 × 5cm
2to 50 × 50cm
2.
6. according to the preparation method of the big area lead iodide thick film one of claim 1 to 5 Suo Shu, it is characterized in that before using, using ethanol ultrasonic cleaning and/or acetone ultrasonic cleaning as the glass of substrate, after cleaning, put into vacuum drying oven and dry.
7. the facilities and equipments of the big area lead iodide thick film preparation method described in one of claim 1 to 6, it is characterized in that comprising: vacuum cavity (8), be positioned at the thermal baffle (7) of vacuum cavity, panel heater (5), raw material supporting body graphite plate (4), substrate (2), oriented heat dissipating plate (1) and quartzy back-up block (6), the vacuum-pumping system (9) being communicated with vacuum cavity, and temperature-measuring element is positioned at temperature survey and the Controlling System (10) at vacuum cavity temperature point place, on panel heater is placed at the bottom of vacuum chamber body cavity by thermal baffle, raw material supporting body graphite plate is positioned on panel heater, oriented heat dissipating plate by quartzy back-up block be placed in raw material carrier graphite plate directly over, substrate and oriented heat dissipating plate fit tightly, face the raw material on the supporting body graphite plate of below.
8. big area lead iodide thick film preparation method's according to claim 7 facilities and equipments, is characterized in that the distance between oriented heat dissipating plate and the raw material carrier graphite plate of its below is to make the lower surface of substrate and the upper surface at the high-purity iodate lead powder of raw material end keep the distance of 1 to 50 millimeter.
9. big area lead iodide thick film preparation method's according to claim 7 facilities and equipments, is characterized in that panel heater, raw material carrier graphite plate and the substrate that is positioned on oriented heat dissipating plate is positioned at the cavity being surrounded by thermal baffle, quartzy back-up block and oriented heat dissipating plate.
10. big area lead iodide thick film preparation method's according to claim 7 facilities and equipments, the temperature element that it is characterized in that temperature survey and Controlling System (10) is placed on edge and the raw material carrier graphite plate of raw material and is close to.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107574409A (en) * | 2017-11-02 | 2018-01-12 | 南京大学 | A kind of high-purity lead iodide films preparation method of morphology controllable |
| CN107881472A (en) * | 2017-11-23 | 2018-04-06 | 鲁东大学 | A kind of CsPbI3The preparation method of film |
| CN108735830A (en) * | 2018-07-18 | 2018-11-02 | 成都信息工程大学 | Driving radiation detector and preparation method certainly based on Schottky electrode and lead iodide |
| CN109585477A (en) * | 2018-10-31 | 2019-04-05 | 奕瑞影像科技（太仓）有限公司 | Flat-panel detector structure and preparation method thereof |
| CN109735898A (en) * | 2018-11-27 | 2019-05-10 | 成都信息工程大学 | A kind of preparation method of the lead iodide polycrystalline film based on Vacuum sublimation |
| CN110230039A (en) * | 2019-07-02 | 2019-09-13 | 中南大学 | A kind of method of single layer molybdenum sulfide regulation lead iodide growth |
| CN114890459A (en) * | 2022-05-10 | 2022-08-12 | 黑龙江省科学院石油化学研究院 | Preparation and purification method of lead iodide serving as raw material of perovskite solar cell |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107574409A (en) * | 2017-11-02 | 2018-01-12 | 南京大学 | A kind of high-purity lead iodide films preparation method of morphology controllable |
| CN107881472A (en) * | 2017-11-23 | 2018-04-06 | 鲁东大学 | A kind of CsPbI3The preparation method of film |
| CN108735830A (en) * | 2018-07-18 | 2018-11-02 | 成都信息工程大学 | Driving radiation detector and preparation method certainly based on Schottky electrode and lead iodide |
| CN108735830B (en) * | 2018-07-18 | 2024-01-30 | 成都信息工程大学 | Self-driven radiation detector based on Schottky electrode and lead iodide and preparation method |
| CN109585477A (en) * | 2018-10-31 | 2019-04-05 | 奕瑞影像科技（太仓）有限公司 | Flat-panel detector structure and preparation method thereof |
| CN109585477B (en) * | 2018-10-31 | 2021-03-19 | 奕瑞影像科技（太仓）有限公司 | Flat panel detector structure and preparation method thereof |
| CN109735898A (en) * | 2018-11-27 | 2019-05-10 | 成都信息工程大学 | A kind of preparation method of the lead iodide polycrystalline film based on Vacuum sublimation |
| CN110230039A (en) * | 2019-07-02 | 2019-09-13 | 中南大学 | A kind of method of single layer molybdenum sulfide regulation lead iodide growth |
| CN114890459A (en) * | 2022-05-10 | 2022-08-12 | 黑龙江省科学院石油化学研究院 | Preparation and purification method of lead iodide serving as raw material of perovskite solar cell |
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Application publication date: 20141126 |