CN113394344B - Direct-indirect mixed perovskite X-ray detector and light yield calculation method of scintillator of direct-indirect mixed perovskite X-ray detector - Google Patents

Direct-indirect mixed perovskite X-ray detector and light yield calculation method of scintillator of direct-indirect mixed perovskite X-ray detector Download PDF

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CN113394344B
CN113394344B CN202110658915.1A CN202110658915A CN113394344B CN 113394344 B CN113394344 B CN 113394344B CN 202110658915 A CN202110658915 A CN 202110658915A CN 113394344 B CN113394344 B CN 113394344B
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魏浩桐
刘璐璐
杨柏
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Jilin University
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    • H—ELECTRICITY
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    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
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    • G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/16—Measuring radiation intensity
    • G01T1/20—Measuring radiation intensity with scintillation detectors
    • G01T1/2018—Scintillation-photodiode combinations
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/16—Measuring radiation intensity
    • G01T1/20—Measuring radiation intensity with scintillation detectors
    • G01T1/202—Measuring radiation intensity with scintillation detectors the detector being a crystal
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    • G01—MEASURING; TESTING
    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
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Abstract

A direct-indirect mixed perovskite X-ray detector and a light yield calculation method of an indirect X-ray detection scintillator material belong to the technical field of X-ray detection. From bottom to top, the anode Au, the hole transport layer Spiro-OMeTAD, the direct-indirect mixed perovskite X-ray detection pressure measuring chip material and the electron transport layer C60A hole blocking layer BCP and a cathode Cr. Cs of the device3Cu2I5The scintillator can be oriented to MAPbI3The semiconductor generates charge energy transfer, and the response time is greatly shortened to 36.6 ns. In addition, the device effectively inhibits the ion migration phenomenon under high electric field intensity, so that the lowest detection dosage rate of the device is higher than that of a direct X-ray detector MAPBI3And an indirect type X-ray detecting device Cs3Cu2I5A 1.5-fold and a 10-fold decrease, respectively. The new X-ray detector provides new opportunities and challenges for next generation products.

Description

Direct-indirect mixed perovskite X-ray detector and light yield calculation method of scintillator of direct-indirect mixed perovskite X-ray detector
Technical Field
The invention belongs to the technical field of X-ray detection, and particularly relates to a direct-indirect mixed perovskite X-ray detector and a method for calculating the light yield of an indirect X-ray detection scintillator material.
Background
The X-ray has high photon energy and strong penetrability, and is widely used for medical examination, radiotherapy, product quality examination, safety examination, aerospace and the like. As a means of converting X-ray photon signals into electrical signals, X-ray detectors are a key part of X-ray application systems. According to the detection principle, the perovskite X-ray detector is divided into an indirect perovskite X-ray detector and a direct perovskite X-ray detector. An indirect perovskite X-ray detector based on a scintillation crystal first converts X-rays into visible light and then converts the visible light into an electrical signal by means of an image sensor. Visible light may scatter in the scintillation crystal during the conversion process, which limits the quantum efficiency and spatial resolution of the indirect-type X-ray detector to a large extent. In addition, the indirect X-ray detector is too bulky to operate anywhere and anytime due to the need to couple with an image sensor. More importantly, most scintillators have a severe afterglow effect, which often results in a long radiation life, so that the response time of the device is prolonged and real-time imaging cannot be realized.
The direct perovskite X-ray detector is a process that a detection material absorbs X-rays to directly generate electron-hole pairs and then outputs charge signals through an external circuit, so that intermediate energy conversion loss is avoided. However, due to the strong X-ray transmission capability, the detection material often requires a relatively thick active layer to completely absorb the X-ray photons. In addition, in order to make the electrical signal converted by the X-ray reach both ends of the electrode vertically, it is usually necessary to apply a high voltage to the device to form a high electric field strength, thereby reducing the carrier diffusion length and preventing signal crosstalk between different pixels in the imaging application. However, it often results in devices with large dark currents causing ion mobility, resulting in photocurrent hysteresis, and also accelerating degradation of perovskite-based electronic devices. Therefore, the development of a perovskite X-ray detector with fast response time, low-dose X-ray detection, good stability and low cost is urgently needed.
Disclosure of Invention
The invention aims to provide a direct-indirect mixed X-ray detector which has the advantages of high response speed, low lower limit of X-ray dose detection, good stability, low cost and the like. The method is characterized in that the method for calculating the light yield of the scintillator material of the indirect X-ray detector saves the cost of using an integrating sphere and provides a method for estimating the light yield of the scintillator for the research field.
1. The invention relates to a preparation method of a direct-indirect mixed X-ray detection material tablet, which comprises the following steps:
(a) will CH3NH3I (MAI) and PbI2Dissolving the raw materials into gamma-butyrolactone (GBL) according to a molar ratio of 1:1, dissolving the raw materials at 70-90 ℃ to obtain a yellow clear solution, quickly filtering the yellow clear solution by using a 0.22 mu m filter head, heating the filtered solution at 110-130 ℃, and slowly volatilizing the solvent to separate out black CH3NH3PbI3(MAPbI3) A crystal;
(b) subjecting the MAPbI prepared in step (a) to3Heating the single crystal for 8-12 hours at 50-70 ℃ in vacuum, and completely removing the solvent;
(c) MAPbI with complete removal of the solvent from step (b)3Grinding the single crystal in an agate mortar for 30-50 min to obtain a direct X-ray detection material MAPbI3A solid powder;
(d) dissolving CsI and CuI in N, N-Dimethylformamide (DMF) according to the molar ratio of 3:2, carrying out ultrasonic treatment for 10-15 min, and filtering the obtained solution by using a filter head with the diameter of 0.22 mu m; placing the obtained yellow clear solution in an open watch glass, and slowly volatilizing the solvent at room temperature to separate out colorless transparent Cs3Cu2I5A crystal;
(e) subjecting the Cs prepared in step (d) to3Cu2I5Heating the single crystal for 8-12 h at 50-70 ℃ in vacuum, completely removing the solvent, and grinding in an agate mortar for 30-50 min to obtain the indirect X-ray detection material Cs3Cu2I5A solid powder;
(f) respectively weighing the MAPbI obtained in the step (c)3Solid powder and Cs obtained in step (e)3Cu2I5Placing the solid powder in an agate mortar for continuously grinding for 10-20 min, and fully and uniformly mixing the solid powder and the agate mortar; cs3Cu2I5Is MAPbI320-40% of the mass;
(g) adding the mixed material obtained in the step (f) into a circular tabletting grinding tool with the diameter of 10-15 mm, and tabletting under the pressure of 0.25-0.3 GPa for 4-5 min;
(h) and (g) carrying out thermal annealing treatment on the pressed wafer in the step (g), wherein the annealing temperature is 100-120 ℃, and the annealing time is 10-20 min, so that the direct-indirect mixed perovskite X-ray detection pressure wafer material for preparing the X-ray detector is obtained.
2. The invention also provides a preparation method of the direct-indirect mixed perovskite X-ray detector, which comprises the following steps of an anode Au, a hole transport layer Spiro-OMeTAD, a direct-indirect mixed perovskite X-ray detection material lamination material and an electron transport layer C from bottom to top60The direct-indirect mixed perovskite X-ray detection pressure measuring chip material is an active layer for absorbing X-ray photons, and the preparation method of the device comprises the following steps:
(a) sticking a direct-indirect mixed type perovskite X-ray detection pressure sheet material on glass (the thickness of the glass is 1mm), then spin-coating a Spiro-OMeTAD chlorobenzene solution on the upper surface of the pressure sheet material, wherein the spin-coating rotation speed is 800-1200 rpm, the spin-coating time is 25-35 s, the concentration of the Spiro-OMeTAD in the Spiro-OMeTAD chlorobenzene solution is 30-35 mg/mL, and the coating amount of the Spiro-OMeTAD chlorobenzene solution is 10-20 mu L/1.326cm2(ii) a Annealing for 3-5 min at 80-120 ℃ to obtain a hole transport layer Spiro-OMeTAD with the thickness of 30-150 nm on the surface of the pressing sheet material;
(b) evaporating an Au electrode on the surface of the hole transport layer Spiro-OMeTAD in the step (a) to form a layer with the thickness of 20-50 nm;
(c) taking the pressing sheet material of the step (b) off the glass, turning the pressing sheet material and placing the pressing sheet material on the glass again, and then evaporating the electron transmission layer C on the surface of one side of the pressing sheet material60The thickness is 20-40 nm;
(d) an electron transport layer C in step (C)60Evaporating and plating a hole blocking layer BCP with the thickness of 8-10 nm;
(e) and (d) evaporating and plating cathode Cr on the hole blocking layer BCP in the step (d) to obtain a direct-indirect mixed type perovskite X-ray detection device with the thickness of 20-50 nm, wherein the thickness of the device is 1.40-1.50 mm.
In the present invention, the vapor deposition is preferably vacuum vapor deposition, and the degree of vacuum in the vapor deposition is preferably 2 × 10-4～5×10-4Pa，C60Preferably the evaporation rate of
Figure GDA0003210108700000032
The evaporation rate of BCP is preferably
Figure GDA0003210108700000033
The evaporation rate of Au is preferably
Figure GDA0003210108700000034
The evaporation rate of Cr is preferably
Figure GDA0003210108700000035
In the present invention, the Spiro-OMeTAD is named 2,2',7,7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino ] -9,9' -spirobifluorene in the Chinese name, and the BCP is named 2, 9-dimethyl-4, 7-biphenyl-1, 10-phenanthroline in the Chinese name, and all of the above drugs are commercially available without further purification. The structural formulas are respectively as follows:
Figure GDA0003210108700000031
3. the invention provides a method for calculating the light yield of a scintillator material of an indirect X-ray detector, which comprises the following steps:
(a) weighing a certain amount of Cs3Cu2I5Grinding the scintillator crystal by using an agate mortar for 30-50 min;
(b) and (b) adding the material obtained in the step (a) into a circular tabletting grinding tool with the diameter of 13mm, wherein the pressure is 0.25-0.3 GPa, and the tabletting time is 4-5 min.
(c) Subjecting the Cs obtained in step (b) to3Cu2I5Tablet placementOn the silicon diode, adjusting the X-ray dosage rate by changing the thickness of different lead plates, and correcting the X-ray dosage rate by using a commercial X-ray dosimeter; when X-rays are applied, they will penetrate the scintillator surface and generate excitons internally, followed by Cs3Cu2I5Blue fluorescence emitted by the scintillator is collected by a silicon diode, and finally, a pulse current signal is output through an external circuit; the pulse current signal is Cs3Cu2I5A common current signal of the scintillator and the silicon diode response to X-rays; then obtaining Cs by adjusting different X-ray dose rates3Cu2I5A common current signal responded by the scintillator and the silicon diode under different X-ray dose rates;
(d) cs in step (c) in order to reject the current signal of the silicon diode in response to X-rays3Cu2I5A layer of black adhesive tape is pasted between the scintillator and the silicon diode; one of the purposes of adding the black adhesive tape is that the black adhesive tape can block the fluorescence emitted by the scintillator and the signal not received by the silicon diode, and the second is the Cs3Cu2I5The scintillator is placed on the black adhesive tape, so as to ensure that the absorption efficiency of the silicon diode on the X-ray is consistent with that of the step (c); and (c) adjusting the same X-ray dose rate as that in the step (c) to obtain current signals of the silicon diode at different X-ray dose rates.
(e) Cs obtained in the step (c) under different X-ray dose rates3Cu2I5Subtracting the current signal of the silicon diode obtained in the step (d) from the current signal of the sum of the scintillator and the silicon diode to obtain a value which is Cs3Cu2I5A current signal of the scintillator;
(f) converting the current signals obtained in the step (e) under different X-ray dose rates into corresponding light intensities according to the following formula:
Figure GDA0003210108700000041
Figure GDA0003210108700000042
wherein I0Is the light intensity, IsIs the current signal value, R is the responsivity, S is the area of the silicon diode, EQEsiIs the quantum efficiency of a silicon diode, q is the charge, h is the planck constant, and upsilon is the frequency. Wherein EQEsiThe quantum efficiency tester is used for testing.
(g) Calculating the light intensity obtained in the step (f) under different X-ray dose rates to obtain Cs under different X-ray dose rates3Cu2I5The Light Yield (LY) of the scintillator, the formula is as follows:
Figure GDA0003210108700000043
Figure GDA0003210108700000044
Figure GDA0003210108700000045
wherein N is1Is the number of photons emitted by the scintillator, N2Is the number of photons, I, theoretically generated by irradiation of 120keV X-rays on the scintillator0Is the light intensity, S1The surface area of a sphere is taken as the radius of the distance between the silicon diode and the center of scintillator emission, t is the response time of the scintillator, h is the planckian constant, and upsilon is the frequency. D is the X-ray dose rate, phi is the absorption efficiency of the sample on X-rays, mumIs the mass attenuation coefficient, E is the X-ray energy of a single photon in 120keV, S1The surface area of the sphere, which is the radius of the distance between the silicon diode and the center of scintillator emission, is taken as t, the response time of the scintillator.
In the present invention, Cs obtained by the method for calculating the light yield of a scintillator3C2I5The average value of (A) is 26000Photos/MeV, and the theoretical reported value is 29000Photos/MeV approach.
Compared with the prior art, the direct-indirect mixed X-ray detector with quick response and low dose rate detection and the preparation method thereof provided by the invention have the following advantages:
the invention provides a direct-indirect mixed perovskite tabletting device with quick response and low dose detection rate, which can be used for 120KeV high-energy hard X-ray detection. Due to Cs3Cu2I5And MAPbI3Energy level matching between, Cs3Cu2I5The scintillator can be oriented to MAPbI3The semiconductor is subjected to rapid charge energy transfer, so that the direct-indirect mixed perovskite device is opposite to Cs3Cu2I5The response time of the indirect detection material of the scintillator is reduced from the original 1.07 mu s to 36.6 ns. In addition, since the scintillator Cs3Cu2I5Present in MAPbI3In the grain boundary of (1), MAPbI is blocked3The resistivity of the direct-indirect mixed perovskite is increased, the dark current and the noise are reduced, the ion migration phenomenon is effectively inhibited under high electric field intensity, and the lowest detection dose of the device is relative to that of a direct X-ray detection device MAPbI3Reduced by 1.5 times, and compared with an indirect X-ray detection device Cs3Cu2I5The reduction is 10 times. Under the electric field strength of 700V/cm, after the device is placed for 26 days under the condition of no packaging air, the original photocurrent signal is still kept for the hard X-ray pulse, and the loss of the signal-to-noise ratio is avoided, so that the device has good working stability. In addition, we also provide a theoretical model for measuring the light yield of the scintillator, and Cs is obtained by formula calculation3Cu2I5The light yield value is close to that reported in the literature, so that the use of an expensive integrating sphere is avoided, and the cost of experimental testing is saved.
Drawings
FIG. 1 is a schematic structural diagram of an X-ray detector according to the present invention, and a mechanism diagram (a) and an energy level structure diagram (b); which comprises the following steps: the anode comprises an anode 1, a hole transport layer 2, a direct-indirect mixed perovskite active layer 3, an electron transport layer 4, a hole blocking layer 5 and a cathode 6; .
FIG. 2 shows the preparation of Cs with different mass ratios3Cu2I5The lowest detected dose map of the perovskite detector in response to X-rays.
FIG. 3 shows the preparation of 30% Cs3Cu2I5Hybrid X-ray detector and direct X-ray detector MAPbI3The abscissa of the resistivity test curve is the applied electric field strength of the device, and the ordinate is the dark current density of the device.
FIG. 4 shows the preparation of 30% Cs3Cu2I5Hybrid X-ray detector and direct X-ray detector MAPbI3The abscissa of the noise test curve of (2) is frequency, and the ordinate is noise of the device.
FIG. 5 shows the preparation of 30% Cs3Cu2I5Ion mobility curves of the devices at high electric field strengths.
FIG. 6 shows Cs prepared3Cu2I5Time resolved spectroscopic data of the press sheet material.
FIG. 7 shows the preparation of 30% Cs3Cu2I5Transient photocurrent response curves of the devices under continuous-100V bias.
FIG. 8 shows Cs prepared3Cu2I5Theoretical calculation curve of light yield of scintillator sheet material.
FIG. 9 shows the preparation of 30% Cs3Cu2I5The photocurrent stability curve of the device for the X response, with the abscissa being the time to continuously apply a-100V bias to the device and the ordinate being the photocurrent of the device.
Fig. 1 shows a schematic structural diagram of the X-ray detector of the present invention, as well as a mechanism diagram (a) and an energy level diagram (b) (a schematic structural diagram of a direct-indirect hybrid perovskite tablet device X-ray detector). The composite material comprises an Au anode 1, a Spiro-OMeTAD hole transport layer 2, a direct-indirect mixed perovskite active layer 3 and C60An electron transport layer 4, a BCP hole blocking layer 5 and a Cr cathode 6. MAPbI can be seen from the energy level diagram (FIG. 1b)3And Cs3Cu2I5Two material formationHeterojunction, Cs3Cu2I5Both electrons and holes can be transferred to MAPbI3. From the charge transfer process, we propose that there are two different charge collection paths in a hybrid X-ray detector (fig. 1 a): path 1 is MAPbI3Direct absorption of X-rays generates electron-hole pairs, which are charge collected under continuous bias. Path 2 is Cs3Cu2I5Absorbing X-rays and rapidly transferring electrons and holes to MAPbI before it recombines with radiation3And then charge collection is performed according to path 1.
FIG. 2 shows the preparation of Cs with different mass ratios3Cu2I5The perovskite detector responds to the lowest detection dose graph of X-ray (prepared Cs containing different mass ratios)3Cu2I5The lowest detection dose rate data of the perovskite detector in response to X-rays). The results show that the mass fraction is 30% Cs3Cu2I5The lowest detection quantity rate of the device is the lowest and can reach 0.41 mu Gyair s-1(far below medical dose rate of 5.5 μ Gyair s-1) Is a direct detection device MAPbI3(minimum detection dose rate of 0.63. mu. Gy)air s-1) 1.5 times of that of the material scintillator Cs, and indirectly detects the material scintillator Cs3Cu2I5(minimum detection rate of 4. mu. Gy)air s-1) 10 times higher than the original value.
FIG. 3 shows the preparation of 30% Cs3Cu2I5Hybrid X-ray detector and direct X-ray detector MAPbI3Resistivity test curve (30% Cs)3Cu2I5X-ray detector and direct X-ray detector MAPbI3Resistivity test data). Data in the figure indicate 30% Cs3Cu2I5The bulk resistivity of the perovskite X-ray detection device is 5.40X 107Omega cm, ratio direct detection device MAPbI3(6.53×107Ω cm) 1.21 times higher, higher resistivity indicates 30% Cs3Cu2I5Dark current ratio MAPbI of device3The direct type X-ray detection device is low.
FIG. 4 is a drawingPrepared 30% Cs3Cu2I5Hybrid X-ray detector and direct X-ray detector MAPbI3Noise test curve (30% Cs)3Cu2I5Device and direct X-ray detection tabletting device MAPbI3Noise test data). Wherein the Instrument noise is the noise of the test Instrument system. The results showed 30% Cs3Cu2I5Device comparison with direct detection device MAPbI3Has low noise.
FIG. 5 shows the preparation of 30% Cs3Cu2I5Ion migration curve of device at high electric field intensity (prepared 30% Cs)3Cu2I5Ion mobility data for devices at different high electric field strengths). The results show that MAPbI is relative to a direct detection device3The ion migration of the device under high electric field intensity is effectively inhibited, which lays a foundation for low-dosage-rate X-ray detection.
FIG. 6 shows Cs prepared3Cu2I5Time-resolved spectroscopic data of the sheet Material (prepared Cs)3Cu2I5Time-resolved spectroscopic data of the press sheet material), the results indicated Cs3Cu2I5The fluorescence lifetime of (a) was 1.07. mu.s.
FIG. 7 shows the preparation of 30% Cs3Cu2I5Transient photocurrent response curve (prepared 30% Cs) of the device under continuous-100V bias3Cu2I5Transient photocurrent response data for a sheeting device under a continuous-100V bias). The result shows that the device has a fast response speed which can reach 36.6 ns.
FIG. 8 shows Cs prepared3Cu2I5Theoretical calculation curve of light yield of scintillator pressure sheet Material (Cs prepared)3Cu2I5Theoretical calculation data of the light yield of the scintillator). The result shows that the average value of the light yield calculated by the formula is 26000Photons/MeV under different dosage rates, and is close to the value 29000Photons/MeV reported in the literature.
FIG. 9 shows the preparation of 30% Cs3Cu2I5Photocurrent stability curve of device to X response (prepared 30% Cs)3Cu2I5Photocurrent pulse signal of the device in response to X-rays). The result shows that the device still maintains the original photocurrent signal for 120KeV hard X-ray pulse under the electric field strength of 700V/cm and the condition of no packaging air after being placed for 26 days, and the signal-to-noise ratio loss does not exist, so that the device has good working stability.
Detailed Description
The present invention will be further described with reference to the following drawings and specific examples, but the present invention is not limited to the following examples. In the present invention, unless otherwise specified, each component in the preparation method is a commercially available product well known to those skilled in the art.
Example 1:
the invention provides a preparation method of a direct-indirect mixed X-ray detection material tablet, which comprises the following steps:
(a) will CH3NH3I (MAI) and PbI2Dissolving in gamma-butyrolactone (GBL) at a molar ratio of 1:1, heating at 80 deg.C to obtain yellow clear solution, rapidly filtering with 0.22 μm filter head, heating the filtered solution at 120 deg.C, slowly volatilizing the solvent to obtain MAPbI3Black crystals.
(b) Subjecting the MAPbI prepared in step (a) to3Heating the single crystal at 60 deg.C for 10 hr under vacuum to completely remove solvent;
(c) drying the MAPbI in the step (b)3The single crystals were ground in an agate mortar for 40min to make bulk single crystals into solid powder.
(d) Dissolving CsI and CuI in N, N-Dimethylformamide (DMF) according to the molar ratio of 3:2, performing ultrasonic treatment for 12min, filtering the obtained solution by using a 0.22 mu m filter head to obtain a yellow clear solution, placing the yellow clear solution in an open watch glass, and slowly volatilizing the solvent at room temperature to separate out colorless transparent Cs3Cu2I5A crystal;
(e) subjecting the Cs prepared in step (d) to3Cu2I5Heating the single crystal at 60 deg.C for 10 hr under vacuum to completely remove solvent, and grinding in agate mortar to 40min, so that the bulk single crystal becomes a solid powder.
(f) Separately weighing the MAPbI prepared in the step (c)3Solid powder and Cs prepared in step (e)3Cu2I5Placing the solid powder in an agate mortar, and continuously grinding for 15min until the solid powder and the agate mortar are fully and uniformly mixed;
(g) adding the mixed material obtained in the step (f) into a circular tabletting grinding tool with the diameter of 13mm, and tabletting under the pressure of 0.3GPa for 5 min;
(h) and (g) carrying out thermal annealing treatment on the pressed wafer in the step (g), wherein the annealing temperature is 100 ℃, and the annealing time is 15min, so that the direct-indirect mixed perovskite X-ray detection pressure wafer material for preparing the X-ray detector is obtained.
In the present invention, the indirect X-ray detecting material Cs3Cu2I5Detecting MAPbI for direct X-ray 330% of the mass.
Example 2
The invention provides a direct-indirect mixed type perovskite X-ray detector which consists of an anode, a hole transmission layer, a direct-indirect mixed type perovskite X-ray detection pressure measuring sheet material, an electron transmission layer, a hole barrier layer and a cathode from bottom to top, wherein a direct-indirect mixed type perovskite X-ray detection pressure sheet is an active layer which is made of materials and absorbs X-ray photons, and the preparation method comprises the following steps:
(a) and (3) pasting the direct-indirect mixed perovskite X-ray detection pressing sheet material on square glass, wherein the area of the glass is 1.5 multiplied by 1.5cm, then spin-coating chlorobenzene solution containing Spiro-OMeTAD on the front surface of the pressing sheet material, and then annealing at 100 ℃ for 5min to obtain the pressing sheet material containing the hole transport layer Spiro-OMeTAD. The thickness of the hole transport layer was 50 nm.
(b) And (b) evaporating an Au electrode on the spin-coated hole transport layer Spiro-OMeTAD in the step (a) to form a thickness of 50 nm.
(c) Taking the pressing sheet material of the step (b) off the glass, turning the pressing sheet material and placing the pressing sheet material on the glass again, and then evaporating the electron transmission layer C on the surface of one side of the pressing sheet material60The thickness is 30 nm;
(d) continuing at C of step (C)60And a hole blocking layer BCP is vapor-plated on the electron transport layer, and the thickness is 10 nm.
(e) And (d) continuously evaporating cathode Cr on the hole blocking layer BCP of the step (d) to a thickness of 50 nm. Finally, the direct-indirect mixed perovskite X-ray detector can be obtained. The thickness of the prepared direct-indirect mixed perovskite X-ray detector is 1.45 mm.
The rotating speed of the spin coating in the step (a) is 1000rpm, and the time is 30 s. The concentration of the chlorobenzene solution of Spiro-OMeTAD is 30 mg/mL. The amount of the chlorobenzene solution coated by the Spiro-OMeTAD is 15 mu L/1.326cm2。
In the present invention, the vapor deposition is vacuum vapor deposition, and the degree of vacuum in the vapor deposition is 4 × 10-4Pa，C60Has an evaporation rate of
Figure GDA0003210108700000091
The evaporation rate of BCP is
Figure GDA0003210108700000092
The evaporation rate of Au is
Figure GDA0003210108700000093
The evaporation rate of Cr is
Figure GDA0003210108700000094
Comparative example 1:
the invention provides a tabletting step of a direct X-ray detection material and a preparation method of a tabletting device, which comprises the following steps:
(a) mixing MAI with PbI2Dissolving in GBL at a molar ratio of 1:1, dissolving at 80 deg.C to obtain yellow clear solution, rapidly filtering with 0.22 μm filter head, heating the filtered solution at 120 deg.C, and slowly evaporating to separate MAPbI3Black crystals.
(b) Subjecting the MAPbI prepared in step (a) to3The single crystal was heated at 60 ℃ for 10 hours under vacuum to completely remove the solvent.
(c) Drying in step (b)MAPbI3The single crystals were ground in an agate mortar for 40min to make bulk single crystals into solid powder.
(d) Subjecting the MAPbI obtained in step (c) to3Adding the solid powder into a circular tabletting grinding tool with the diameter of 13mm, and tabletting under the condition of the pressure of 0.3GPa for 5 min;
(e) and (d) carrying out thermal annealing treatment on the pressed wafer in the step (d), wherein the annealing temperature is 100 ℃, and the annealing time is 15min, so that the direct perovskite X-ray detection pressure wafer material for preparing the X-ray detector is obtained.
(f) Applying the press sheet material obtained in step (e) to square glass with an area of 1.5 × 1.5cm, and spin-coating a chlorobenzene solution containing Spiro-OMeTAD on the front surface of the press sheet material, wherein the spin-coating speed is preferably 1000rpm and the time is preferably 30 s. The concentration of the solution of Spiro-OMeTAD in chlorobenzene is preferably 30 mg/mL. The amount of the chlorobenzene solution coated by the Spiro-OMeTAD is preferably 15 mu L/1.326cm2. Then, annealing was performed at 100 ℃ for 5min to obtain a laminate material containing a hole transport layer Spiro-OMeTAD. The thickness of the hole transport layer was 50 nm.
(g) And (f) evaporating an Au electrode on the spin-coated hole transport layer Spiro-OMeTAD in the step (f) to form a thickness of 50 nm.
(h) Taking the pressing sheet material of the step (g) off the glass, turning the pressing sheet material, placing the pressing sheet material on the glass again, and then evaporating the electron transmission layer C on the surface of one side of the pressing sheet material60The thickness is 30 nm;
(i) continuing at C of step (h)60And a hole blocking layer BCP is vapor-plated on the electron transport layer, and the thickness is 10 nm.
(j) And (f) continuously evaporating cathode Cr on the hole blocking layer BCP of the step (i) to a thickness of 50 nm. Finally, the direct perovskite X-ray detector can be obtained. The prepared direct perovskite X-ray detector MAPbI3Is 0.98 mm.
The spin coating in step (e) is preferably performed at 1000rpm for 30 s. The concentration of the solution of Spiro-OMeTAD in chlorobenzene is preferably 30 mg/mL. The amount of the chlorobenzene solution coated by the Spiro-OMeTAD is preferably 15 mu L/1.326cm2。
In the present invention, the vapor deposition is vacuum vapor deposition, and the degree of vacuum in the vapor deposition is 4 × 10-4Pa，C60Has an evaporation rate of
Figure GDA0003210108700000101
The evaporation rate of BCP is
Figure GDA0003210108700000102
The evaporation rate of Au is
Figure GDA0003210108700000103
The evaporation rate of Cr is
Figure GDA0003210108700000104
Comparative example 2:
the invention provides a tabletting step of an indirect X-ray detection material and a preparation method of a tabletting device, which comprises the following steps:
(a) dissolving CsI and CuI in DMF at a molar ratio of 3:2, performing ultrasonic treatment for 12min, filtering the obtained solution with a filter tip of 0.22 μm to obtain a yellow clear solution, placing the yellow clear solution in an open watch glass, and slowly volatilizing the solvent at room temperature to separate out colorless transparent Cs3Cu2I5A crystal;
(b) subjecting the Cs prepared in step (a) to3Cu2I5Heating the single crystal at 60 ℃ for 10h under vacuum to completely remove the solvent, and grinding in an agate mortar for 40min to obtain solid powder of the bulk single crystal.
(c) Subjecting the Cs obtained in step (b) to3Cu2I5Adding the solid powder into a circular tabletting grinding tool with the diameter of 13mm, and tabletting under the condition of the pressure of 0.3GPa for 5 min;
(d) and (c) carrying out thermal annealing treatment on the pressed wafer in the step (c), wherein the annealing temperature is 100 ℃, and the annealing time is 15min, so that the indirect perovskite X-ray detection pressure wafer material for preparing the X-ray detector is obtained.
(e) And (d) attaching the pressing sheet material of the step (d) on square glass, wherein the area of the glass is 1.5 multiplied by 1.5cm, spin-coating a chlorobenzene solution containing Spiro-OMeTAD on the front surface of the pressing sheet material, and then annealing at 100 ℃ for 5min to obtain the pressing sheet material containing the hole transport layer Spiro-OMeTAD. The thickness of the hole transport layer was 50 nm.
(f) And (e) evaporating an Au electrode on the spin-coated hole transport layer Spiro-OMeTAD in the step (e) to form a thickness of 50 nm.
(g) Taking the pressing sheet material of the step (f) off the glass, turning the pressing sheet material, placing the pressing sheet material on the glass again, and evaporating the electron transmission layer C on the surface of one side of the pressing sheet material60The thickness is 30 nm;
(h) c continuing in step (g)60And a hole blocking layer BCP is vapor-plated on the electron transport layer, and the thickness is 10 nm.
(i) And (h) continuously evaporating cathode Cr on the hole blocking layer BCP of the step (h) to form a thickness of 50 nm. Finally, the indirect perovskite X-ray detector can be obtained. Prepared indirect perovskite X-ray detector Cs3Cu2I5Is 1.60 mm.
The spin coating in step (e) is preferably performed at 1000rpm for 30 s. The concentration of the solution of Spiro-OMeTAD in chlorobenzene is preferably 30 mg/mL. The amount of the chlorobenzene solution coated by the Spiro-OMeTAD is preferably 15 mu L/1.326cm2。
In the present invention, the vapor deposition is vacuum vapor deposition, and the degree of vacuum in the vapor deposition is 4 × 10-4Pa，C60Has an evaporation rate of
Figure GDA0003210108700000111
The evaporation rate of BCP is
Figure GDA0003210108700000112
The evaporation rate of Au is
Figure GDA0003210108700000113
The evaporation rate of Cr is
Figure GDA0003210108700000114
Example 3
The invention provides a method for calculating the Light Yield (LY) of a scintillator material of an indirect X-ray detector, which comprises the following steps:
(a) weighing a certain amount of Cs3Cu2I5Scintillator crystals were ground with an agate mortar for at least 40 min.
(b) And (c) adding the material obtained in the step (a) into a circular tabletting grinding tool with the diameter of 13mm, wherein the pressure is 0.3GPa, and the tabletting time is 5 min.
(c) Subjecting the Cs obtained in step (b) to3Cu2I5The tablets were placed on silicon diodes and the dose rate of the X-rays was then adjusted by varying the thickness of the lead plates and corrected with a commercial X-ray dosimeter. Wherein when an X-ray dose rate is applied, X-rays will penetrate the scintillator surface and generate excitons internally, followed by Cs3Cu2I5Blue fluorescence emitted by the scintillator is collected by the silicon diode, and finally, a pulse current signal is output through an external circuit. The pulse current signal is Cs3Cu2I5Current signals of the scintillator and silicon diode response to X-rays. Then obtaining Cs by adjusting different X-ray dose rates3Cu2I5Current signals of the scintillator and the silicon diode at different X-ray dose rates.
(d) In order to exclude the current signal of the silicon diode in response to X-ray, Cs of step (c)3Cu2I5One purpose of the black adhesive tape is to block the fluorescence emitted by the scintillator and prevent the signal from being received by the silicon diode, and the other purpose is to stick a layer of black adhesive tape between the scintillator and the silicon diode3Cu2I5The scintillator is placed on the black adhesive tape, so as to ensure that the absorption efficiency of the silicon diode on the X-ray is consistent with that of the step (c); and (c) adjusting the same X-ray dose rate as that in the step (c) to obtain current signals of the silicon diode at different X-ray dose rates.
(e) Cs obtained in the step (c) under different X-ray dose rates3Cu2I5Of scintillators plus silicon diodesSubtracting the current signal of the silicon diode obtained in the step (d) from the current signal to obtain a value which is Cs3Cu2I5Current signal of the scintillator.
(f) Converting the photocurrent obtained in step (e) at different X-ray dose rates into corresponding light intensity. Specifically, the following formula is used:
Figure GDA0003210108700000121
Figure GDA0003210108700000122
wherein I0Is the light intensity, IsIs the current signal, R is the responsivity, S is the area of the silicon diode, EQEsiIs the quantum efficiency of silicon diodes. q is the charge, h is the planck constant, and ν is the frequency. Wherein EQEsiThe quantum efficiency tester is used for testing.
(g) Calculating the light intensity obtained in the step (f) under different X-ray dose rates to obtain Cs under different X-ray dose rates3Cu2I5Light Yield (LY) of the scintillator. The specific calculation formula is as follows:
Figure GDA0003210108700000123
Figure GDA0003210108700000124
Figure GDA0003210108700000125
wherein N is1Is the number of photons emitted by the scintillator, N2Is the number of photons, I, theoretically generated by irradiation of 120keV X-rays on the scintillator0Is the light intensity, S1So as to use a silicon diode and a scintillator emission centerThe distance between is the surface area of the sphere of radius, t is the response time of the scintillator, h is the planck constant, and υ is the frequency. D is the X-ray dose rate, phi is the absorption efficiency of the sample on X-rays, mumIs the mass attenuation coefficient, E is the X-ray energy of a single photon in 120keV, S1The surface area of the sphere, which is the radius of the distance between the silicon diode and the center of scintillator emission, is taken as t, the response time of the scintillator. The light yield of a scintillator is expressed by the ability of the scintillator to emit light, which represents the ability of a particle to convert energy through the scintillator to light energy, with the number of photons detected by the photodetector. Light yield of the scintillator by the method the number of photons N generated by the scintillator1Number of photons N generated in the sample in response to the X-ray irradiation2The ratio of (a) to (b).
The direct-indirect mixed perovskite tabletting device with quick response, low dose rate detection and low cost can be used for 120KeV high-energy hard X-ray detection. The novel X-ray detector combines the advantages of a direct perovskite semiconductor and an indirect perovskite scintillator and provides new opportunities and challenges for next-generation products.

Claims (5)

1. A direct-indirect hybrid perovskite X-ray detector, characterized by: from bottom to top, the anode Au, the hole transport layer Spiro-OMeTAD, the direct-indirect mixed perovskite X-ray detection material lamination material and the electron transport layer C60A hole blocking layer BCP and a cathode Cr; the direct-indirect mixed perovskite X-ray detection pressure cell material is an active layer for absorbing X-ray photons, and is prepared by the following steps:
1) will CH3NH3I and PbI2Dissolving the raw materials into gamma-butyrolactone according to a molar ratio of 1:1, dissolving the raw materials into a yellow clear solution at 70-90 ℃, quickly filtering the yellow clear solution by using a filter head with the diameter of 0.22 mu m, heating the filtered solution at 110-130 ℃, and slowly volatilizing the solvent to separate out black MAPbI3A crystal;
2) MAPbI prepared in the step (1)3Heating the single crystal for 8-12 hours at 50-70 ℃ in vacuum, and completely removing the solvent;
3) MAPbI with complete removal of the solvent from step (2)3Grinding the single crystal in an agate mortar for 30-50 min to obtain a direct X-ray detection material MAPbI3A solid powder;
4) dissolving CsI and CuI in N, N-dimethylformamide according to the molar ratio of 3:2, carrying out ultrasonic treatment for 10-15 min, and filtering the obtained solution by using a filter head with the diameter of 0.22 mu m; placing the obtained yellow clear solution in an open watch glass, and slowly volatilizing the solvent at room temperature to separate out colorless transparent Cs3Cu2I5A crystal;
5) the Cs prepared in the step (4)3Cu2I5Heating the single crystal for 8-12 h at 50-70 ℃ in vacuum, completely removing the solvent, and grinding in an agate mortar for 30-50 min to obtain the indirect X-ray detection material Cs3Cu2I5A solid powder;
6) respectively weighing the MAPbI obtained in the step (3)3Solid powder and Cs obtained in step (5)3Cu2I5Placing the solid powder in an agate mortar for continuously grinding for 10-20 min, and fully and uniformly mixing the solid powder and the agate mortar; cs3Cu2I5Is MAPbI320-40% of the mass;
7) adding the mixed material obtained in the step (6) into a circular tabletting grinding tool with the diameter of 10-15 mm, and tabletting under the pressure of 0.25-0.3 GPa for 4-5 min;
8) and (3) carrying out thermal annealing treatment on the wafer pressed in the step (7), wherein the annealing temperature is 100-120 ℃, and the annealing time is 10-20 min, so as to obtain the direct-indirect mixed perovskite X-ray detection wafer material for preparing the X-ray detector.
2. A method for preparing a direct-indirect hybrid perovskite X-ray detector as claimed in claim 1, comprising the steps of:
a) attaching the direct-indirect mixed perovskite X-ray detection pressing sheet material to glass, spin-coating a chlorobenzene solution of Spiro-OMeTAD on the upper surface of the pressing sheet material, annealing at 100 ℃, and obtaining a hole transport layer Spiro-OMeTAD with the thickness of 30-150 nm on the upper surface of the pressing sheet material;
b) evaporating an Au electrode on the surface of the hole transport layer Spiro-OMeTAD in the step a) with the thickness of 20-50 nm;
c) taking the press sheet material of the step b) off the glass, turning the press sheet material and placing the press sheet material on the glass again, and then evaporating an electron transmission layer C on the surface of one side of the press sheet material60The thickness is 20-40 nm;
d) electron transport layer C in step C)60Evaporating and plating a hole blocking layer BCP with the thickness of 8-10 nm;
e) and d) evaporating and plating cathode Cr on the hole blocking layer BCP in the step d) to obtain a direct-indirect mixed type perovskite X-ray detector with the thickness of 20-50 nm, wherein the thickness of the detector is 1.40-1.50 mm.
3. The method for producing a direct-indirect hybrid perovskite X-ray detector as claimed in claim 2, wherein: the spin-coating rotation speed of the chlorobenzene solution of the Spiro-OMeTAD is 800-1200 rpm, the spin-coating rotation time is 25-35 s, the concentration of the Spiro-OMeTAD in the chlorobenzene solution of the Spiro-OMeTAD is 30-35 mg/mL, and the coating amount of the chlorobenzene solution of the Spiro-OMeTAD is 10-20 mu L/1.326cm2(ii) a Then annealing for 3-5 min, wherein the annealing temperature range is 80-120 ℃.
4. The method for producing a direct-indirect hybrid perovskite X-ray detector as claimed in claim 2, wherein: the vapor deposition is vacuum vapor deposition with vacuum degree of 2 × 10-4～5×10-4Pa；C60Has an evaporation rate of
Figure FDA0003114491550000021
The evaporation rate of BCP is
Figure FDA0003114491550000022
The evaporation rate of Au is
Figure FDA0003114491550000023
The evaporation rate of Cr is
Figure FDA0003114491550000024
5. A method for calculating the light yield of a scintillator material of an indirect X-ray detector comprises the following steps:
(a) weighing a certain amount of Cs3Cu2I5Grinding the scintillator crystal by using an agate mortar for at least 30-50 min;
(b) adding the material obtained in the step (a) into a circular tabletting grinding tool with the diameter of 13mm, wherein the pressure is 0.25-0.3 GPa, and the tabletting time is 4-5 min;
(c) subjecting the Cs obtained in step (b) to3Cu2I5Placing the pressed sheet on a silicon diode, adjusting the dosage rate of the X-rays by changing the thickness of different lead plates, and correcting the dosage rate of the X-rays by using a commercial X-ray dosimeter; wherein when an X-ray dose rate is applied, X-rays will penetrate the scintillator surface and generate excitons internally, followed by Cs3Cu2I5Blue fluorescence emitted by the scintillator is collected by a silicon diode, and finally, a pulse current signal is output through an external circuit; the pulse current signal is Cs3Cu2I5A current signal of the scintillator and silicon diode common response to X-rays; then obtaining Cs by adjusting different X-ray dose rates3Cu2I5Current signals of the scintillator and the silicon diode under different X-ray dose rates;
(d) in order to exclude the current signal of the silicon diode in response to X-ray, Cs of step (c)3Cu2I5One purpose of the black adhesive tape is to block the fluorescence emitted by the scintillator and prevent the signal from being received by the silicon diode, and the other purpose is to stick a layer of black adhesive tape between the scintillator and the silicon diode3Cu2I5The scintillator is placed on the black adhesive tape, so as to ensure that the absorption efficiency of the silicon diode on the X-ray is consistent with that of the step (c); then, adjusting the same X-ray dose rate as that in the step (c) to obtain current signals of the silicon diode under different X-ray dose rates;
(e) cs obtained in the step (c) under different X-ray dose rates3Cu2I5Subtracting the current signal of the silicon diode obtained in the step (d) from the current signal of the sum of the scintillator and the silicon diode to obtain a value which is Cs3Cu2I5A current signal of the scintillator;
(f) converting the photocurrents obtained in the step (e) under different X-ray dose rates into corresponding light intensities, wherein the calculation formula is as follows:
Figure FDA0003114491550000031
Figure FDA0003114491550000032
wherein I0Is the light intensity, IsIs the current signal, R is the responsivity, S is the area of the silicon diode, EQEsiIs the quantum efficiency of a silicon diode; q is the charge, h is the planck constant, and upsilon is the frequency; wherein EQEsiThe method comprises the following steps of (1) testing by using a quantum efficiency tester;
(g) calculating the light intensity obtained in the step (f) under different X-ray dose rates to obtain Cs under different X-ray dose rates3Cu2I5The Light Yield (LY) of the scintillator is calculated as follows:
Figure FDA0003114491550000033
Figure FDA0003114491550000034
Figure FDA0003114491550000035
wherein N is1Is the number of photons emitted by the scintillator, N2Is the number of photons, I, theoretically generated by 120KeV X-ray irradiation on the scintillator0Is the light intensity, S1The surface area of a sphere taking the distance between a silicon diode and the emitting center of the scintillator as a radius is taken as a reference, t is the response time of the scintillator, h is the Planck constant, and upsilon is the frequency; d is the X-ray dose rate, phi is the absorption efficiency of the sample on X-rays, mumIs the mass attenuation coefficient, E is the X-ray energy of a single photon in 120KeV, S1The surface area of the sphere, which is the radius of the distance between the silicon diode and the center of scintillator emission, is taken as t, the response time of the scintillator.
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