CN115403065A - Preparation method of cesium-copper halide crystal - Google Patents
Preparation method of cesium-copper halide crystal Download PDFInfo
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- CN115403065A CN115403065A CN202211044612.1A CN202211044612A CN115403065A CN 115403065 A CN115403065 A CN 115403065A CN 202211044612 A CN202211044612 A CN 202211044612A CN 115403065 A CN115403065 A CN 115403065A
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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 a cesium copper halide crystal, which comprises the following steps: providing a compound with a chemical formula 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, heating the reactant 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 is very simple in the whole preparation process, 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 serving as a metal halide material has the advantages of multiple luminescent bands, good luminescent performance, high fluorescence quantum yield and the like in the fields of luminescence and irradiation detection. At present, the synthesis method of the cesium-copper halide material is not perfect enough, and generally a solution method is used for preparing a powder material or a Bridgman method is used for preparing a single crystal material. The two methods respectively have the defects of low purity and complex and long-time process, and the further application research of the cesium copper halide material is severely limited.
Disclosure of Invention
The embodiment of the application provides a preparation method of a cesium-copper halide crystal, which aims to solve the technical problems of low purity and complex process of the existing method.
The embodiment of the application provides a preparation method of a cesium copper halide crystal, which comprises the following steps:
providing a compound with a chemical formula 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, heating the reactant 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 present application, the placing the reactant under a predetermined vacuum and heating to a predetermined temperature includes the steps of:
placing the reactant under the predetermined vacuum degree;
and heating the reactants under the preset vacuum degree in a segmented mode until the preset temperature is reached.
In some embodiments of the present application, the X is I, the CsX and CuX are in a molar ratio of 3:2.
in some embodiments of the present application, the step heating comprises the steps of:
heating the reactant to 200 ℃, and keeping the temperature for at least 10min;
heating the reactant at 200 ℃ to 300 ℃, and keeping the temperature for at least 10min;
heating the reactant at 300 ℃ to 350 ℃, and keeping the temperature for at least 10min;
the reaction was heated at 350 ℃.
In some embodiments of the present application, the X is a combination of two elements, I and Cl, and the molar ratio of Cs, cu, cl and I atoms in the reactant is 5:3:6:2.
in some embodiments of the present application, the step heating comprises the steps of:
heating the reactant to 200 ℃, and keeping the temperature for at least 10min;
heating the reactant at 200 ℃ to 300 ℃, and preserving the heat for at least 10min;
heating the reactant at 300 ℃ to 400 ℃, and preserving the heat for at least 10min;
the reaction was heated at 400 ℃.
In some embodiments of the present application, the predetermined temperature is 380-420 ℃.
In some embodiments of the present application, the predetermined vacuum level is 0.8 × 10 -3 -1.2×10 -3 Pa。
In some embodiments of the present application, the predetermined cooling rate is not higher than 15 ℃/h.
In some embodiments of the present application, the predetermined time is not shorter than 6h.
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, the appropriate halide raw material is provided, the proportion of each element in the halide raw material is adjusted to be the same as that of a target crystal to be prepared, the halide raw material is heated to be molten to obtain a melt, the melt is continuously kept to move inside to be uniformly mixed, and then the melt is cooled at a preset cooling rate to naturally crystallize to form the target crystal, so that the whole preparation process is very simple, and the obtained product has high purity.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present application and together with the description, serve to explain the principles of the application.
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious for those skilled in the art to obtain other drawings without inventive labor.
FIG. 1 is a schematic flow chart of a method for preparing cesium copper halide crystals provided in the examples of the present application;
FIG. 2 shows Cs prepared in example 1 of the present application 3 Cu 2 I 5 XRD test result pattern of crystal;
FIG. 3 shows Cs prepared in example 2 of the present application 5 Cu 3 Cl 6 I 2 XRD test result pattern of crystal.
Detailed Description
The present application will be specifically explained below with reference to specific embodiments and examples, and the advantages and various effects of the present application will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are provided to illustrate and not to limit the application.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings 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. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present application are commercially available or can be prepared by an existing method.
At present, the synthesis method of the cesium-copper halide material is not perfect enough, and generally a solution method is used for preparing a powder material or a Bridgman method is used for preparing a single crystal material. The two methods have the defects of poor material preparation performance and complex and long-time process, and seriously limit the further application research of the cesium-copper halide material.
In order to solve the technical problems, the general idea of the technical scheme provided by the embodiment of the application is as follows:
the embodiment of the application provides a preparation method of a cesium copper halide crystal, which comprises the following steps:
s1: providing a compound with a chemical formula 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 in a preset vacuum degree and heating to a preset temperature, and simultaneously carrying out internal movement of the reactant 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 halogen in cesium copper halide materials generally does not include fluorine because the atomic radius of fluorine is too small to allow fluorine to replace other halogens with a greater effect 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 ratio of CsX and CuX can be formulated by one skilled in the art according to the specific formula of the cesium copper halide crystal to be prepared according to conventional knowledge in the art.
In the present application, the purpose of bringing the reactants to a predetermined degree of vacuum is to bring the reactants to a suitable pressure, capable of producing a solid-to-liquid phase transition at the corresponding temperature; meanwhile, the method also has the function of reducing oxygen and other elements in the environment where the reactants are located, so that the cesium copper halide crystal obtained by the reaction is purer.
In the present application, the meaning of bringing the reactants into internal motion is: the substances in the reactant move mutually, so that various substances in the reactant are uniformly mixed. Such internal movement may be, for example, a vortex, a swirl, or the like in the fluid, migration of particles in the powder, or internal flow of a mixture of the powder and the fluid. Allowing the reactants to continue to move internally includes, but is not limited to, agitating the reactants, shaking the container holding the reactants.
Those skilled in the art will understand that the manner of mixing in step S1 may be conventional in the art, and may be, 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 crystalline structure of atoms or ions within the melt.
In some embodiments of the present application, the step S2 of placing the reactant under a predetermined vacuum degree and heating to a predetermined temperature includes the steps of:
s21: placing the reactant under the predetermined vacuum degree;
s22: and heating the reactants under the preset vacuum degree in a segmented mode until the preset temperature is reached.
It will be understood by those skilled in the art that staged heating refers to heating the reactants to a certain temperature followed by incubation and subsequent further heating until a predetermined temperature is reached. The purpose of the gradient heating is to ensure that the original powder is fully mixed and reacted in the swinging process, so that the reaction is slowly carried out, and the raw material powder is prevented from reacting too fast to form a heterogeneous phase. And simultaneously prevents the oxidation of the raw materials when the reaction speed is too high.
In some embodiments of the present application, the X is I, the CsX and CuX are in a molar ratio of 3:2.
as will be understood by those skilled in the art, molar ratios refer to the ratio of the amounts of the materials.
As will be understood by those skilled in the art, csI and CuI are expressed as 3:2 is Cs 3 Cu 2 I 5 。
In some embodiments of the present application, the step heating comprises the steps of:
s2211: heating the reactant to 200 ℃, and keeping the temperature for at least 10min;
s2212: heating the reactant at 200 ℃ to 300 ℃, and preserving the heat for at least 10min;
s2213: heating the reactant at 300 ℃ to 350 ℃, and keeping the temperature for at least 10min;
s2214: the reaction was heated at 350 ℃.
As can be understood by those skilled in the art, the purpose of gradient heating is to allow the original powder to be mixed and reacted sufficiently during the swinging process, so that the reaction is slow, and the raw powder is prevented from reacting too fast to form a heterogeneous phase. And simultaneously, the oxidation of the raw materials can be prevented when the reaction speed is too high.
In some embodiments of the present application, the X is a combination of two elements, I and Cl, and the molar ratio of Cs, cu, cl and I atoms in the reactant is 5:3:6:2.
as can be appreciated by those skilled in the art, the molar ratio of Cs, cu, cl, I atoms in the reactants is 5:3:6:2, preparing the obtained cesium copper halide crystal into Cs 5 Cu 3 Cl 6 I 2 。
In some embodiments of the present application, the step heating comprises the steps of:
s2221: heating the reactant to 200 ℃, and keeping the temperature for at least 10min;
s2222: heating the reactant at 200 ℃ to 300 ℃, and keeping the temperature for at least 10min;
s2223: heating the reactant at 300 ℃ to 400 ℃, and preserving the heat for at least 10min;
s2224: the reaction was heated at 400 ℃.
In some embodiments of the present application, the predetermined temperature in step S2 is 380-420 ℃.
As can be understood by those skilled in the art, at 380-420 ℃, the reactants can be transformed into a molten state to form the melt, ions in the melt have strong mobility and are uniformly distributed, and the ions are easy to crystallize into cesium halide copper crystals when cooled; at the same time, the reactants are very stable at the temperature and can not be decomposed.
In some embodiments of the present application, in step S2, the predetermined vacuum degree is 0.8 × 10 -3 -1.2×10 -3 Pa。
It will be appreciated by those skilled in the art that at this vacuum level, the reactants are more readily converted to the liquid phase. And the vacuum degree can remarkably reduce oxygen and other elements in the reaction environment.
In some embodiments of the present application, the predetermined cooling rate is not higher than 15 ℃/h.
As will be appreciated by those skilled in the art, a low cooling rate facilitates slow crystallization of the melt and growth of a regular crystal structure.
In some embodiments of the present application, the predetermined time is not shorter than 6h.
It will be appreciated by those skilled in the art that the predetermined time is not less than 6 hours, which will allow the reactants to absorb heat sufficiently to form a uniformly mixed melt.
In some embodiments of the present application, in step S2, the subjecting of the reactant to the internal movement for the predetermined time is realized by a rocking furnace.
As can be understood by those skilled in the art, the rocking furnace is a tube furnace, and can realize the functions of heating the quartz tube and rocking the quartz tube at the same time.
The present application is further illustrated below with reference to specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present application. The experimental methods of the following examples, which are not specified under specific conditions, are generally determined according to national standards. If there is no corresponding national standard, it is carried out according to the universal international standard, the conventional conditions, or the conditions recommended by the manufacturer.
Example 1
Sa: providing a molar ratio of 3:2CsI and CuI, mixing and submerging in a mortar for 30min to form a reactant;
sb: adding the reactant into the quartz tube, vacuumizing the quartz tube, sealing the quartz tube, and controlling the vacuum degree in the quartz tube to be 10 when the quartz tube is sealed -3 Pa；
And (C) Sc: placing the sealed quartz tube in a swinging furnace, swinging at a swinging speed of 10r/min, and heating in sections until the temperature reaches 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 (4) crystals.
The step heating specifically comprises the following steps:
heating the reactant to 200 ℃, and preserving the heat for 10min;
heating the reactant at 200 ℃ to 300 ℃, and preserving the heat for 10min;
heating the reactant at 300 ℃ to 350 ℃, and preserving the heat for 10min;
the reaction was heated to 400 ℃ at 350 ℃.
The 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, cs was prepared 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 a pure phase.
Example 2
Sa: providing a molar ratio of 5:1:2, mixing the CsCl, the CuCl and the CuI, and then submerging the mixture for 30min by using a mortar to form a reactant;
sb: adding the reactant into the quartz tube, vacuumizing the quartz tube, sealing the quartz tube, and controlling the vacuum degree in the quartz tube to be 10 during tube sealing -3 Pa；
And (C) Sc: placing the sealed quartz tube in a swinging furnace, swinging at a swinging speed of 10r/min, and heating in sections until the temperature reaches 450 ℃ and preserving heat for 6 hours at 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 (4) crystals.
The step heating specifically comprises the following steps:
heating the reactant to 200 ℃, and preserving the heat for 10min;
heating the reactant at 200 ℃ to 300 ℃, and preserving the heat for 10min;
heating the reactant at 300 ℃ to 400 ℃, and preserving the heat for 10min;
the reaction was heated to 450 ℃ at 400 ℃.
The XRD test characterization was performed on the sample prepared in this example, and the test results refer to fig. 2.
As can be seen from FIG. 2, cs was prepared 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 a pure phase. .
Various embodiments of the application may exist in a range; it is to be understood that the description in range format is merely for convenience and brevity and should not be construed as an inflexible limitation on the scope of the application; accordingly, the described range descriptions should be considered to have specifically disclosed all the possible sub-ranges as well as individual numerical values within that range. For example, it is contemplated that the 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 stated range, such as 1, 2, 3, 4, 5, and 6, as applicable regardless of the range. In addition, whenever a numerical range is indicated herein, it is meant to include any number (fractional or integer) recited within the indicated range.
In this application, where the context requires no explicit explanation, the use of directional words such as "upper" and "lower" in particular refers to the direction of the drawing in the figures. In addition, in the description of the present specification, the terms "include", "includes" and the like mean "including but not limited to". Also, 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 another like element in a process, method, article, or apparatus that comprises the element. In this document, 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" describes an association relationship of associated objects, meaning that there may be three relationships, e.g., a and/or B, may mean: a is present alone, A and B are present simultaneously, and B is present alone. For the association relationship of more than three associated objects described by "and/or", it means that any one of the three associated objects may exist alone, or any at least two of the three associated objects may exist simultaneously, for example, for a, and/or B, and/or C, it may mean that any one of A, B, C exists alone, or any two of the three associated objects exist simultaneously, or three of the three associated objects exist simultaneously. As used herein, "at least one" means one or more, "a plurality" means two or more. "at least one," "at least one of the following," or similar expressions, refer to any combination of these items, including any combination of the singular or plural items. For example, "at least one (a), b, or c", or "at least one (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, and c may be single or plural, respectively.
The above description is merely exemplary of the present application and is presented to enable those skilled in the art to understand and practice the present 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 (10)
1. A preparation method of cesium copper halide crystals is characterized by comprising the following steps of:
providing a compound with a chemical formula 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 in a preset vacuum degree and heating to a preset temperature, and simultaneously carrying out internal movement of the reactant for a preset time to obtain a melt;
cooling the melt at a predetermined cooling rate to obtain the cesium copper halide crystals.
2. The method for preparing cesium copper halide crystals according to claim 1, wherein said step of placing said reactants under a predetermined vacuum and heating to a predetermined temperature comprises the steps of:
placing the reactant under the predetermined vacuum degree;
and heating the reactants under the preset vacuum degree in a segmented mode until the preset temperature is reached.
3. The method of making cesium copper halide crystals according to claim 2, wherein said X is I, said CsX and CuX are in a molar ratio of 3:2.
4. the method of preparing cesium copper halide crystals according to claim 3, wherein said step-wise heating comprises the steps of:
heating the reactant to 200 ℃, and keeping the temperature for at least 10min;
heating the reactant at 200 ℃ to 300 ℃, and preserving the heat for at least 10min;
heating the reactant at 300 ℃ to 350 ℃, and keeping the temperature for at least 10min;
the reaction was heated at 350 ℃.
5. The method for preparing cesium copper halide crystals according to claim 1, wherein X is a combination of two elements Cl and I, and the molar ratio of Cs, cu, cl and I atoms in the reactants is 5:3:6:2.
6. the method of preparing cesium copper halide crystals according to claim 5, wherein said step-wise heating comprises the steps of:
heating the reactant to 200 ℃, and keeping the temperature for at least 10min;
heating the reactant at 200 ℃ to 300 ℃, and preserving the heat for at least 10min;
heating the reactant at 300 ℃ to 400 ℃, and preserving the heat for at least 10min;
the reaction was heated at 400 ℃.
7. The method for preparing cesium copper halide crystals according to claim 1, wherein the predetermined temperature is 380-450 ℃.
8. The method for producing cesium copper halide crystals according to claim 1, wherein said predetermined degree of vacuum is 0.8 x 10 -3 -1.2×10 -3 Pa。
9. The method for preparing cesium copper halide crystals according to claim 1, wherein said predetermined cooling rate is not higher than 15 ℃/h.
10. The method for producing cesium copper halide crystals according to claim 1, wherein the predetermined time is not shorter than 6 hours.
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