CN111792665B - Method for high-pressure solid-phase synthesis of copper-cesium-iodide lead-free quantum dots - Google Patents

Method for high-pressure solid-phase synthesis of copper-cesium-iodide lead-free quantum dots Download PDF

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CN111792665B
CN111792665B CN202010691061.2A CN202010691061A CN111792665B CN 111792665 B CN111792665 B CN 111792665B CN 202010691061 A CN202010691061 A CN 202010691061A CN 111792665 B CN111792665 B CN 111792665B
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CN111792665A (en
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孙立忠
陈浩
徐昌富
申星
刘�英
黎佳昕
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Abstract

The invention discloses a method for high-pressure solid-phase synthesis of copper-cesium iodide lead-free quantum dots, which comprises the steps of uniformly mixing CsI and CuI according to a molar ratio of 3:2, tabletting, and processing under a high pressure of not less than 1GPa to obtain a copper-cesium iodide quantum dot nano material. The invention takes copper iodide and cesium iodide as precursors, adopts high-pressure solid-phase synthesis, has simple and controllable process, does not need inert atmosphere protection in the preparation process, and obtains the copper iodide and cesium iodide quantum dot with high photoluminescence intensity.

Description

Method for high-pressure solid-phase synthesis of copper-cesium-iodide lead-free quantum dots
Technical Field
The invention relates to the technical field of nano materials, in particular to a method for synthesizing lead-free perovskite copper-iodine-cesium quantum dots through a high-pressure solid phase.
Background
Quantum dots, also known as semiconductor nanocrystals. Generally refers to nanoparticles having a radius less than or close to the exciton bohr radius. Because quantum of the quantum dots in the three-dimensional direction is limited, the quantum dots belong to zero-dimensional nano materials, and the size of the quantum dots is about ten nanometers generally. In comparison with other materials, quantum dots have a quantum confinement effect, and as the size of the quantum dots is reduced, a continuous energy level structure will be transformed into a discrete discontinuous energy level structure. After being excited by light with certain wavelength energy, photons in the valence band absorbing certain energy are excited into the conduction band, and electrons in the excited state jump from the conduction band to the valence band, and release energy in the form of light, so that a remarkable fluorescence phenomenon is emitted.
Under the support of nanotechnology, a brand-new nano material, namely, all-inorganic perovskite quantum dot is gradually discovered, wherein the lead-based perovskite quantum dot is taken as a prominent representative. The appearance of all-inorganic perovskite quantum dots is widely concerned and researched due to the advantages of high fluorescence yield, long fluorescence life, adjustable emission peak, high stability after modification and the like. For the representative lead-based perovskite quantum dots, lead is an important factor for further development of the photoelectric industry. Research and development on inorganic lead-halogen perovskite quantum dots are gradually perfected, but a fatal problem is that the toxicity of lead ions hinders the large-scale use of the perovskite quantum dots. For example, chinese patent CN106590644A synthesizes lead-cesium bromide quantum dots containing lead ions, which is a lead-halogen perovskite quantum dot, and its toxicity limits its wide use. It is therefore important to find other ions instead of lead ions.
The currently used lead ion substitutes are ions such as Sn, Bi and Sb, but the currently used synthesis methods for substituting these ions for lead ions are all solution methods, for example, chinese patent CN201910045416.8 synthesizes copper-doped quantum dots by solution methods, but the preparation process is extremely complicated and needs to be accurately controlled, and nitrogen gas needs to be introduced to prevent the copper ions from being oxidized to prevent the required sample from being obtained.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for synthesizing copper-cesium-iodide lead-free quantum dots by a high-pressure solid phase method.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a method for synthesizing iodine copper cesium lead-free quantum dots through high-pressure solid phase synthesis comprises the steps of uniformly mixing CsI and CuI according to a molar ratio of 3:2, tabletting, and processing under high pressure of not less than 1GPa to obtain the iodine copper cesium quantum dot nano material.
Furthermore, the pressure of the tabletting is 15-20 MPa, and the time is 5-10 min.
Further, the high pressure is 1-5 GPa.
Further, the high pressure is 3 GPa.
Further, the temperature of the high-pressure treatment is 150-350 ℃.
Further, the temperature of the high pressure treatment is 250 ℃.
Furthermore, the time of the high-pressure treatment is 2-6 h.
The invention obtains the nanometer material by applying high pressure to the sample after tabletting treatment, the nanometer particles have small size and high surface energy, and the atoms on the surface account for a considerable proportion. The surface atoms of the substance are in a state of interaction only with the internal atoms, which are always kept in equilibrium due to the attraction or repulsion of the surrounding atoms. This means for luminescent materials that the surface atoms are in a relatively higher energy state than the internal atoms, making the atoms more reactive and thus exhibiting higher photoluminescence intensity. Meanwhile, because the sample is in a compact environment under high pressure and no air enters, the preparation process of the invention does not need inert atmosphere protection.
The invention has the advantages that:
1. the invention adopts high-pressure solid-phase synthesis, only uses CsI and CuI as synthesis raw materials, has simple and controllable preparation process, does not need inert atmosphere protection in the preparation process, and can be controllably synthesized in the air.
2. The crystal grain size of the copper-cesium iodide quantum dot prepared by the method is small, and the photoluminescence intensity is high.
3. The invention only uses CsI-CuI as a synthetic raw material, and compared with the lead-halogen perovskite quantum dot, the obtained copper-iodine-cesium quantum dot material has no toxicity and can be widely used.
4. The invention replaces Pb ions with Cu ions, and has cheaper economic benefit compared with Sn, Bi, Sb, Ag and other ions.
Drawings
FIG. 1 is a graph showing the fluorescence excitation spectrum at 450nm of a sample obtained in example 2;
FIG. 2 is a 310nm fluorescence emission spectrum of the samples obtained in comparative examples 1 to 2 and examples 1 to 3;
FIG. 3 is an X-ray diffraction pattern of a sample obtained in comparative example 1-2;
FIG. 4 is an X-ray diffraction pattern of samples prepared in examples 1-3;
FIG. 5 is an X-ray diffraction chart of the samples obtained in comparative examples 1-2 and examples 1-3.
Detailed Description
The present invention will be further described with reference to specific embodiments.
Example 1
CsI 60mol％；
CuI 40mol％；
The method for preparing the sample by adopting the high-pressure solid-phase reaction method comprises the following steps:
(1) Respectively weighing required raw materials according to a molar ratio;
(2) grinding the raw materials in an agate mortar respectively, uniformly mixing, putting into a tablet machine die, and keeping the pressure at 20MPa for 10min to completely tablet the powder mixture;
(3) putting the prepared sample into a graphite tube, putting a graphite block and a boron nitride block into the graphite tube to enable planes of two ends to be parallel, sleeving the boron nitride tube outside the graphite tube, putting molybdenum sheets at two ends, putting electrodes at the same time to enable planes of the two ends to be parallel, and putting the boron nitride tube into a die required by a cubic press to enable two faces of a die with electrodes to be kept on the same horizontal plane;
(4) and (3) putting the prepared die sample into a cubic press, and preserving heat and pressure for 2 hours at the temperature of 150 ℃ under the condition of 3GPa to obtain the copper-cesium-iodide quantum dots, wherein the crystal grain parameters are shown in Table 1.
Example 2
CsI 60mol％；
CuI 40mol％；
The method for preparing the sample by adopting the high-pressure solid-phase reaction method comprises the following steps:
(1) weighing required raw materials respectively according to a molar ratio;
(2) grinding the raw materials in an agate mortar respectively, uniformly mixing, putting into a die of a tablet machine, and keeping the pressure for 10min at 20MPa to completely tablet the powder mixture;
(3) putting the prepared sample into a graphite tube, putting a graphite block and a boron nitride block into the graphite tube to enable planes of two ends to be parallel, sleeving the boron nitride tube outside the graphite tube, putting molybdenum sheets at two ends, putting electrodes at the same time to enable planes of the two ends to be parallel, and putting the boron nitride tube into a die required by a cubic press to enable two faces of a die with electrodes to be kept on the same horizontal plane;
(4) And (3) putting the prepared die sample into a cubic press, and preserving heat and pressure for 2 hours at the conditions of 3GPa and 250 ℃ to obtain the copper-cesium-iodide quantum dot, wherein the crystal grain parameters are shown in Table 1.
Example 3
CsI 60mol％；
CuI 40mol％；
The method for preparing the sample by adopting the high-pressure solid-phase reaction method comprises the following steps:
(1) respectively weighing required raw materials according to a molar ratio;
(2) grinding the raw materials in an agate mortar respectively, uniformly mixing, putting into a die of a tablet machine, and keeping the pressure for 10min at 20MPa to completely tablet the powder mixture;
(3) putting the prepared sample into a graphite tube, putting a graphite block and a boron nitride block into the graphite tube to enable planes of two ends to be parallel, sleeving the boron nitride tube outside the graphite tube, putting molybdenum sheets at two ends, putting electrodes at the same time to enable planes of the two ends to be parallel, and putting the boron nitride tube into a die required by a cubic press to enable two faces of a die with electrodes to be kept on the same horizontal plane;
(4) and (3) putting the prepared die sample into a cubic press, and carrying out heat preservation and pressure maintaining for 2 hours under the conditions of 3GPa and 350 ℃ to obtain the copper-cesium-iodide quantum dot, wherein the crystal grain parameters are shown in Table 1.
Comparative example 1
CsI 60mol％；
CuI 40mol％；
The method for preparing the sample by adopting the solution method comprises the following steps:
(1) weighing required raw materials respectively according to a molar ratio;
(2) Adding weighed CsI and CuI into 2ml N, N-dimethylformamide, introducing nitrogen at 70 ℃, and stirring for 5min on a magnetic stirrer to obtain a precursor solution;
(3) then injecting the precursor solution into toluene, introducing nitrogen, and stirring and reacting for 3min at the speed of 9000 rpm;
(4) then, nitrogen is introduced into the centrifuge, the mixture is centrifuged for 6min at the speed of 9000rpm, precipitates are taken out, and the precipitates are washed by toluene for four times to obtain copper-cesium iodide nanocrystals, wherein the crystal grain parameters are shown in table 1.
Comparative example 2
CsI 60mol％；
CuI 40mol％；
The method for preparing the sample by adopting the normal-pressure solid-phase reaction method specifically comprises the following steps:
(1) weighing required raw materials respectively according to a molar ratio;
(2) grinding the raw materials in an agate mortar respectively, uniformly mixing, putting into a die of a tablet machine, and keeping the pressure for 10min at 20MPa to completely tablet the powder mixture;
(3) then the prepared sample is put into a corundum crucible and is put into a tube furnace, then the temperature is kept for 2h at 350 ℃ under the protection of atmosphere, and then the sample is cooled to room temperature along with the tube furnace to prepare the sample, wherein the crystal grain parameters are shown in table 1.
TABLE 1 tables of grain parameters for samples prepared in comparative examples 1-2 and examples 1-3
Figure BDA0002589383510000051
As can be seen from table 1, the samples of the present invention produced by high pressure (examples 1-3) have much smaller grain sizes than those of the samples produced by comparative examples 1-2, because the smaller the interatomic distance is at high pressure, the more difficult the grain growth is, and the pressure can effectively change the interatomic distance and thus the structure of the substance.
Performance and spectrum testing: the samples prepared in comparative examples 1-2 and examples 1-3 were subjected to fluorescence excitation emission spectroscopy and X-ray diffraction analysis, respectively.
As shown in FIG. 1, for the excitation spectrum of the sample, it is known that the central wavelength of the emission of the cesium iodocopper quantum dot is 450nm, and the sample is excited by using the excitation light of 200-400nm, and it is determined that the light emitting the strongest light at 450nm can be obtained by exciting the sample by using the excitation light of 310 nm.
As shown in fig. 2, for the emission spectrum of the sample, the sample was de-excited at the central wavelength of excitation light of 310nm measured by the excitation spectrum, the central wavelength of emission light of the sample was measured at 452nm in the range of 350-650nm, and it can be seen from the emission spectrum that the emission intensity of example 2 is the highest and the emission intensity of comparative example 2 is the lowest, because the grain size of the quantum dot nanomaterial synthesized by high pressure is much smaller than that of the sample synthesized by the synthesis and solution method under normal pressure, and because the grain size is too small, the quantum confinement effect and the surface effect are caused, the exciton luminescence caused by the quantum confinement effect and the activity of atoms caused by the surface effect are higher, and thus the small-sized copper-cesium iodide quantum dot material has higher photoluminescence intensity.
As shown in FIG. 3, which is an X-ray diffraction pattern of the sample prepared in comparative example 1-2, it can be seen from XRD that the phase synthesized in comparative example 1-2 is Cs 3(Cu2I5) The reason why this is possible is because the properties of the material are closely related to the size and dimensions of the material. The low-pressure phase structure of the crystal grains is Cs due to the enlargement of the size of the crystal grains3(Cu2I5) Such that it changes from a 0-dimensional quantum dot structure to a 1-dimensional nanowire structure.
As shown in FIG. 4, which is an X-ray diffraction pattern of the samples obtained in examples 1 to 3, it can be seen that Cs was successfully synthesized by the high pressure method3Cu2I5A quantum dot structure.
As shown in FIG. 5, in the X-ray diffraction patterns of the samples obtained in comparative examples 1-2 and examples 1-3, it can be seen that the diffraction peaks of comparative examples 1-2 and examples 1-3 are significantly different because the phase structure of examples 1-3 is Cs3Cu2I5While comparative examples 1-2 had a phase structure of Cs3(Cu2I5) The reason for this is because as the nanomaterial grows in size, it grows from quantum dots to nanowires.

Claims (4)

1. A method for synthesizing iodine copper cesium leadless quantum dots by high-pressure solid phase is characterized by comprising the following steps: uniformly mixing CsI and CuI according to the molar ratio of 3:2, tabletting, and then processing under the high pressure of 1-5 GPa to obtain the copper-cesium-iodide quantum-dot nano material; the temperature of the high-pressure treatment is 150-350 ℃; the high-pressure treatment time is 2-6 h.
2. The method for high-pressure solid-phase synthesis of the copper-cesium-iodide lead-free quantum dot according to claim 1, wherein the method comprises the following steps: the pressure of the tabletting is 15-20 MPa, and the time is 5-10 min.
3. The method for high-pressure solid-phase synthesis of the copper-cesium-iodide lead-free quantum dot according to claim 1, wherein the method comprises the following steps: the high pressure is 3 GPa.
4. The method for high-pressure solid-phase synthesis of the copper-cesium-iodide lead-free quantum dot according to claim 1, wherein the method comprises the following steps: the temperature of the high pressure treatment was 250 ℃.
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