CN106947463B - Preparation method of CdS-coated inorganic perovskite nano material, product and application thereof - Google Patents

Preparation method of CdS-coated inorganic perovskite nano material, product and application thereof Download PDF

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CN106947463B
CN106947463B CN201710166337.3A CN201710166337A CN106947463B CN 106947463 B CN106947463 B CN 106947463B CN 201710166337 A CN201710166337 A CN 201710166337A CN 106947463 B CN106947463 B CN 106947463B
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inorganic perovskite
octadecene
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唐孝生
李诗琪
臧志刚
刘洪均
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Chongqing Ding Ding Photoelectric Technology Co Ltd
Chongqing University
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Chongqing University
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Abstract

The invention relates to a preparation method of CdS-coated inorganic perovskite nano material, which comprises the steps of mixing cadmium oxide, oleic acid and octadecene under the environment of continuous nitrogen, heating for reaction to obtain cadmium oleate solution, adding octadecene and sulfur powder to obtain cadmium oleate-sulfur powder solution, and dropwise adding the cadmium oleate-sulfur powder mixed solution into CsPbX3And (x ═ Cl, Br and I), and centrifuging after the reaction is finished to obtain the CdS coated inorganic perovskite nano material. The CdS-coated inorganic perovskite nano material prepared by the method has high stability, and fluorescence is not quenched when the CdS-coated inorganic perovskite nano material is contacted with water; and the fluorescent material has non-flicker property, the fluorescent intensity track can not be greatly changed, and the fluorescent material is particularly important in the application of light-emitting diodes.

Description

Preparation method of CdS-coated inorganic perovskite nano material, product and application thereof
Technical Field
The invention belongs to the technical field of nano particles, and relates to a preparation method of a CdS-coated inorganic perovskite nano material, and a product and application thereof.
Background
Inorganic perovskite nano material (CsPbX)3X ═ Cl, Br, I) is a novel functional material, has special properties in the aspects of light emitting diodes, solar cells, photodetectors and the like, and is widely applied to the field of photoelectric devices, perovskite quantum dots prepared by a thermal injection method are reported for the first time on Nano Kuaiji (Nano Lett.,2015,15(6),3692) of the American chemical society, but perovskite quantum dots prepared by the method have weak stability, and fluorescence is gradually quenched when the perovskite quantum dots are contacted with water. And the perovskite quantum dots have obvious flicker, which is not favorable for the application of the perovskite quantum dots in the aspect of light-emitting diodes. In recent years, CsPbX3Nanomaterials have attracted a great deal of research attention, particularly their scintillation and stability. For example, the American chemical society, Nano Lett.,2016,16(10),6425, reported a simple colloidal preparation method, which successfully prepared non-scintillating CsPbI3A perovskite material; nanoscale,2017,9(2),631 of the royal chemical society of England reported an increase in CsPbX3A method for water stabilization, whereby the perovskite is dissolved in a polar solvent by replacing the surface ligand. There is a need for a new preparation method for CsPbX3The perovskite nano material can inhibit the flicker and improve the stability at the same time.
Disclosure of Invention
In view of this, the present invention aims to provide a method for preparing a CdS-coated inorganic perovskite nano-material and a product thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
1. a preparation method of a CdS-coated inorganic perovskite nano material comprises the following steps:
(1) under the environment of continuous nitrogen, cadmium oxide, oleic acid and octadecene are mixed and react to obtain a cadmium oleate solution;
(2) adding oleylamine, octadecene and sulfur powder into the cadmium oleate solution obtained in the step (1) to obtain a cadmium oleate-sulfur powder solution;
(3) dropwise adding the cadmium oleate-sulfur powder mixed solution obtained in the step (2) into CsPbX3And in the solution, centrifuging after the reaction is finished to obtain the CdS coated inorganic perovskite nano material, wherein X is Cl, Br or I.
Further, the mass-volume ratio (mg: ml: ml) of the cadmium oxide, the oleic acid and the octadecene in the step (1) is 100: 1: 1.
further, the reaction conditions in the step (1) are heating to 210-280 ℃ for reaction for 1 hour, and then cooling to 110-150 ℃ for reaction for 30 minutes.
Further, the volume ratio of the cadmium oleate solution, the oleylamine and the octadecene in the step (2) is 1: 0.4: 4, the volume-mass (ml: mg) ratio of the cadmium oleate solution to the sulfur powder is 1: 9.6 to 16.
Further, the CsPbX in the step (3)3The volume ratio of the solution to the cadmium oleate-sulfur powder mixed solution is 1.2: 1, the CsPbX3CsPbX in solution3The amount of material was 0.027mmol, with X being Cl, Br or I.
Further, the CsPbX in the step (3)3The preparation method of the solution comprises the following steps:
a) cesium carbonate, octadecene and oleic acid were added in mass volumes (mg: ml: ml) ratio of 100: 3.5-4.5: 0.5-0.7, stirring for 1 hour at 120 ℃, and marking as A solution;
b) mixing lead halide and octadecene, stirring at 120 deg.C for 1 hr, heating to 150 deg.C, sequentially injecting oleic acid and oleylamine, stirring for 3 min, and injecting the solution A in step a) to obtain CsPbX3A solution; the lead halide is lead chloride, lead bromide or lead iodide; and X is Cl, Br or I.
Further, the molar concentration of the lead halide in the step b) is 0.036-0.04 mmol/ml, and the molar volumes of the lead halide, the oleic acid and the oleylamine (mmol: ml: ml) ratio of 0.18-0.2: 0.5: 0.5.
further, step b) the molar volume of the lead halide and a solution (mmol: ml) is 0.45-0.5: 1.
2. the CdS-coated inorganic perovskite nano material prepared by the preparation method.
And 3, applying the CdS-coated inorganic perovskite nano material to the preparation of a light-emitting diode, a solar cell or a photoelectric detector.
The invention has the beneficial effects that: 1. core-shell structure CsPbX3The @ CdS nano material has high stability, and fluorescence is not quenched when the material is contacted with water. 2. Core-shell structure CsPbX3The @ CdS nano material has non-flicker property, the fluorescence intensity track can not be greatly changed, and the @ CdS nano material is particularly important in the application of a light-emitting diode. 3. Synthesis of core-shell structure CsPbX3The @ CdS nano material has good dispersibility and uniform size and is square about 25 nm.
Drawings
In order to make the object, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings for explanation:
FIG. 1 shows inorganic perovskite CsPbBr with core-shell structure3A preparation scheme of @ CdS;
FIG. 2 shows inorganic perovskite CsPbBr with core-shell structure3XRD pattern of @ CdS;
FIG. 3 shows inorganic perovskite CsPbBr with core-shell structure3@ CdS TEM photograph;
FIG. 4 shows inorganic perovskite CsPbBr with core-shell structure3@ CdS TEM photograph;
FIG. 5 shows inorganic perovskite CsPbBr with core-shell structure3@ CdS high-resolution transmission electron microscope photograph;
FIG. 6 shows inorganic perovskite CsPbBr with core-shell structure3@ CdS high-resolution transmission electron microscope photograph;
FIG. 7 shows inorganic perovskite CsPbBr with core-shell structure3Line scan of @ CdS;
FIG. 8 shows inorganic perovskite CsPbBr with core-shell structure3Mapping plot of @ CdS;
FIG. 9 shows the inorganic perovskite CsPbBr of the left bottle core-shell structure3@ CdS and right bottle of common inorganic perovskite CsPbBr3Photographs of water stability dispersed in toluene, respectively;
FIG. 10 shows CsPbBr in core-shell structure3@ CdS and common cubic CsPbBr3Fluorescent trace plot.
FIG. 11 is a core-shell junctionStructure inorganic perovskite CsPbBr3A statistical plot of the particle size of @ CdS;
wherein the bottles on the left in FIGS. 9a, b, c, d are all provided with an upper CsPbBr layer3@ CdS, lower layer water; the right bottle is filled with an upper CsPbBr layer3The lower layer of water is a photo of two bottles after water is respectively added into the two bottles; b is a fluorescent photograph under an ultraviolet lamp after water is respectively added into the two bottles; c is a photograph of two bottles after shaking simultaneously for one minute; d is a fluorescent photograph under an ultraviolet lamp after two bottles were shaken simultaneously for one minute;
in FIG. 10, a is CsPbBr with core-shell structure3Fluorescence trace plot of @ CdS; b is a common cubic structure CsPbBr3A fluorescent trace plot; c is core-shell structure CsPbBr3Screenshots of fluorescence tracks of @ CdS at 20 seconds, 40 seconds and 60 seconds; d is a common cubic structure CsPbBr3Video screenshots of the fluorescence trace at 20 seconds, 40 seconds, 60 seconds.
Detailed Description
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1 preparation of CdS-coated inorganic perovskite nanomaterial
(1) Under the environment of mechanical stirring and continuous nitrogen, 383mg of cadmium oxide, 3.8ml of oleic acid and 3.8ml of octadecene are mixed, heated to 240 ℃, mixed and stirred for 1 hour, and then cooled to 110 ℃, mixed and stirred for 30 minutes to obtain a cadmium oleate solution;
(2) adding 12.8mg of sulfur powder, 0.4ml of oleylamine and 4ml of octadecene into 1ml of cadmium oleate solution to obtain a cadmium oleate-sulfur powder mixed solution;
(3) 100mg of cesium carbonate was mixed with 4ml of octadecene and 0.6ml of oleic acid, and stirred at 120 ℃ for 1 hour;
(4)69mg of lead bromide is mixed with 5ml of octadecylene, the mixture is stirred for 1 hour at the temperature of 120 ℃, then 0.5ml of oleic acid and 0.5ml of oleylamine are injected in sequence when the temperature is raised to 150 ℃, and after the mixture is stirred for 3 minutes, 0.4ml of cesium carbonate, the mixture of octadecylene and oleic acid is injected to obtain CsPbBr3A solution;
(5) when CsPbBr is used in the step (4)3After the solution has reacted for 5 seconds, it is thenDropwise adding the cadmium oleate-sulfur powder mixed solution obtained in the step (2) within 20 minutes;
(6) centrifuging and purifying the reaction liquid obtained in the step (5) at 8000 rpm to finally obtain the CdS-coated inorganic perovskite nano material, which is also called inorganic perovskite CsPbBr with a core-shell structure in the embodiment3@CdS。
FIG. 1 shows inorganic perovskite CsPbBr with core-shell structure3A preparation scheme of @ CdS; FIG. 2 shows that the inorganic perovskite CsPbBr with the core-shell structure prepared in this example is3XRD pattern of @ CdS; FIG. 3 shows that the inorganic perovskite CsPbBr with the core-shell structure prepared by the present example is3@ CdS TEM photograph; FIG. 4 shows the preparation of inorganic perovskite CsPbBr with core-shell structure in this example3@ CdS TEM photograph; FIG. 5 shows that the inorganic perovskite CsPbBr with the core-shell structure prepared in this example is3@ CdS high-resolution transmission electron microscope photograph; FIG. 6 shows that the inorganic perovskite CsPbBr with the core-shell structure prepared in this example is3@ CdS high-resolution transmission electron microscope photograph; FIG. 7 shows that the inorganic perovskite CsPbBr with the core-shell structure prepared in this example is3Line Scan element analysis graph of @ CdS on one Line; FIG. 8 shows that the inorganic perovskite CsPbBr with the core-shell structure prepared in this example is3Mapping element analysis diagram of the whole face of @ CdS, and the distribution of each element in quantum dots can be seen in both FIG. 7 and FIG. 8; FIG. 9 shows the inorganic perovskite CsPbBr of the left bottle core-shell structure3@ CdS and right bottle of common inorganic perovskite CsPbBr3Photographs of water stability dispersed in toluene, respectively; in the left-hand bottle in FIGS. 9a, b, c, d, there is an upper CsPbBr layer3@ CdS, lower layer water; the right bottle is filled with an upper CsPbBr layer3The lower layer of water is a photo of two bottles after water is respectively added into the two bottles; b is a fluorescent photograph under an ultraviolet lamp after water is respectively added into the two bottles; c is a photograph of two bottles after shaking simultaneously for one minute; d is a fluorescent photograph under an ultraviolet lamp after two bottles were shaken simultaneously for one minute; as can be seen in FIG. 9, the right vial of the common cubic CsPbBr was shaken for about 1 minute simultaneously3Fluorescence quenching of the nanomaterial, and left bottle core-shell structure CsPbBr3The fluorescence of the nanomaterial is not affected. As can be seen from FIG. 10, CsPbBr in core-shell structure3Compared with the fluorescence trace graph of the nano material with the common cubic structure CsPbBr3The nano material is obviously stable, and the core-shell structure CsPbBr is shown3Nano material ratio of common CsPbBr3The flicker is well suppressed. FIG. 11 shows inorganic perovskite CsPbBr with core-shell structure3@ CdS particle size statistical plot.
The experiments prove that the inorganic perovskite (CsPbX) with the core-shell structure prepared by the technical scheme3@ CdS, X ═ Cl, Br, I) have high stability, fluorescence is not quenched when contacting water, and also have non-blinking properties, and fluorescence intensity traces do not change greatly.
Example 2 preparation of CdS-coated inorganic perovskite nanomaterial
(1) Under the environment of mechanical stirring and continuous nitrogen, 383mg of cadmium oxide, 3.8ml of oleic acid and 3.8ml of octadecene are mixed, heated to 210 ℃, mixed and stirred for 1 hour, cooled to 110 ℃, mixed and stirred for 30 minutes, and a cadmium oleate solution is obtained;
(2) adding 16mg of sulfur powder, 0.4ml of oleylamine and 4ml of octadecene into 1ml of cadmium oleate solution to obtain a cadmium oleate-sulfur powder mixed solution;
(3) 105mg of cesium carbonate was mixed with 4.5ml of octadecene and 0.7ml of oleic acid, and stirred at 120 ℃ for 1 hour;
(4)73.4mg of lead bromide is mixed with 5ml of octadecene, the mixture is stirred for 1 hour at 120 ℃, then 0.5ml of oleic acid and 0.5ml of oleylamine are injected in sequence when the temperature is raised to 150 ℃, and after the mixture is stirred for 3 minutes, 0.4ml of cesium carbonate, the mixture of octadecene and oleic acid is injected to obtain CsPbBr3A solution;
(5) when CsPbBr is used in the step (4)3After the solution reacts for 5 seconds, dropwise adding the cadmium oleate-sulfur powder mixed solution obtained in the step (2) within the next 20 minutes;
(6) centrifuging and purifying the reaction liquid obtained in the step (5) at 8000 rpm to finally obtain the CdS-coated inorganic perovskite nano material, which is also called inorganic perovskite CsPbBr with a core-shell structure in the embodiment3@CdS。
Example 3 preparation of CdS-coated inorganic perovskite nanomaterial
(1) Under the environment of mechanical stirring and continuous nitrogen, 383mg of cadmium oxide, 3.8ml of oleic acid and 3.8ml of octadecene are mixed, heated to 260 ℃, mixed and stirred for 1 hour, cooled to 110 ℃, mixed and stirred for 30 minutes, and a cadmium oleate solution is obtained;
(2) adding 9.6mg of sulfur powder, 0.4ml of oleylamine and 4ml of octadecene into 1ml of cadmium oleate solution to obtain a cadmium oleate-sulfur powder mixed solution;
(3) 100mg of cesium carbonate was mixed with 3.7ml of octadecene and 0.5ml of oleic acid, and stirred at 120 ℃ for 1 hour;
(4)71mg of lead bromide is mixed with 5ml of octadecene, the mixture is stirred for 1 hour at the temperature of 120 ℃, then 0.5ml of oleic acid and 0.5ml of oleylamine are injected in sequence when the temperature is raised to 150 ℃, after the mixture is stirred for 3 minutes, 0.4ml of cesium carbonate, the mixture of octadecene and oleic acid is injected to obtain CsPbBr3A solution;
(5) when CsPbBr is used in the step (4)3After the solution reacts for 5 seconds, dropwise adding the cadmium oleate-sulfur powder mixed solution obtained in the step (2) within the next 20 minutes;
(6) centrifuging and purifying the reaction liquid obtained in the step (5) at 8000 rpm to finally obtain the CdS-coated inorganic perovskite nano material, which is also called inorganic perovskite CsPbBr with a core-shell structure in the embodiment3@CdS。
Example 4 preparation of CdS-coated inorganic perovskite nanomaterial
(1) Under the environment of mechanical stirring and continuous nitrogen, 383mg of cadmium oxide, 3.8ml of oleic acid and 3.8ml of octadecene are mixed, heated to 240 ℃, mixed and stirred for 1 hour, and then cooled to 120 ℃, mixed and stirred for 30 minutes to obtain a cadmium oleate solution;
(2) adding 12.8mg of sulfur powder, 0.4ml of oleylamine and 4ml of octadecene into 1ml of cadmium oleate solution to obtain a cadmium oleate-sulfur powder mixed solution;
(3) 100mg of cesium carbonate was mixed with 4ml of octadecene and 0.6ml of oleic acid, and stirred at 120 ℃ for 1 hour;
(4) mixing 52mg lead chloride with 5ml octadecene, stirring at 120 deg.C for 1 hr, raising temperature to 150 deg.C, sequentially injecting 0.5ml oleic acid and 0.5ml oleylamine, stirring for 3 min, and injecting 0.4ml cesium carbonate, octadecene andoleic acid mixture to obtain CsPbCl3A solution;
(5) when CsPbCl is used in the step (4)3After the solution reacts for 5 seconds, dropwise adding the cadmium oleate-sulfur powder mixed solution obtained in the step (2) within the next 20 minutes;
(6) centrifuging and purifying the reaction liquid obtained in the step (5) at 8000 rpm to finally obtain the CdS-coated inorganic perovskite nano material, which is also called inorganic perovskite CsPbCl with a core-shell structure in the embodiment3@CdS。
Example 5 preparation of CdS-coated inorganic perovskite nanomaterials
(1) Under the environment of mechanical stirring and continuous nitrogen, 383mg of cadmium oxide, 3.8ml of oleic acid and 3.8ml of octadecene are mixed, heated to 220 ℃, mixed and stirred for 1 hour, cooled to 120 ℃, mixed and stirred for 30 minutes, and a cadmium oleate solution is obtained;
(2) adding 12.8mg of sulfur powder, 0.4ml of oleylamine and 4ml of octadecene into 1ml of cadmium oleate solution to obtain a cadmium oleate-sulfur powder mixed solution;
(3) 100mg of cesium carbonate was mixed with 4ml of octadecene and 0.6ml of oleic acid, and stirred at 120 ℃ for 1 hour;
(4) mixing 87mg lead iodide with 5ml octadecene, stirring at 120 deg.C for 1 hr, heating to 150 deg.C, sequentially adding 0.5ml oleic acid and 0.5ml oleylamine, stirring for 3 min, and adding 0.4ml cesium carbonate, octadecene and oleic acid to obtain CsPbCl3A solution;
(5) when CsPbCl is used in the step (4)3After the solution reacts for 5 seconds, dropwise adding the cadmium oleate-sulfur powder mixed solution obtained in the step (2) within the next 20 minutes;
(6) centrifuging and purifying the reaction liquid obtained in the step (5) at 8000 rpm to finally obtain the CdS-coated inorganic perovskite nano material, which is also called inorganic perovskite CsPbI with a core-shell structure in the embodiment3@CdS。
Example 6 preparation of CdS-coated inorganic perovskite nanomaterials
(1) Under the environment of mechanical stirring and continuous nitrogen, 383mg of cadmium oxide, 3.8ml of oleic acid and 3.8ml of octadecene are mixed, heated to 280 ℃, mixed and stirred for 1 hour, and then cooled to 150 ℃, mixed and stirred for 30 minutes to obtain a cadmium oleate solution;
(2) adding 11.2mg of sulfur powder, 0.4ml of oleylamine and 4ml of octadecene into 1ml of cadmium oleate solution to obtain a cadmium oleate-sulfur powder mixed solution;
(3) 100mg of cesium carbonate was mixed with 4.2ml of octadecene and 0.6ml of oleic acid, and stirred at 120 ℃ for 1 hour;
(4) mixing 92mg lead iodide with 5ml octadecene, stirring at 120 deg.C for 1 hr, heating to 150 deg.C, sequentially injecting 0.5ml oleic acid and 0.5ml oleylamine, stirring for 3 min, and injecting 0.4ml cesium carbonate, octadecene and oleic acid mixture to obtain CsPbBr3A solution;
(5) when CsPbBr is used in the step (4)3After the solution reacts for 5 seconds, dropwise adding the cadmium oleate-sulfur powder mixed solution obtained in the step (2) within the next 20 minutes;
(6) centrifuging and purifying the reaction liquid obtained in the step (5) at 8000 rpm to finally obtain the CdS-coated inorganic perovskite nano material, which is also called inorganic perovskite CsPbBr with a core-shell structure in the embodiment3@CdS。
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.

Claims (10)

1. A preparation method of a CdS-coated inorganic perovskite nano material is characterized by comprising the following steps:
(1) under the environment of continuous nitrogen, cadmium oxide, oleic acid and octadecene are mixed and react to obtain a cadmium oleate solution;
(2) adding oleylamine, octadecene and sulfur powder into the cadmium oleate solution obtained in the step (1) to obtain a cadmium oleate-sulfur powder solution;
(3) dropwise adding the cadmium oleate-sulfur powder mixed solution obtained in the step (2) into CsPbX3In solution, reactionAnd centrifuging after finishing, thus obtaining the CdS coated inorganic perovskite nano material, wherein X is Cl, Br or I.
2. The preparation method of claim 1, wherein the mass-to-volume ratio of the cadmium oxide, the oleic acid and the octadecene in the step (1) is 100: 1: 1, mg: ml: and (3) ml.
3. The preparation method of claim 1, wherein the reaction conditions in step (1) are heating to 210 ~ 280 ℃ for 1 hour, and cooling to 110 ~ 150 ℃ for 30 minutes.
4. The preparation method of claim 1, wherein the volume ratio of the cadmium oleate solution to the oleylamine to the octadecene in the step (2) is 1: 0.4: 4, and the volume mass ratio of the cadmium oleate solution to the sulfur powder is 1: 9.6 ~ 16, ml: mg.
5. The method according to claim 1, wherein the CsPbX of step (3) is used as a carrier of the CsPbX3The volume ratio of the solution to the cadmium oleate-sulfur powder mixed solution is 1.2: 1, the CsPbX3CsPbX in solution3The amount of material was 0.027mmol, with X being Cl, Br or I.
6. The method according to claim 1, wherein the CsPbX of step (3) is used as a carrier of the CsPbX3The preparation method of the solution comprises the following steps:
a) cesium carbonate, octadecene and oleic acid are mixed according to the mass volume ratio of 100: 3.5 ~ 4.5.5: 0.5 ~ 0.7.7, mg: ml: ml, and stirred at 120 ℃ for 1 hour, and the mixture is marked as A solution;
b) mixing lead halide and octadecene, stirring at 120 deg.C for 1 hr, heating to 150 deg.C, sequentially injecting oleic acid and oleylamine, stirring for 3 min, and injecting the solution A in step a) to obtain CsPbX3A solution; the lead halide is lead chloride, lead bromide or lead iodide; and X is Cl, Br or I.
7. The preparation method of claim 6, wherein the molar concentration of the lead halide in the step b) is 0.036 ~ 0.04.04 mmol/ml, and the molar volume ratio of the lead halide, the oleic acid and the oleylamine is 0.18 ~ 0.2.2: 0.5: 0.5, mmol: ml: ml.
8. The method according to claim 6, wherein the molar volume of the lead halide and the A solution in the step b) is 0.45 ~ 0.5.5: 1, mmol: ml.
9. The CdS-coated inorganic perovskite nano-material prepared by the preparation method of any one of claims 1 ~ 8.
10. Use of the CdS coated inorganic perovskite nanomaterial as claimed in claim 9 in the manufacture of a light emitting diode, a solar cell, or a photodetector.
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