CN116249361A - Manufacturing method of X-ray detector - Google Patents
Manufacturing method of X-ray detector Download PDFInfo
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- CN116249361A CN116249361A CN202211702773.5A CN202211702773A CN116249361A CN 116249361 A CN116249361 A CN 116249361A CN 202211702773 A CN202211702773 A CN 202211702773A CN 116249361 A CN116249361 A CN 116249361A
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- ito glass
- ball milling
- manufacturing
- ray detector
- perovskite layer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
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Abstract
The invention discloses a manufacturing method of an X-ray detector. According to the invention, the anisotropic conductive adhesive is adopted as the bonding layer, and the perovskite layer and the ITO glass substrate are heterogeneous integrated, so that the problem of the falling of the perovskite layer caused by different thermal expansion coefficients of the perovskite layer and the substrate can be well avoided. Meanwhile, ACA glue is used as a bonding layer, so that stronger bonding force can be provided, and the manufactured device has better mechanical stability.
Description
Technical Field
The invention relates to the technical field of X-ray detectors, in particular to a manufacturing method of an X-ray detector.
Background
Flat panel X-ray detectors are of great interest in various applications such as medical imaging, non-destructive testing and security inspection. Halide perovskite is promising for use in semiconductor direct X-ray detectors due to its high X-ray blocking capability, low trap density, and long carrier lifetime characteristics. The halide perovskite currently being widely studied has shown great advantage and wide prospect in semiconductor direct detection. At present, the semiconductor area array detector is mainly manufactured in two modes, namely, an X-ray absorption layer is uniformly manufactured on a substrate directly, and the X-ray absorption layer is combined with the substrate in a heterogeneous integration mode. However, since the perovskite layer and the substrate have very different coefficients of thermal expansion, the phenomenon that the substrate and the perovskite layer are separated or air holes are generated due to expansion and shrinkage easily occurs in the annealing process, and the application of the perovskite layer is seriously affected. At the same time, some substrates tend not to be resistant to high temperatures, which greatly limits the annealing temperature of the perovskite layer.
Disclosure of Invention
The invention provides a manufacturing method of an X-ray detector, which solves the technical problem that in the prior art, phenomena of falling off or air holes are easily generated between a substrate and a perovskite layer due to expansion and shrinkage in the annealing process.
The invention provides a manufacturing method of an X-ray detector, which comprises the following steps:
immersing ITO glass into acetone for cleaning;
weighing FAI, MAI, pbI according to a preset proportion 2 Placing the mixture into a ball milling tank, and adding an antisolvent into the ball milling tank for ball milling;
drying the slurry after ball milling;
putting the dried powder into a tablet press to prepare a perovskite layer;
dropping ACA glue on the cleaned ITO glass;
covering the perovskite layer on ITO glass with ACA glue;
and annealing the ITO glass covered with the perovskite layer, and cooling to room temperature.
Specifically, before the ITO glass is immersed in acetone for cleaning, the method further comprises:
adding deionized water and detergent into the ITO glass, ultrasonically cleaning for 30min, and then flushing with deionized water.
Specifically, after the ITO glass is washed by immersing in acetone, the method further comprises:
taking out the cleaned ITO glass, flushing the ITO glass with absolute ethyl alcohol, blow-drying the ITO glass with a nitrogen gun, and treating the ITO glass with Plasma for 5min.
Specifically, the adding of the antisolvent into the ball milling tank for ball milling comprises the following steps:
and adding an ethyl acetate antisolvent into the ball milling tank, and ball milling for 12h under the condition of 600 r/min.
Specifically, the drying treatment of the slurry after ball milling comprises the following steps:
transferring the slurry after ball milling to a vacuum drying oven, and drying overnight at 80 ℃.
Specifically, after the ACA paste is dropped on the cleaned ITO glass, the method further includes:
and scraping the ACA glue with a scraper to be smooth.
Specifically, the annealing the ITO glass covered with the perovskite layer, and then cooling to room temperature, includes:
transferring the ITO glass covered with the perovskite layer to a hot stage at 150 ℃, annealing for 15min, and naturally cooling to room temperature.
One or more technical schemes provided by the invention have at least the following technical effects or advantages:
according to the invention, the perovskite layer and the ITO glass substrate are heterogeneous integrated by adopting the anisotropic conductive adhesive (ACA adhesive) as the bonding layer, so that the problem of the falling of the perovskite layer caused by different thermal expansion coefficients of the perovskite layer and the substrate can be well avoided. Meanwhile, ACA glue is used as a bonding layer, so that stronger bonding force can be provided, and the manufactured device has better mechanical stability.
Drawings
FIG. 1 is a flow chart of a method for fabricating an X-ray detector according to an embodiment of the present invention;
FIG. 2 is an optical microscope image of ACA glue in an embodiment of the present invention;
FIG. 3 is a graph showing tensile stress test results of ITO glass/ACA gel and ITO glass/ACA gel/perovskite layer prepared by the embodiment of the invention;
fig. 4 is an SEM cross-sectional view of the ITO glass/ACA paste/perovskite layer structure prepared by the example of the present invention.
Detailed Description
The embodiment of the invention solves the technical problem that the phenomena of falling off or generating air holes between a substrate and a perovskite layer are easy to occur due to expansion and shrinkage in the annealing process in the prior art by providing the manufacturing method of the X-ray detector.
In order to better understand the above technical solutions, the following detailed description will refer to the accompanying drawings and specific embodiments.
Referring to fig. 1, a method for manufacturing an X-ray detector according to an embodiment of the present invention includes:
step S110: immersing ITO glass into acetone for cleaning;
describing this step in detail, immersing the ITO glass in acetone for cleaning, comprising:
the ITO glass is immersed in acetone for ultrasonic cleaning for 30min.
In order to sufficiently clean the impurities on the surface of the ITO glass, the method further comprises the following steps of:
placing ITO glass on a glass cleaning frame, adding deionized water and detergent into the ITO glass, ultrasonically cleaning for 30min, then washing with deionized water, and placing into absolute ethyl alcohol for standby.
In order to improve the hydrophilicity of the ITO glass, after immersing the ITO glass in acetone for cleaning, the method further comprises:
taking out the cleaned ITO glass, flushing the ITO glass with absolute ethyl alcohol, blow-drying the ITO glass with a nitrogen gun, and treating the ITO glass with Plasma for 5min.
Step S120: weighing FAI, MAI, pbI according to a preset proportion 2 Placing into a ball milling tank, adding anti-dissolution agent into the ball milling tankBall milling is performed; specifically, the perovskite layer adopts FA 0.5 MA 0.5 PbI 3 In order to prevent the influence of water and oxygen in the air, the system weighs high-purity FAI, MAI, pbI in a glove box according to a certain mole ratio 2 Put into a ball milling tank.
Specifically, adding an antisolvent into a ball milling tank for ball milling, comprising:
ethyl acetate antisolvent was added to the ball milling pot and ball milled for 12h at 600 r/min.
Step S130: drying the slurry after ball milling;
the step is specifically described, and the slurry after ball milling is dried and comprises the following steps:
the slurry after ball milling was transferred to a vacuum oven and dried overnight at 80 ℃.
Step S140: putting the dried powder into a tablet press to prepare a perovskite layer;
the method specifically illustrates the step, namely, taking the dried powder and putting the powder into a tablet press to prepare a perovskite layer, wherein the method comprises the following steps:
taking 2g of dried powder, placing into a tablet press, and pressing for 120s under 15MPa to obtain 2.5X12.5 cm 2 Is ready for use.
Step S150: placing ITO glass on an operation table, and dripping ACA glue on the cleaned ITO glass;
in order to uniformly spread ACA glue on the ITO glass, after the ACA glue is dripped on the cleaned ITO glass, the method further comprises the following steps:
the ACA glue is scraped to be flat by a micron-sized scraper.
Step S160: covering the perovskite layer on ITO glass with ACA glue, and lightly pressing the perovskite layer by hand to ensure that the perovskite layer is in uniform contact with the ACA glue.
Step S170: the ITO glass covered with the perovskite layer was annealed, and then cooled to room temperature.
Describing this step specifically, the ITO glass covered with the perovskite layer is annealed, and then cooled to room temperature, including:
the ITO glass covered with the perovskite layer is transferred to a hot stage at 150 ℃ and annealed for 15min, and then naturally cooled to room temperature.
Referring to fig. 2, the conductive particles of the ACA paste used in the example of the present invention are nickel particles having a diameter of about 1.5 μm, and are surrounded by a polymer. Referring to fig. 3, the tensile stress of about 400N can be resisted between the aca paste and the ITO glass substrate, and the tensile force of about 170N can be resisted even after the perovskite layer is covered. FIG. 4 shows a cross-sectional SEM image of the ITO glass/ACA gum/perovskite structure prepared by an embodiment of the present invention, and it can be seen that the thickness of the ACA gum is about 8. Mu.m.
According to the embodiment of the invention, the perovskite layer and the ITO glass substrate after annealing treatment are compounded through the bonding layer, so that the X-ray flat panel detector with low dark current and high spatial resolution can be manufactured, the problem of perovskite layer falling caused by different thermal expansion coefficients in the annealing process is perfectly solved, and the perovskite layer can be directly heated to a proper temperature, so that the X-ray flat panel detector has a wide application prospect.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (7)
1. A method of manufacturing an X-ray detector, comprising:
immersing ITO glass into acetone for cleaning;
weighing FAI, MAI, pbI according to a preset proportion 2 Placing the mixture into a ball milling tank, and adding an antisolvent into the ball milling tank for ball milling;
drying the slurry after ball milling;
putting the dried powder into a tablet press to prepare a perovskite layer;
dropping ACA glue on the cleaned ITO glass;
covering the perovskite layer on ITO glass with ACA glue;
and annealing the ITO glass covered with the perovskite layer, and cooling to room temperature.
2. The method of manufacturing an X-ray detector according to claim 1, further comprising, before said immersing the ITO glass in acetone for cleaning:
adding deionized water and detergent into the ITO glass, ultrasonically cleaning for 30min, and then flushing with deionized water.
3. The method of manufacturing an X-ray detector according to claim 1, further comprising, after the washing of the ITO glass by immersing in acetone:
taking out the cleaned ITO glass, flushing the ITO glass with absolute ethyl alcohol, blow-drying the ITO glass with a nitrogen gun, and treating the ITO glass with Plasma for 5min.
4. The method for manufacturing an X-ray detector according to claim 1, wherein adding an antisolvent to the ball milling tank for ball milling comprises:
and adding an ethyl acetate antisolvent into the ball milling tank, and ball milling for 12h under the condition of 600 r/min.
5. The method for manufacturing an X-ray detector according to claim 1, wherein the drying the slurry after ball milling comprises:
transferring the slurry after ball milling to a vacuum drying oven, and drying overnight at 80 ℃.
6. The method of manufacturing an X-ray detector according to claim 1, further comprising, after the dropping of the ACA paste on the cleaned ITO glass:
and scraping the ACA glue with a scraper to be smooth.
7. The method of manufacturing an X-ray detector according to claim 1, wherein annealing the ITO glass covered with the perovskite layer, and then cooling to room temperature, comprises:
transferring the ITO glass covered with the perovskite layer to a hot stage at 150 ℃, annealing for 15min, and naturally cooling to room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211702773.5A CN116249361A (en) | 2022-12-28 | 2022-12-28 | Manufacturing method of X-ray detector |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211702773.5A CN116249361A (en) | 2022-12-28 | 2022-12-28 | Manufacturing method of X-ray detector |
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| Publication Number | Publication Date |
|---|---|
| CN116249361A true CN116249361A (en) | 2023-06-09 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202211702773.5A Pending CN116249361A (en) | 2022-12-28 | 2022-12-28 | Manufacturing method of X-ray detector |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117651465A (en) * | 2024-01-29 | 2024-03-05 | 西安电子科技大学 | Multi-step tabletting perovskite heterogeneous crystallization circle X-ray detector and preparation method thereof |
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2022
- 2022-12-28 CN CN202211702773.5A patent/CN116249361A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117651465A (en) * | 2024-01-29 | 2024-03-05 | 西安电子科技大学 | Multi-step tabletting perovskite heterogeneous crystallization circle X-ray detector and preparation method thereof |
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