CN115403065B - Preparation method of cesium copper halide crystal - Google Patents
Preparation method of cesium copper halide crystal Download PDFInfo
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- CN115403065B CN115403065B CN202211044612.1A CN202211044612A CN115403065B CN 115403065 B CN115403065 B CN 115403065B CN 202211044612 A CN202211044612 A CN 202211044612A CN 115403065 B CN115403065 B CN 115403065B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/006—Compounds containing, besides copper, two or more other elements, with the exception of oxygen or hydrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/02—Crystallisation from solutions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Abstract
The embodiment of the application provides a preparation method of cesium copper halide crystals, which comprises the following steps: providing a compound with chemical formulas of CsX and CuX, and uniformly mixing to obtain a reactant, wherein X is at least one of Cl, br and I; placing the reactant under a preset vacuum degree and heating to a preset temperature, and simultaneously enabling the reactant to perform internal movement for a preset time to obtain a melt; cooling the melt at a predetermined cooling rate to obtain the cesium copper halide crystals. The preparation method of the cesium copper halide crystal provided by the embodiment of the application has the advantages that the whole preparation process is very simple, and the obtained product has very high purity.
Description
Technical Field
The application relates to the field of luminescence and irradiation detection, in particular to a preparation method of cesium copper halide crystals.
Background
The cesium copper halide (Cs-Cu-X) material used as a metal halide material has the advantages of multiple light-emitting wave bands, good light-emitting performance, high fluorescence quantum yield and the like in the field of light-emitting and irradiation detection. At present, the synthesis method of cesium copper halide materials is not perfect, and powder materials are generally prepared by a solution method or single crystal materials are prepared by a Bridgman method. The two methods have the defects of lower purity, complex process and long time consumption, and further application research of cesium copper halogen materials is severely limited.
Disclosure of Invention
The embodiment of the application provides a preparation method of cesium copper halide crystals, which aims to solve the technical problems of lower purity and complex process of the existing method.
The embodiment of the application provides a preparation method of cesium copper halide crystals, which comprises the following steps:
providing a compound with chemical formulas of CsX and CuX, and uniformly mixing to obtain a reactant, wherein X is at least one of Cl, br and I;
placing the reactant under a preset vacuum degree and heating to a preset temperature, and simultaneously enabling the reactant to perform internal movement for a preset time to obtain a melt;
cooling the melt at a predetermined cooling rate to obtain the cesium copper halide crystals.
In some embodiments of the application, the step of placing the reactant under a predetermined vacuum and heating to a predetermined temperature comprises the steps of:
placing the reactant under the predetermined vacuum;
and heating reactants in a segmented way under a preset vacuum degree until the preset temperature is reached.
In some embodiments of the application, X is I, and the molar ratio of CsX to CuX is 3:2.
in some embodiments of the application, the staged heating includes the steps of:
heating the reactant to 200 ℃, and preserving heat for at least 10min;
heating the reactant at 200 ℃ to 300 ℃ and preserving heat for at least 10min;
heating the reactant at 300 ℃ to 350 ℃ and preserving heat for at least 10min;
the reactants were heated at 350 ℃.
In some embodiments of the application, X is a combination of two elements Cl, I, and the molar ratio of Cs, cu, cl, I atoms in the reactant is 5:3:6:2.
in some embodiments of the application, the staged heating includes the steps of:
heating the reactant to 200 ℃, and preserving heat for at least 10min;
heating the reactant at 200 ℃ to 300 ℃ and preserving heat for at least 10min;
heating the reactant at 300 ℃ to 400 ℃ and preserving heat for at least 10min;
the reactants were heated at 400 ℃.
In some embodiments of the application, the predetermined temperature is 380-420 ℃.
In some embodiments of the application, the predetermined vacuum is 0.8X10 -3 -1.2×10 -3 Pa。
In some embodiments of the application, the predetermined cooling rate is no higher than 15 ℃/h.
In some embodiments of the application, the predetermined time is not less than 6 hours.
Compared with the prior art, the technical scheme provided by the embodiment of the application has the following advantages:
according to the preparation method of the cesium copper halide crystal, provided by the embodiment of the application, the proper halide raw material is provided, the proportion of each element in the halide raw material is adjusted to be the same as that of the target crystal to be prepared, the halide raw material is heated to be molten to obtain the melt, the internal movement of the melt is continuously kept to uniformly mix the melt, and then the melt is cooled at a preset cooling rate to naturally crystallize the melt to form the target crystal, so that the whole preparation process is quite simple, and the obtained product has quite high purity.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the application and together with the description, serve to explain the principles of the application.
In order to more clearly illustrate the embodiments of the application or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, and it will be obvious to a person skilled in the art that other drawings can be obtained from these drawings without inventive effort.
FIG. 1 is a schematic flow chart of a method for preparing cesium copper halide crystals according to an embodiment of the present application;
FIG. 2 shows Cs obtained in example 1 of the present application 3 Cu 2 I 5 XRD test result patterns of the crystals;
FIG. 3 shows Cs obtained in example 2 of the present application 5 Cu 3 Cl 6 I 2 XRD test results pattern of crystals.
Detailed Description
The advantages and various effects of the present application will be more clearly apparent from the following detailed description and examples. It will be understood by those skilled in the art that these specific embodiments and examples are intended to illustrate the application, not to limit the application.
Throughout the specification, unless specifically indicated otherwise, the terms used herein should be understood as meaning as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. In case of conflict, the present specification will control.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present application are commercially available or may be prepared by existing methods.
At present, the synthesis method of cesium copper halide materials is not perfect, and powder materials are generally prepared by a solution method or single crystal materials are prepared by a Bridgman method. The two methods have the defects of poor material preparation performance, complex process and long time consumption, and further application research of cesium copper halogen materials is severely limited.
The technical scheme provided by the embodiment of the application aims to solve the technical problems, and the overall thought is as follows:
the embodiment of the application provides a preparation method of cesium copper halide crystals, which comprises the following steps:
s1: providing a compound with chemical formulas of CsX and CuX, and uniformly mixing to obtain a reactant, wherein X is at least one of Cl, br and I;
s2: placing the reactant under a preset vacuum degree and heating to a preset temperature, and simultaneously enabling the reactant to perform internal movement for a preset time to obtain a melt;
s3: cooling the melt at a predetermined cooling rate to obtain the cesium copper halide crystals.
It will be appreciated by those skilled in the art that the halogens in cesium copper halide materials generally do not include fluorine because the atomic radius of fluorine is too small and replacing other halogens with fluorine has a significant impact on the crystal structure.
Those skilled in the art will appreciate that CsX is at least one of CsCl, csBr, csI and CuX is at least one of CuCl, cuBr, cuI.
The ratios of CsX and CuX can be formulated by those skilled in the art according to the specific chemical formulas of cesium copper halide crystals to be prepared as is conventional in the art.
In the present application, the purpose of bringing the reactants to a predetermined vacuum is to bring them to a suitable pressure, capable of producing a solid-to-liquid phase transition at the corresponding temperature; meanwhile, the method has the effect of reducing oxygen and other elements in the environment where the reactant is located, so that cesium copper halide crystals obtained by the reaction are purer.
In the present application, the means of causing the reactants to undergo internal movement are: the substances inside the reactants move mutually, so that various substances inside the reactants are uniformly mixed. Such internal movement may be, for example, a vortex or swirl flow within the fluid, or migration of particles within the powder, or internal flow of a mixture of powder and fluid. Continuing the internal movement of the reactants includes, but is not limited to, agitating the reactants, shaking a container containing the reactants.
It will be appreciated by those skilled in the art that the mixing in step S1 may be performed in a conventional manner in the art, for example, stirring or grinding.
It will be appreciated by those skilled in the art that cooling the melt at a predetermined cooling rate, i.e., controlling the cooling rate, facilitates the formation of a regular crystal structure of atoms or ions within the melt.
In some embodiments of the application, in step S2, the step of placing the reactant under a predetermined vacuum and heating to a predetermined temperature includes the steps of:
s21: placing the reactant under the predetermined vacuum;
s22: and heating reactants in a segmented way under a preset vacuum degree until the preset temperature is reached.
As will be appreciated by those skilled in the art, staged heating refers to maintaining the temperature of the reactants after they have been heated to a certain temperature, and then continuing to heat until a predetermined temperature is reached. The purpose of the gradient heating is to allow the original powder to fully mix and react in the swinging process, so that the reaction is slow, and the raw powder is prevented from reacting too fast to form a mixed phase. And simultaneously, oxidation of raw materials is prevented when the reaction speed is too high.
In some embodiments of the application, X is I, and the molar ratio of CsX to CuX is 3:2.
as will be understood by those skilled in the art, the molar ratio refers to the ratio of the amounts of the substances.
Those skilled in the art will appreciate that CsI and CuI are described as 3:2, and Cs is the cesium copper halide crystal prepared by mixing the molar ratio of 2 3 Cu 2 I 5 。
In some embodiments of the application, the staged heating includes the steps of:
s2211: heating the reactant to 200 ℃, and preserving heat for at least 10min;
s2212: heating the reactant at 200 ℃ to 300 ℃ and preserving heat for at least 10min;
s2213: heating the reactant at 300 ℃ to 350 ℃ and preserving heat for at least 10min;
s2214: the reactants were heated at 350 ℃.
It will be appreciated by those skilled in the art that the purpose of the gradient heating is to allow the original powder to mix well during the rocking process so that the reaction proceeds slowly, preventing the raw powder from reacting too fast to form a heterogeneous phase. Meanwhile, the oxidation of raw materials can be prevented when the reaction speed is too high.
In some embodiments of the application, X is a combination of two elements Cl, I, and the molar ratio of Cs, cu, cl, I atoms in the reactant is 5:3:6:2.
those skilled in the art will appreciate the moles of Cs, cu, cl, I atoms in the reactantsThe molar ratio is 5:3:6:2, the prepared cesium copper halide crystal is Cs 5 Cu 3 Cl 6 I 2 。
In some embodiments of the application, the staged heating includes the steps of:
s2221: heating the reactant to 200 ℃, and preserving heat for at least 10min;
s2222: heating the reactant at 200 ℃ to 300 ℃ and preserving heat for at least 10min;
s2223: heating the reactant at 300 ℃ to 400 ℃ and preserving heat for at least 10min;
s2224: the reactants were heated at 400 ℃.
In some embodiments of the application, in step S2, the predetermined temperature is 380-420 ℃.
Those skilled in the art will appreciate that at 380-420 ℃, the reactants can be converted into a molten state to form the melt, and ions in the melt have strong activity and uniform distribution and are easy to crystallize into cesium-copper halide crystals when cooled; at the same time, the reactant is very stable at this temperature, and no decomposition occurs.
In some embodiments of the present application, in step S2, the predetermined vacuum degree is 0.8X10 -3 -1.2×10 -3 Pa。
Those skilled in the art will appreciate that at this vacuum level, the reactants more readily convert to the liquid phase. And the vacuum degree can remarkably reduce oxygen and other elements in the reaction environment.
In some embodiments of the application, the predetermined cooling rate is no higher than 15 ℃/h.
Those skilled in the art will appreciate that low cooling rates facilitate slow crystallization of the melt and growth of a regular crystal structure.
In some embodiments of the application, the predetermined time is not less than 6 hours.
It will be appreciated by those skilled in the art that the predetermined time is not less than 6 hours, and that the reactants may be allowed to absorb heat sufficiently to form a well mixed melt.
In some embodiments of the application, in step S2, said subjecting the reactants to an internal movement for a predetermined time is achieved in particular by means of a rocking oven.
It will be appreciated by those skilled in the art that the rocking furnace is a tube furnace that can perform the function of heating the quartz tube while rocking the quartz tube.
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. The experimental procedures, which are not specified in the following examples, are generally determined according to national standards. If the corresponding national standard does not exist, the method is carried out according to the general international standard, the conventional condition or the condition recommended by the manufacturer.
Example 1
Sa: providing a molar ratio of 3:2CsI and CuI are mixed and submerged for 30min by using a mortar to form reactants;
sb: adding reactants into a quartz tube, vacuumizing the quartz tube, sealing the tube, and controlling the vacuum degree in the quartz tube to be 10 when sealing the tube -3 Pa；
Sc: placing the quartz tube after tube sealing in a swinging furnace, swinging at a swinging speed of 10r/min, heating in sections until reaching 400 ℃, and preserving heat for 6 hours at 400 ℃;
sd: cooling the quartz tube to 30 ℃ at a cooling rate of 15 ℃/h to obtain Cs 3 Cu 2 I 5 And (5) a crystal.
Wherein the step of sectioning heating specifically comprises the following steps:
heating the reactant to 200 ℃, and preserving heat for 10min;
heating the reactant at 200 ℃ to 300 ℃ and preserving heat for 10min;
heating the reactant at 300 ℃ to 350 ℃ and preserving heat for 10min;
the reaction was heated to 400 c at 350 c.
XRD test was performed on the sample prepared in this example, and the test results are shown in FIG. 1.
As can be seen from FIG. 1, the prepared Cs 3 Cu 2 I 5 The peak position is consistent with the standard XRD peak position, which shows that the prepared Cs 3 Cu 2 I 5 Is pure phase.
Example 2
Sa: providing a molar ratio of 5:1:2 CsCl, cuCl and CuI are mixed and submerged for 30min by a mortar to form reactants;
sb: adding reactants into a quartz tube, vacuumizing the quartz tube, sealing the tube, and controlling the vacuum degree in the quartz tube to be 10 when sealing the tube -3 Pa；
Sc: placing the quartz tube after tube sealing in a swinging furnace, swinging at a swinging speed of 10r/min, heating in sections until the temperature reaches 450 ℃, and preserving heat for 6 hours at the temperature of 450 ℃;
sd: cooling the quartz tube to 30 ℃ at a cooling rate of 15 ℃/h to obtain Cs 5 Cu 3 Cl 6 I 2 And (5) a crystal.
Wherein the step of sectioning heating specifically comprises the following steps:
heating the reactant to 200 ℃, and preserving heat for 10min;
heating the reactant at 200 ℃ to 300 ℃ and preserving heat for 10min;
heating the reactant at 300 ℃ to 400 ℃ and preserving heat for 10min;
the reaction was heated to 450 ℃ at 400 ℃.
XRD test was performed on the sample prepared in this example, and the test results are shown in FIG. 2.
As can be seen from FIG. 2, the prepared Cs 5 Cu 3 Cl 6 I 2 The peak position is consistent with the standard XRD peak position, which shows that the prepared Cs 5 Cu 3 Cl 6 I 2 Is pure phase. .
Various embodiments of the application may exist in a range of forms; it should be understood that the description in a range format is merely for convenience and brevity and should not be construed as a rigid limitation on the scope of the application; it is therefore to be understood that the range description has specifically disclosed all possible sub-ranges and individual values within that range. For example, it should be considered that a description of a range from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5, and 6, wherever applicable. In addition, whenever a numerical range is referred to herein, it is meant to include any reference number (fractional or integer) within the indicated range.
In the present application, unless otherwise specified, terms such as "upper" and "lower" are used specifically to refer to the orientation of the drawing in the figures. In addition, in the description of the present specification, the terms "include", "comprising" and the like mean "including but not limited to". Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising … …" does not exclude the presence of other like elements in a process, method, article or apparatus that comprises the element. Relational terms such as "first" and "second", and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Herein, "and/or" describing an association relationship of an association object means that there may be three relationships, for example, a and/or B, may mean: a alone, a and B together, and B alone. For the association relation of more than three association objects described by the "and/or", it means that any one of the three association objects may exist alone or any at least two of the three association objects exist simultaneously, for example, for a, and/or B, and/or C, any one of the A, B, C items may exist alone or any two of the A, B, C items exist simultaneously or three of the three items exist simultaneously. Herein, "at least one" means one or more, and "a plurality" means two or more. "at least one", "at least one" or the like refer to any combination of these items, including any combination of single item(s) or plural items(s). For example, "at least one (individual) of a, b, or c," or "at least one (individual) of a, b, and c," may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, c may be single or multiple, respectively.
The foregoing is only a specific embodiment of the application to enable those skilled in the art to understand or practice the application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (3)
1. The preparation method of the cesium copper halide crystal is characterized by comprising the following steps of:
providing a compound with chemical formulas of CsX and CuX, and uniformly mixing to obtain a reactant, wherein X is at least one of Cl, br and I;
placing the reactant under the predetermined vacuum; heating reactants under a preset vacuum degree in a segmented way until reaching the preset temperature, and simultaneously enabling the reactants to perform internal movement for a preset time to obtain a melt;
cooling the melt at a predetermined cooling rate to obtain the cesium copper halide crystals;
and X is I, and the mol ratio of CsX to CuX is 3:2;
the step of heating comprises the following steps:
heating the reactant to 200 ℃, and preserving heat for at least 10min;
heating the reactant at 200 ℃ to 300 ℃ and preserving heat for at least 10min;
heating the reactant at 300 ℃ to 350 ℃ and preserving heat for at least 10min;
heating the reactant at 350 ℃;
the preset temperature is 380-450 ℃;
the predetermined vacuum degree is 0.8X10 -3 -1.2×10 -3 Pa；
The predetermined cooling rate is not higher than 15 ℃/h;
the predetermined time is not shorter than 6 hours.
2. The method for preparing cesium copper halide crystals according to claim 1, wherein X is a combination of two elements of Cl and I, and the molar ratio of Cs, cu, cl, I atoms in the reactant is 5:3:6:2.
3. the method for preparing cesium copper halide crystals of claim 2, wherein the step of heating in stages comprises the steps of:
heating the reactant to 200 ℃, and preserving heat for at least 10min;
heating the reactant at 200 ℃ to 300 ℃ and preserving heat for at least 10min;
heating the reactant at 300 ℃ to 400 ℃ and preserving heat for at least 10min;
the reactants were heated at 400 ℃.
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