CN113035900A - Direct electromagnetic radiation detector and preparation method thereof - Google Patents
Direct electromagnetic radiation detector and preparation method thereof Download PDFInfo
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Abstract
The invention is suitable for the field of electromagnetic radiation detectors, and discloses a direct electromagnetic radiation detector and a preparation method thereof, the direct electromagnetic radiation detector comprises an electrode layer, a packaging layer, an N-type semiconductor layer, a light absorption layer, a P-type semiconductor layer, a transparent conducting layer and a substrate, the transparent conducting layer, the P-type semiconductor layer, the light absorption layer, the N-type semiconductor layer, the packaging layer and the electrode layer are sequentially arranged on the substrate from bottom to top, the transparent conducting layer is divided into a plurality of pixel areas arranged at intervals along the incident direction vertical to the electromagnetic radiation, the electrode layer is divided into a plurality of photoelectric signal acquisition areas arranged at intervals along the incident direction parallel to the electromagnetic radiation, the transparent conducting layer is electrically connected with the electrode layer, the detector can simultaneously utilize the plurality of photoelectric signal acquisition areas to simultaneously acquire information of the plurality of pixel areas, thereby improving the, thus, only a small dose of electromagnetic radiation is required to enable high sensitivity detection.
Description
Technical Field
The invention relates to the field of electromagnetic radiation detectors, in particular to a direct electromagnetic radiation detector and a preparation method thereof.
Background
Electromagnetic radiation detectors, particularly X-ray detectors, are widely used in the fields of medical imaging, security inspection, nondestructive testing, quality inspection, and the like. When the X-ray penetrates the object, its attenuation signal is recorded by the X-ray detector. Different parts of the object contain different element compositions, and the absorption and attenuation capabilities of the X-ray are different, so that electric signals with different intensities are formed on the X-ray detector.
In the medical field, the use of X-ray imaging is becoming more and more popular, and higher requirements are also placed on radiation safety. Sometimes, higher doses of X-rays are used in order to improve detection sensitivity, however high dose X-ray scans, such as Computed Tomography (CT), can damage DNA and increase the risk of cancer in the patient.
Therefore, it is necessary to prepare an electromagnetic radiation ray detector having higher sensitivity so as to reduce the dose of the electromagnetic radiation ray.
Disclosure of Invention
A first object of the present invention is to provide a direct-type electromagnetic radiation detector capable of achieving high-sensitivity detection with a smaller dose of electromagnetic radiation.
In order to achieve the purpose, the invention provides the following scheme:
the utility model provides a direct type electromagnetic radiation detector, includes electrode layer, encapsulated layer, N type semiconductor layer, light-absorbing layer, P type semiconductor layer, transparent conducting layer and basement, transparent conducting layer P type semiconductor layer the light-absorbing layer N type semiconductor layer the encapsulated layer with supreme locating in proper order down is followed to the electrode layer on the basement, transparent conducting layer divides the pixel region that a plurality of interval set up into along perpendicular to electromagnetic radiation's incident direction, the electrode layer is along being on a parallel with electromagnetic radiation's incident direction divides the photoelectric signal collection region that a plurality of interval set up into, transparent conducting layer with electrode layer electric connection.
Preferably, the thickness of the light absorbing layer is 300-700 nm.
Preferably, the light absorbing layer comprises a perovskite material.
Preferably, the light absorbing layer comprises lead-iodotricalcium titanium methylacrylate, and the thickness of the light absorbing layer is 300 nm.
Preferably, the N-type semiconductor layer comprises PCBM.
Preferably, the P-type semiconductor layer includes nickel oxide.
Preferably, the direct electromagnetic radiation detector further comprises a signal acquisition and processing device, and the transparent conductive layer and the electrode layer are respectively connected with the signal acquisition and processing device.
A second object of the present invention is to provide a method for manufacturing a direct electromagnetic radiation detector, comprising the steps of:
providing a substrate, wherein the surface of the substrate is plated with a transparent conducting layer;
dividing the transparent conductive layer into a plurality of pixel areas arranged at intervals along the incident direction vertical to the electromagnetic radiation;
forming a P-type semiconductor layer on the surface of the transparent conducting layer;
forming a light absorption layer on the surface of the P-type semiconductor layer;
forming an N-type semiconductor layer on the surface of the light absorption layer;
forming a packaging layer on the surface of the N-type semiconductor layer;
and forming an electrode layer on the packaging layer, wherein the electrode layer is divided into a plurality of photoelectric signal acquisition areas arranged at intervals along the incident direction parallel to the electromagnetic radiation, and the preparation of the detector is completed.
Preferably, the specific implementation manner of forming the P-type semiconductor layer on the surface of the transparent conductive layer is as follows: preparing an acetonitrile ethanol solution, and injecting the acetonitrile ethanol solution after being uniformly stirred into a measuring flask containing nickel oxide powder; stirring the nickel oxide powder until the nickel oxide powder is fully dissolved to obtain a nickel oxide solution with the concentration of 5 mg/ml; and spraying a nickel oxide solution on the surface of the transparent conducting layer to form a P-type semiconductor layer.
Preferably, the light absorbing layer is prepared from a lead-iodine-tricalcium-titanium-methyl-acrylate solution, and the specific implementation mode of forming the light absorbing layer on the surface of the P-type semiconductor layer is as follows:
preparing a perovskite precursor solution from methyl iodide (MAI) and lead diiodide (PbI)2) Synthesizing, wherein the ratio of the methyl iodide acrylate to the lead diiodide is 0.3;
putting the sample with the formed P-type semiconductor layer into a glove box, taking a perovskite precursor solution by using a liquid gun, and uniformly coating the perovskite precursor solution on the four corners and the center of the sample;
placing the sample coated with the perovskite precursor solution on the surface of a spin coater, and carrying out rotary coating on the sample;
in the process of spin coating the sample, toluene is dripped on the surface of the sample to extract the perovskite material, and a light absorption layer is formed.
Preferably, the embodiment of forming the N-type semiconductor layer on the surface of the light absorbing layer is as follows: preparing a PCBM solution, and uniformly coating the PCBM solution on four corners and the center of a sample with a light absorption layer; and putting the sample on the surface of a spin coater, and carrying out spin coating on the sample to form the N-type semiconductor layer.
Preferably, an electrode layer is formed on the encapsulation layer, and the electrode layer is divided into a plurality of photoelectric signal acquisition regions arranged at intervals along a direction parallel to the incident direction of the electromagnetic radiation, and the embodiment of the photoelectric signal acquisition regions is as follows:
providing a mask plate, wherein the mask plate is provided with a plurality of coating regions arranged at intervals in a penetrating manner, and the plurality of coating regions are arranged side by side along the incident direction parallel to the electromagnetic radiation;
covering the mask on the surface of the sample with the packaging layer, filling an electrode material in the plating layer area, and forming an electrode layer by the electrode material.
Preferably, an electrode layer is formed on the encapsulation layer, and the electrode layer is divided into a plurality of photoelectric signal acquisition regions arranged at intervals along a direction parallel to the incident direction of the electromagnetic radiation, and the embodiment of the photoelectric signal acquisition regions is as follows:
providing a mask plate, wherein the mask plate is provided with a plating layer region in a penetrating manner;
covering the surface of the sample on which the packaging layer is formed with the mask, filling an electrode material in the plating layer area, wherein the electrode material forms an electrode layer;
and dividing the electrode layer into a plurality of photoelectric signal acquisition regions arranged at intervals along the incident direction parallel to the electromagnetic radiation.
The direct electromagnetic radiation detector provided by the invention can simultaneously utilize a plurality of photoelectric signal acquisition regions to simultaneously acquire information of a plurality of pixel regions, so that the sensitivity of the detector can be improved, and high-sensitivity detection can be realized only by using a small amount of electromagnetic radiation.
The preparation method is simple to operate, and the direct electromagnetic radiation detector with high sensitivity can be prepared.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a schematic diagram of a direct electromagnetic radiation detector according to an embodiment of the present invention;
FIG. 2 is a flow chart of a method of fabricating a direct electromagnetic radiation detector provided by an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a first mask according to an embodiment of the present invention;
FIG. 4 is a schematic structural diagram of an electrode layer prepared from the mask of FIG. 3;
fig. 5 is a schematic structural diagram of a second mask according to an embodiment of the present invention.
The reference numbers illustrate:
10. an electrode layer; 11. a photoelectric signal acquisition area; 20. a packaging layer; 30. an N-type semiconductor layer;
40. a light absorbing layer; 50. a P-type semiconductor layer; 60. a transparent conductive layer; 61. a pixel region; 70. a substrate;
80. a signal acquisition processing device; 90. a mask plate; 91. a silver plating region.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that all the directional indicators (such as up, down, left, right, front, and rear … …) in the embodiment of the present invention are only used to explain the relative position relationship between the components, the movement situation, etc. in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indicator is changed accordingly.
It will also be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present.
In addition, the descriptions related to "first", "second", etc. in the present invention are for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
As shown in fig. 1 to 5, which are direct type electromagnetic radiation detectors of an embodiment of the invention. The structure and function characteristics of the direct electromagnetic radiation detector will be exemplified by X-rays in electromagnetic radiation.
It should be noted that the X-ray described in this embodiment is only an exemplary illustration, and the direct electromagnetic radiation detector of this embodiment may also be applied to other electromagnetic radiation. In fig. 1, the X direction is parallel to the incident direction of the X-ray, and the Y direction is perpendicular to the incident direction of the X-ray.
Referring to fig. 1-5, a direct electromagnetic radiation detector according to an embodiment of the present invention includes an electrode layer, a package layer, an N-type semiconductor layer, a light absorption layer, a P-type semiconductor layer, a transparent conductive layer, and a substrate, wherein the transparent conductive layer, the P-type semiconductor layer, the light absorption layer, the N-type semiconductor layer, the package layer, and the electrode layer are sequentially stacked on the substrate from bottom to top, the transparent conductive layer is divided into a plurality of pixel regions arranged at intervals along a direction perpendicular to an incident direction of X-rays, namely, when viewed from the Y direction, a plurality of pixel areas arranged at intervals can be seen, the electrode layer is divided into a plurality of photoelectric signal acquisition areas arranged at intervals along the direction parallel to the incidence direction of the X-ray, that is, when viewed from the X direction, a plurality of photoelectric signal collecting regions arranged at intervals can be seen, and the transparent conductive layer is electrically connected with the electrode layer, that is, each energy channel can acquire information of all pixel regions. The incident X-ray is generated by the X-ray tube, the photon energy is in the range of about 1-200 keV, and the corresponding wavelength is in the range of 0.006-1 nm. The absorption probability of the light absorption layer to X-ray photons with the energy range of 20-120 keV is larger than 95%, and the attenuation coefficient of the X-ray light absorption layer (104) is about 0.5-5 times of that of the silicon material.
In the conventional X-ray detector, the X-ray is incident from top to bottom, in the direct electromagnetic radiation detector of this embodiment, the X-ray is incident from one side of the detector (as in the X direction in fig. 1), the high-energy X-ray has a stronger penetration capability, and images are performed several times along the X-ray propagation direction. The direct electromagnetic radiation detector of the embodiment simultaneously realizes the excellent detection performances of small volume, low cost, simple configuration, high sensitivity, energy spectrum resolution and the like.
It is understood that the number of pixel regions may be divided according to actual situations, for example, the transparent conductive layer may be divided into 258 independent regions, and two regions at two ends are omitted to form 256 independent pixel regions.
It is understood that the number of the photoelectric signal collecting regions can be divided according to actual situations, for example, the electrode layer can be divided into four photoelectric signal collecting regions, so that information can be collected for 256 pixel regions simultaneously by using four energy channels.
Preferably, the substrate can be made of any material such as glass, stainless steel sheet, ceramic, etc.
Preferably, the transparent conductive layer can be made of any one of fluorine-doped tin oxide, indium-doped tin oxide, aluminum-doped zinc oxide, and the like. The preparation method of the transparent conductive layer comprises the following steps:
step 1: the glass, ceramic and the like with any transparent conducting layer plated on the surface of which fluorine-doped tin oxide (FTO), indium-doped tin oxide (ITO), aluminum-doped zinc oxide (AZO) and the like are adopted as a substrate.
If a stainless steel sheet is used as the flexible substrate, a silicon dioxide insulating layer is plated on the surface of the stainless steel sheet, and then a transparent conductive layer is plated. Specifically, the embodiment of the silicon dioxide plating insulating layer is as follows: and plating a silicon dioxide thin layer with the thickness of 100-300 nm on the surface of the stainless steel by using a magnetron sputtering method. The transparent conductive layer plating embodiment is: and plating a transparent conductive layer with the thickness of 500-1000 nm on the silicon dioxide insulating layer by using a magnetron sputtering method.
Step 2: and scribing the transparent conductive layer in parallel by using laser scribing, and dividing the transparent conductive layer into a plurality of pixel areas arranged at intervals. Such as: the transparent conductive layer is divided into 258 independent areas by scribing 257 times, and two areas at two ends are cut off to form 256 independent pixels for collecting photoelectric signals of different pixels.
Preferably, the P-type semiconductor layer is prepared by nickel oxide, and the preparation method of the P-type semiconductor layer is as follows:
preparing acetonitrile ethanol solution, stirring uniformly by using a rotor, injecting into a small weighing bottle containing nickel oxide powder, stirring and ensuring that the nickel oxide is fully dissolved. And then spraying nickel oxide on the surface of the transparent conductive layer in a fume hood, wherein the specific implementation mode is as follows: placing the substrate plated with the transparent conducting layer on a titanium-based heating plate, setting the temperature of the titanium-based heating plate to be 550 ℃, connecting compressed air by using a spray gun, adding a nickel oxide solution into a liquid storage cavity of the spray gun by using an injector, spraying the nickel oxide solution on the surface of the transparent conducting layer at a constant speed to form a nickel oxide film with the thickness of 20-30nm, and annealing the nickel oxide film after spraying.
Preferably, the thickness of the light absorbing layer is 300-700nm, and different materials are selected to prepare the light absorbing layer, and the thickness of the light absorbing layer is different. It should be noted that, since in this embodiment, X-rays are incident from one side of the detector, the thickness of the light absorbing layer can be made a little thicker than that of a conventional photoelectric conversion layer, so that X-rays can be kept transmitted within the light absorbing layer.
Further, the light-absorbing layer is made of perovskite materials, and compared with amorphous selenium materials which are commonly used as photoelectric conversion materials in the prior art, the absorption coefficient of the perovskite materials for X rays is higher, so that the light-absorbing layer made of perovskite materials has wider forbidden band width and higher sensitivity to the X rays, the change of light energy can be accurately detected under the X rays with lower dosage, and the detection efficiency is effectively improved.
Specifically, the light absorbing layer is made of materials including, but not limited to, CdTe (cadmium telluride), MAPbBr3(methylaminolead bromide), Cs2AgBiBr6(double perovskite cesium silver bismuth bromide), (NH)4)3Bi2I9Si (silicon). For example, when the light-absorbing layer employs MAPbI3When the (methyl acrylate lead iodide tricalcium titanium ore) solution is prepared, the effect is better when the thickness of the light absorption layer is 300 nm. When the light absorption layer is prepared by CsMAFA organic-inorganic mixed perovskite, the effect is better when the thickness of the light absorption layer is 700 nm.
Preferably, the light absorbing layer is prepared by using methyl methacrylate lead iodide tris (MAPbI)3) The perovskite solution is taken as an example of a light absorbing layer, and the preparation method is as follows:
preparing a perovskite precursor solution, wherein the perovskite precursor solution is prepared from methyl iodide acrylate (MAI) and lead diiodide (PbI)2) The synthesis comprises the following steps that the ratio of methyl iodide acrylate to lead diiodide is 0.3, and the whole synthesis process is carried out in a glove box with an inert gas environment: the surface size of the sample was 15mm, and the MAI was weighed to 0.2067 g, and the PbI was weighed20.5993 g was weighed into a 3ml brown glass bottle as a solute, and then the solvent was measured by a pipette gun in a glove box, 300. mu.l of gamma-butyrolactone (GBL) and 700. mu.l of dimethyl sulfoxide (DMSO) were uniformly mixed as a solvent, and the solute and the solvent were mixed and stirred for 12 hours to be sufficiently dissolved.
Transferring the sample coated with the nickel oxide film into a glove box, taking a perovskite precursor solution by using a liquid transfer gun, uniformly coating the perovskite precursor solution on four corners and the center of the sample, and paying attention to the fact that a liquid transfer opening of the liquid transfer gun cannot touch the surface of the sample; putting a sample on the surface of a spin coater, and performing spin coating, wherein the rotation speed of the spin coater is set to be 1000 revolutions per minute and is rotated for 10 seconds in the process; then the rotating speed is set to be 5000 revolutions per minuteRotating for 30 seconds; at about 18 seconds, toluene (anti-solvent) was added dropwise to the sample surface to extract the perovskite material, forming MAPbI with a green thickness of about 300nm3A perovskite light absorbing layer. The method for dripping toluene comprises the following steps: the mixture was continuously dropped into the sample at a constant flow rate, and 550. mu.l of toluene was dropped onto the surface of the sample having a size of 15mm × 15 mm.
In another embodiment, the method for manufacturing the light absorbing layer may be designed to use a spray coating method, so that a thicker light absorbing layer can be obtained. Specifically, PbI is prepared by aerosol liquid solidification method2And MAI in DMSO/DMF (1: 1 ratio) to form a 0.8mol/L solution. Placing the sample on a heating table, wherein the temperature of the heating table is set to be 130 ℃, the nitrogen flow rate is 2.5L/min, the nozzle width is 1 mm, and the nozzle moving speed is 0.6 cm/s; controlling the thickness of the grown perovskite thin film through different deposition cycle times by using an ultrasonic sprayer; and after the spraying is finished, continuously heating the perovskite film at 100 ℃, and then slowly cooling and annealing. Both the above deposition and annealing processes were carried out under ambient conditions in a closed chemical fume hood.
Preferably, the N-type semiconductor layer comprises PCBM, and the N-type semiconductor layer is prepared by the following method: a PCBM solution was prepared, and 1ml of a commercial PCBM solution was taken out using a 1ml syringe, wherein the commercial PCBM solution used aminobenzene as a solvent and had a concentration of 20 mg/ml.
Uniformly coating the PCBM solution on four corners and the center of the sample with the light absorption layer; and placing the sample on the surface of a spin coater, setting the rotation speed of the spin coater to 2000 rpm, and carrying out spin coating for 30 seconds to form an N-type semiconductor layer with the thickness of about 80 nm. The amount of PCBM used per 15mm by 15mm size sample surface was about 40 microliters.
It can be understood that the N-type semiconductor layer, the light absorbing layer and the P-type semiconductor layer form a P-I-N type semiconductor structure.
Preferably, the material of the packaging layer can be bathocuproine organic small molecule BCP and the like. The preparation method of the packaging layer comprises the following steps:
preparing a BCP solution, and uniformly coating the BCP solution on four corners and the center of a sample on which an N-type semiconductor layer is formed; and placing the sample on the surface of a spin coater, setting the rotation speed of the spin coater to 4000 revolutions per minute, and carrying out spin coating for 30 seconds to form an encapsulation layer with the thickness of about 50 nanometers. The amount of BCP used was about 30 microliters per 15mm by 15mm size sample surface. In this embodiment, the encapsulation layer is provided to protect the light absorbing layer when the electrode layer is further evaporated.
Preferably, the material of the electrode layer may be a metal material with stable performance and convenient bonding, such as molybdenum, nickel, aluminum, silver, gold, and the like. It will be appreciated that the overall thickness of the electrode layer may vary, and that the electrode thickness may be different for different photoelectric signal acquisition regions, preferably the electrode layer increases in a direction parallel to the direction of incidence of the X-rays (the X-direction as shown in fig. 1).
In this embodiment, the electrode layer material is silver. There are two methods for preparing the electrode layer, and the first implementation method is as follows: providing a mask plate, wherein the mask plate is provided with a plurality of silver-plated regions arranged at intervals in a penetrating manner, the silver-plated regions are arranged side by side along the incident direction parallel to the X-ray, the number of the silver-plated regions is determined according to the number of actually required photoelectric signal acquisition regions, and four silver-plated regions are designed in figure 3, so that four photoelectric signal acquisition regions can be formed;
covering the surface of the sample on which the packaging layer is formed with a mask plate, and evaporating a silver electrode with the thickness of about 100nm in a vacuum thermal evaporation chamber, wherein the silver electrode is filled in a silver plating area. The electrode layer obtained by the method is equivalent to be composed of silver electrodes in silver plating areas, the silver electrodes are insulated from each other, the area where each silver electrode is located is equivalent to a photoelectric signal acquisition area, electric signals can be acquired independently, and the function of energy spectrum resolution is achieved.
A second method of implementation of the electrode layer preparation is as follows: providing a mask plate, wherein the mask plate is provided with a silver plating area in a penetrating way; covering a mask on the surface of a sample with a packaging layer, and evaporating a silver electrode with the thickness of about 100nm in a vacuum thermal evaporation chamber, wherein the silver electrode is filled in a silver plating area, and the silver electrode is an integral body and is not divided into a plurality of photoelectric signal acquisition areas; the electrode layer is divided into a plurality of photoelectric signal acquisition areas which are arranged at intervals along the incident direction parallel to the X-ray.
Preferably, the direct electromagnetic radiation detector further comprises a signal acquisition and processing device, the transparent conductive layer and the electrode layer are respectively connected with the signal acquisition and processing device, and the signal acquisition and processing device comprises any one type of energy resolution counting electronic device, electric signal integration electronic device and the like.
The invention also provides a preparation method of the direct electromagnetic radiation detector, which comprises the following steps:
step S10, providing a substrate, the surface of which is plated with a transparent conductive layer.
Step S20, dividing the transparent conductive layer into a plurality of pixel areas arranged at intervals along the incident direction perpendicular to the X-ray;
the preparation method of the transparent conductive layer comprises the following steps: step 1: the glass, ceramic and the like with any transparent conducting layer plated on the surface of which fluorine-doped tin oxide (FTO), indium-doped tin oxide (ITO), aluminum-doped zinc oxide (AZO) and the like are adopted as a substrate.
If a stainless steel sheet is used as the flexible substrate, a silicon dioxide insulating layer is plated on the surface of the stainless steel sheet, and then a transparent conductive layer is plated. Specifically, the embodiment of the silicon dioxide plating insulating layer is as follows: and plating a silicon dioxide thin layer with the thickness of 100-300 nm on the surface of the stainless steel by using a magnetron sputtering method. The transparent conductive layer plating embodiment is: and plating a transparent conductive layer with the thickness of 500-1000 nm on the silicon dioxide insulating layer by using a magnetron sputtering method.
Step 2: and scribing the transparent conductive layer in parallel by using laser scribing, and dividing the transparent conductive layer into a plurality of pixel areas arranged at intervals. Such as: the transparent conductive layer was divided into 258 independent regions by scribing 257 times, and two regions at both ends were cut off to form 256 independent pixels.
In step S30, a P-type semiconductor layer is formed on the surface of the transparent conductive layer.
The preparation method of the P-type semiconductor layer comprises the following steps: preparing acetonitrile ethanol solution, stirring uniformly by using a rotor, injecting into a small weighing bottle containing nickel oxide powder, stirring and ensuring that the nickel oxide is fully dissolved. And then spraying nickel oxide on the surface of the transparent conductive layer in a fume hood, wherein the specific implementation mode is as follows: placing the substrate plated with the transparent conducting layer on a titanium-based heating plate, setting the temperature of the titanium-based heating plate to be 550 ℃, connecting compressed air by using a spray gun, adding a nickel oxide solution into a liquid storage cavity of the spray gun by using an injector, spraying the nickel oxide solution on the surface of the transparent conducting layer at a constant speed to form a nickel oxide film with the thickness of 20-30nm, and annealing the nickel oxide film after spraying.
Step S40 is to form a light absorbing layer on the surface of the P-type semiconductor layer.
The light absorption layer is prepared by adopting methyl acrylate lead iodide tris (MAPbI)3) The perovskite solution is taken as an example of a light absorbing layer, and the preparation method is as follows:
preparing a perovskite precursor solution, wherein the perovskite precursor solution is prepared from methyl iodide acrylate (MAI) and lead diiodide (PbI)2) The synthesis comprises the following steps that the ratio of methyl iodide acrylate to lead diiodide is 0.3, and the whole synthesis process is carried out in a glove box with an inert gas environment: the surface size of the sample was 15mm, and the MAI was weighed to 0.2067 g, and the PbI was weighed20.5993 g was weighed into a 3ml brown glass bottle as a solute, and then the solvent was measured by a pipette gun in a glove box, 300. mu.l of gamma-butyrolactone (GBL) and 700. mu.l of dimethyl sulfoxide (DMSO) were uniformly mixed as a solvent, and the solute and the solvent were mixed and stirred for 12 hours to be sufficiently dissolved.
Transferring the sample coated with the nickel oxide film into a glove box, taking a perovskite precursor solution by using a liquid transfer gun, uniformly coating the perovskite precursor solution on four corners and the center of the sample, and paying attention to the fact that a liquid transfer opening of the liquid transfer gun cannot touch the surface of the sample; putting a sample on the surface of a spin coater, and performing spin coating, wherein the rotation speed of the spin coater is set to be 1000 revolutions per minute and is rotated for 10 seconds in the process; setting the rotating speed to be 5000 revolutions per minute and rotating for 30 seconds; at about 18 seconds, toluene (anti-solvent) was added dropwise to the sample surface to extract the perovskite material, forming MAPbI with a green thickness of about 300nm3A perovskite light absorbing layer. The method for dripping toluene comprises the following steps: the mixture was continuously dropped into the sample at a constant flow rate, and 550. mu.l of toluene was dropped onto the surface of the sample having a size of 15mm × 15 mm.
In another embodiment, the method for manufacturing the light absorbing layer may be designed to use a spray coating method, so that a thicker light absorbing layer can be obtained. Specifically, PbI is prepared by aerosol liquid solidification method2And MAI in DMSO/DMF (1: 1 ratio) to form0.8mol/L solution. Placing the sample on a heating table, wherein the temperature of the heating table is set to be 130 ℃, the nitrogen flow rate is 2.5L/min, the nozzle width is 1 mm, and the nozzle moving speed is 0.6 cm/s; controlling the thickness of the grown perovskite thin film through different deposition cycle times by using an ultrasonic sprayer; and after the spraying is finished, continuously heating the perovskite film at 100 ℃, and then slowly cooling and annealing. Both the above deposition and annealing processes were carried out under ambient conditions in a closed chemical fume hood.
Step S50, forming an N-type semiconductor layer on the surface of the light absorption layer;
the preparation method of the N-type semiconductor layer comprises the following steps: a PCBM solution was prepared, and 1ml of a commercial PCBM solution was taken out using a 1ml syringe, wherein the commercial PCBM solution used aminobenzene as a solvent and had a concentration of 20 mg/ml.
Uniformly coating the PCBM solution on four corners and the center of the sample with the light absorption layer; and placing the sample on the surface of a spin coater, setting the rotation speed of the spin coater to 2000 rpm, and carrying out spin coating for 30 seconds to form an N-type semiconductor layer with the thickness of about 80 nm. The amount of PCBM used per 15mm by 15mm size sample surface was about 40 microliters.
Step S60, forming a packaging layer on the surface of the N-type semiconductor layer;
the preparation method of the packaging layer comprises the following steps: preparing a BCP solution, and uniformly coating the BCP solution on four corners and the center of a sample on which an N-type semiconductor layer is formed; and placing the sample on the surface of a spin coater, setting the rotation speed of the spin coater to 4000 revolutions per minute, and carrying out spin coating for 30 seconds to form an encapsulation layer with the thickness of about 50 nanometers. The amount of BCP used was about 30 microliters per 15mm by 15mm size sample surface. In this embodiment, the encapsulation layer is provided to protect the light absorbing layer when the electrode layer is further evaporated.
And step S70, forming an electrode layer on the packaging layer, wherein the electrode layer is divided into a plurality of photoelectric signal acquisition areas arranged at intervals along the incident direction parallel to the X-ray, and the preparation of the detector is completed.
There are two methods for preparing the electrode layer, and the first implementation method is as follows: providing a mask plate, wherein the mask plate is provided with a plurality of silver-plated regions arranged at intervals in a penetrating manner, and the silver-plated regions are arranged side by side along the incident direction parallel to the X-ray;
covering the surface of the sample on which the packaging layer is formed with a mask plate, and evaporating a silver electrode with the thickness of about 100nm in a vacuum thermal evaporation chamber, wherein the silver electrode is filled in a silver plating area. The electrode layer obtained by the method is equivalent to be composed of silver electrodes in silver plating areas, the silver electrodes are insulated from each other, the area where each silver electrode is located is equivalent to a photoelectric signal acquisition area, electric signals can be acquired independently, and the function of energy spectrum resolution is achieved.
A second method of implementation of the electrode layer preparation is as follows: providing a mask plate, wherein the mask plate is provided with a silver plating area in a penetrating way; covering a mask on the surface of a sample with a packaging layer, and evaporating a silver electrode with the thickness of about 100nm in a vacuum thermal evaporation chamber, wherein the silver electrode is filled in a silver plating area, and the silver electrode is an integral body and is not divided into a plurality of photoelectric signal acquisition areas; the electrode layer is divided into a plurality of photoelectric signal acquisition areas which are arranged at intervals along the incident direction parallel to the X-ray.
The preparation method is simple to operate, and the direct electromagnetic radiation detector with high sensitivity can be prepared.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (13)
1. The utility model provides a direct type electromagnetic radiation detector, its characterized in that includes electrode layer, encapsulated layer, N type semiconductor layer, light-absorbing layer, P type semiconductor layer, transparent conducting layer and basement, transparent conducting layer P type semiconductor layer light-absorbing layer N type semiconductor layer the encapsulated layer with the electrode layer is supreme locating in proper order down on the basement, transparent conducting layer divides the pixel region that a plurality of interval set up along the incident direction of perpendicular to electromagnetic radiation, the electrode layer along being on a parallel with electromagnetic radiation's incident direction divides the photoelectric signal collection region that a plurality of interval set up into, transparent conducting layer with electrode layer electric connection.
2. The direct-type electromagnetic radiation detector as claimed in claim 1, wherein the thickness of said light absorbing layer is 300-700 nm.
3. The direct electromagnetic radiation detector of claim 1 wherein the light absorbing layer comprises a perovskite material.
4. The direct electromagnetic radiation detector of claim 3 wherein said light absorbing layer comprises lead iodotricalcium titanium methacrylate and said light absorbing layer has a thickness of 300 nm.
5. A direct-type electromagnetic radiation detector as claimed in claim 1, wherein said N-type semiconductor layer comprises PCBM.
6. The direct electromagnetic radiation detector of claim 1, wherein the P-type semiconductor layer comprises nickel oxide.
7. The direct-type electromagnetic radiation detector of claim 1, further comprising a signal acquisition processing device, the transparent conductive layer and the electrode layer being respectively connected to the signal acquisition processing device.
8. A method for preparing a direct electromagnetic radiation detector is characterized by comprising the following steps:
providing a substrate, wherein the surface of the substrate is plated with a transparent conducting layer;
dividing the transparent conductive layer into a plurality of pixel areas arranged at intervals along the incident direction vertical to the electromagnetic radiation;
forming a P-type semiconductor layer on the surface of the transparent conducting layer;
forming a light absorption layer on the surface of the P-type semiconductor layer;
forming an N-type semiconductor layer on the surface of the light absorption layer;
forming a packaging layer on the surface of the N-type semiconductor layer;
and forming an electrode layer on the packaging layer, wherein the electrode layer is divided into a plurality of photoelectric signal acquisition areas arranged at intervals along the incident direction parallel to the electromagnetic radiation, and the preparation of the detector is completed.
9. The method according to claim 8, wherein the P-type semiconductor layer is formed on the surface of the transparent conductive layer by: preparing an acetonitrile ethanol solution, and injecting the acetonitrile ethanol solution after being uniformly stirred into a measuring flask containing nickel oxide powder; stirring the nickel oxide powder until the nickel oxide powder is fully dissolved to obtain a nickel oxide solution with the concentration of 5 mg/ml; and spraying a nickel oxide solution on the surface of the transparent conducting layer to form a P-type semiconductor layer.
10. The preparation method of claim 9, wherein the light absorbing layer is prepared from a lead-iodotricalcium titanate methacrylate solution, and the specific implementation of forming the light absorbing layer on the surface of the P-type semiconductor layer is as follows:
preparing a perovskite precursor solution from methyl iodide (MAI) and lead diiodide (PbI)2) Synthesizing, wherein the ratio of the methyl iodide acrylate to the lead diiodide is 0.3;
putting the sample with the formed P-type semiconductor layer into a glove box, taking a perovskite precursor solution by using a liquid gun, and uniformly coating the perovskite precursor solution on the four corners and the center of the sample;
placing the sample coated with the perovskite precursor solution on the surface of a spin coater, and carrying out rotary coating on the sample;
in the process of spin coating the sample, toluene is dripped on the surface of the sample to extract the perovskite material, and a light absorption layer is formed.
11. The production method according to claim 8, wherein an embodiment of forming an N-type semiconductor layer on the surface of the light absorbing layer is: preparing a PCBM solution, and uniformly coating the PCBM solution on four corners and the center of a sample with a light absorption layer; and putting the sample on the surface of a spin coater, and carrying out spin coating on the sample to form the N-type semiconductor layer.
12. The method according to claim 8, wherein an electrode layer is formed on the package layer, and the electrode layer is divided into a plurality of photoelectric signal collecting regions arranged at intervals along a direction parallel to the incident direction of the electromagnetic radiation, and the method comprises the following steps:
providing a mask plate, wherein the mask plate is provided with a plurality of coating regions arranged at intervals in a penetrating manner, and the plurality of coating regions are arranged side by side along the incident direction parallel to the electromagnetic radiation;
covering the mask on the surface of the sample with the packaging layer, filling an electrode material in the plating layer area, and forming an electrode layer by the electrode material.
13. The method according to claim 8, wherein an electrode layer is formed on the package layer, and the electrode layer is divided into a plurality of photoelectric signal collecting regions arranged at intervals along a direction parallel to the incident direction of the electromagnetic radiation, and the method comprises the following steps:
providing a mask plate, wherein the mask plate is provided with a plating layer region in a penetrating manner;
covering the surface of the sample on which the packaging layer is formed with the mask, filling an electrode material in the plating layer area, wherein the electrode material forms an electrode layer;
and dividing the electrode layer into a plurality of photoelectric signal acquisition regions arranged at intervals along the incident direction parallel to the electromagnetic radiation.
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| WO2022179258A1 (en) * | 2021-02-26 | 2022-09-01 | 深圳先进技术研究院 | Direct electromagnetic radiation detector and manufacturing method therefor |
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