CN115323493B - Large-size layered FeOCl single crystal and preparation method thereof - Google Patents
Large-size layered FeOCl single crystal and preparation method thereof Download PDFInfo
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- CN115323493B CN115323493B CN202211166701.3A CN202211166701A CN115323493B CN 115323493 B CN115323493 B CN 115323493B CN 202211166701 A CN202211166701 A CN 202211166701A CN 115323493 B CN115323493 B CN 115323493B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/12—Halides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/68—Crystals with laminate structure, e.g. "superlattices"
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
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Abstract
The application discloses a large-size layered FeOCl single crystal and a preparation method thereof, and belongs to the technical field of preparation of metal oxychloride materials. The application discloses a preparation method of a large-size layered FeOCl single crystal, which adopts FeCl 3` 6H 2 Preparing FeOCl powder by O, and then carrying out heating treatment on the FeOCl powder through different heating program settings of a hot end and a cold end to finally obtain a large-size layered FeOCl single crystal; since FeCl is not used 3 Avoiding FeCl in the preparation process 3 The gasification of the catalyst has no impurity, low environmental pressure in the preparation process, simple and easy realization of preparation conditions and good application prospect. The large-size layered FeOCl single crystal prepared by the method has high purity, good quality and good application value.
Description
Technical Field
The application belongs to the technical field of preparation of metal oxy-chlorine compound materials, and particularly relates to a large-size layered FeOCl single crystal and a preparation method thereof.
Background
Metal oxy-chlorine compound MO x Cl y (m=transition metal or rare earth metal) is a group of compounds bound to metal elements by oxygen and chlorine atoms, which have strong in-plane m—o chemical bonds and weak out-of-plane cl—cl interlayer van der waals interactions, such as FeOCl, znOCl, biOCl and CuOCl; they are a class of ternary lamellar compounds, known for their unique lamellar structure and chemical stability. The layered structure of the metal oxychloride can promote the separation and transmission of charge carriers, can be used as a high-efficiency photocatalyst, such as water decomposition under ultraviolet or visible light, environment restoration and hydrogen production, and the electronic, magnetic and photoluminescent behaviors of the metal oxychloride are also of great concern.
The chemical industry widely produces toxic pollutants and harmful organic compounds, causes serious pollution to water resources, and causes serious problems to the environment and human beings, and the high-efficiency photocatalyst has the advantages of high efficiency, no secondary pollution and the like, so the high-efficiency photocatalyst is widely focused in the field of solving the environmental pollution. Among them, fenton reaction (Fenton) is a powerful solution because of its advantages of safety, economy, high efficiency, environmental protection, etc. Han et al report an excellent Fenton-like catalyst FeOCl, and prepared FeOCl/SiO2 and FeOCl/SBA-15 photocatalysts, further improving the catalytic efficiency of FeOCl.
At present, complex chemical vapor phase method is generally adopted for FeOCl synthesis, continuous reaction is required to be carried out for several days at high temperature of 643K (370 ℃) to form large-size FeOCl, in the synthesis process, the reaction condition is complex, the requirement is high, and meanwhile, because FeCl is adopted as the raw material 3 FeCl in the preparation process 3 Resulting in higher pressures and the presence of FeCl in the synthesized FeOCl 3 And (5) impurities.
Disclosure of Invention
In order to overcome the defects of the prior art, the application aims to provide a large-size layered FeOCl single crystal and a preparation method thereof, which are used for solving the technical problems of high preparation conditions, high cost, large pollution, low yield, poor quality of the obtained large-size FeOCl and the like when the large-size FeOCl is prepared in the prior art.
In order to achieve the above purpose, the application is realized by adopting the following technical scheme:
the application discloses a preparation method of a large-size layered FeOCl monocrystal, which comprises the following steps:
s1: feCl is added 3` 6H 2 O is ground and then is placed in heating equipment for heating treatment, so that FeOCl powder is obtained;
s2: placing the FeOCl powder obtained in the step S1 into a tubular container, and then placing the tubular container into a heating device with a hot end and a cold end, wherein one end of the tubular container is placed at the cold end, and the other end of the tubular container is placed at the hot end;
s3: and heating the hot end and the cold end respectively by a heating program, and obtaining the large-size layered FeOCl monocrystal on the container wall at one end of the tubular container placed at the cold end after the heating treatment.
Further, in S1, the step of the heating treatment is: feCl is added 3` 6H 2 O is placed in a heating device after grinding, then the heating device is vacuumized and filled with nitrogen, and then the heating device is heated to (220-250) DEG C at (5-10) DEG C/min and maintained for (120-180) min.
Further, in S1, the heating device is a single-temperature zone tube furnace.
Further, in S2, the tubular container is an ampoule; the heating equipment with a hot end and a cold end is a double-temperature-zone tube furnace.
Further, in S2, after FeOCl powder is put into a tubular container, the tubular container is vacuumized until the vacuum degree in the tubular container is less than or equal to 10 -5 Torr, sealing the tubular container, and then placing the tubular container in a heating apparatus having a hot end and a cold end.
Further, in S3, the heating procedure of the hot end is: heating the hot end to 380-395 ℃, then preserving heat for 40-50 h, and cooling to room temperature.
Further, in S3, the heating procedure of the cold end is: heating the cold end to 365-375 deg.c, maintaining for 40-50 hr, and cooling to room temperature.
The application also discloses a large-size layered FeOCl single crystal prepared by the preparation method, wherein the size of the large-size layered FeOCl single crystal is (1 multiplied by 5) mm 2 ～(1×10)mm 2 。
Compared with the prior art, the application has the following beneficial effects:
the application discloses a preparation method of a large-size layered FeOCl single crystal, which only uses FeCl 3` 6H 2 O is used as a raw material, feOCl powder is obtained according to treatment, and then the FeOCl powder is subjected to heating treatment through different heating program settings of a hot end and a cold end, and finally the large-size layered FeOCl single crystal is obtained; since FeCl is not used 3 Avoiding FeCl in the preparation process 3 Is gasified without impurity, and is environment in the preparation processThe pressure is low, the preparation conditions are simple and easy to realize, and the preparation method is not used for operation in a glove box; the raw materials are few, so that the preparation cost is reduced; the method for preparing FeOCl single crystal has the advantages of high yield and good application prospect.
The application also discloses a large-size layered FeOCl monocrystal prepared by the preparation method, and the FeCl is not adopted 3 Avoiding FeCl 3 Impurity, the prepared layered FeOCl single crystal has good purity, high quality and excellent performance, and the size of the shaped FeOCl single crystal also reaches (1 multiplied by 5) mm 2 ～(1×10)mm 2 Realizes the breakthrough that no preparation method for large-size layered FeOCl single crystals exists at present, and has good application value.
Drawings
FIG. 1 is an X-ray energy dispersion spectrum of a large-size layered FeOCl single crystal prepared by the application;
FIG. 2 is an XRD pattern of a large-sized layered FeOCl single crystal prepared by the present application;
FIG. 3 is an x-ray photoelectron spectrum of a large-sized layered FeOCl single crystal prepared by the present application.
Wherein: a-Fe element energy spectrum; b-O element energy spectrum; c-Cl element energy spectrum;
FIG. 4 is a Raman spectrum diagram of a large-size layered FeOCl single crystal prepared by the application;
FIG. 5 is a drawing showing the Raman spectrum of FeOCl before and after exposing large-sized layered FeOCl single crystals prepared by the application to air for 9 months.
Detailed Description
So that those skilled in the art can appreciate the features and effects of the present application, a general description and definition of the terms and expressions set forth in the specification and claims follows. Unless otherwise defined, 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, and in the event of a conflict, the present specification shall control.
The theory or mechanism described and disclosed herein, whether right or wrong, is not meant to limit the scope of the application in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features such as values, amounts, and concentrations that are defined herein in the numerical or percent ranges are for brevity and convenience only. Accordingly, the description of a numerical range or percentage range should be considered to cover and specifically disclose all possible sub-ranges and individual values (including integers and fractions) within the range.
Herein, unless otherwise indicated, "comprising," "including," "having," or similar terms encompass the meanings of "consisting of … …" and "consisting essentially of … …," e.g., "a includes a" encompasses the meanings of "a includes a and the other and" a includes a only.
In this context, not all possible combinations of the individual technical features in the individual embodiments or examples are described in order to simplify the description. Accordingly, as long as there is no contradiction between the combinations of these technical features, any combination of the technical features in the respective embodiments or examples is possible, and all possible combinations should be considered as being within the scope of the present specification.
The application provides a preparation method of a large-size high-quality layered FeOCl single crystal, which comprises the following steps:
s1: first, A is carried out 1 g FeCl 3` 6H 2 O raw material is ground, and the ground sample is placed in a quartz boat and transferred into a single-temperature zone tube furnace. Then the tube furnace is vacuum treated and nitrogen is filled for protection. Finally, the furnace is heated up, firstly T is used for 1 Heating at a temperature of T/min 2 C, and maintaining t 1 And (5) min, and finally obtaining FeOCl powder.
S2: then weigh A 2 Placing FeOCl powder prepared in step one into ampoule tube, vacuum-pumping to 10 -5 ～10 - 6 And (3) sealing the ampoule pipe by Torr, and placing the ampoule pipe in a double-temperature zone tubular furnace.
S3: the hot end and the cold end are respectively heated up to T 3 ℃，T 4 Heating t at a temperature of 2 The time period of the time period,after cooling, the quartz tube was broken up and the layered FeOCl single crystal obtained in the cold end tube wall was peeled off with forceps.
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. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
The following examples use instrumentation conventional in the art. The experimental methods, in which specific conditions are not noted in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The following examples used various starting materials, unless otherwise indicated, were conventional commercial products, the specifications of which are conventional in the art. In the description of the present application and the following examples, "%" means weight percent, and "parts" means parts by weight, and ratios means weight ratio, unless otherwise specified.
Example 1
A preparation method of a large-size layered FeOCl single crystal comprises the following steps:
s1: first, 1g of FeCl 3` 6H 2 Grinding the raw material O, then placing the raw material O in a quartz boat, and transferring the quartz boat into a single-temperature zone tube furnace; then carrying out vacuumizing treatment on the single-temperature-zone tubular furnace, filling nitrogen for protection, and finally carrying out heating treatment on the single-temperature-zone tubular furnace, heating to 220 ℃ at 8 ℃/min, and keeping for 120min to obtain FeOCl powder;
s2: 1g of FeOCl powder prepared by S1 is weighed and placed in an ampoule tube, and the ampoule tube is vacuumized to 10 -5 Sealing after Torr, placing the ampoule tube into a heating zone tube furnace, wherein one end of the ampoule tube is placed at a cold end, and the other end of the ampoule tube is placed at a hot end;
s3: heating the hot end and the cold end to 395 ℃ and 375 ℃ respectively, preserving heat for 50 hours, cooling to room temperature, breaking the ampoule tube, and stripping the ampoule tube wall at one end of a tubular container placed at the cold end to obtain the large-size layered FeOCl single crystal.
The large-size layered FeOCl single crystal obtained in this example had a size of about 1X 8mm 2 The yield was about 60%.
Example 2
A preparation method of a large-size layered FeOCl single crystal comprises the following steps:
s1: first, 1g of FeCl 3` 6H 2 Grinding the raw material O, then placing the raw material O in a quartz boat, and transferring the quartz boat into a single-temperature zone tube furnace; then carrying out vacuumizing treatment on the single-temperature-zone tubular furnace, filling nitrogen for protection, and finally carrying out heating treatment on the single-temperature-zone tubular furnace, heating to 230 ℃ at 8 ℃/min, and keeping for 140min to obtain FeOCl powder;
s2: 1g of FeOCl powder prepared by S1 is weighed and placed in an ampoule tube, and the ampoule tube is vacuumized to 10 -5 Sealing after Torr, placing the ampoule tube into a heating zone tube furnace, wherein one end of the ampoule tube is placed at a cold end, and the other end of the ampoule tube is placed at a hot end;
s3: heating the hot end and the cold end to 390 ℃ and 370 ℃ respectively, preserving heat for 45h, cooling to room temperature, breaking the ampoule tube, and stripping the ampoule tube wall at one end of a tubular container placed at the cold end to obtain the large-size layered FeOCl single crystal.
The large-size layered FeOCl single crystal obtained in this example had a size of about 2X 5mm 2 The yield was about 50%.
Example 3
A preparation method of a large-size layered FeOCl single crystal comprises the following steps:
s1: first, 1g of FeCl 3` 6H 2 Grinding the raw material O, then placing the raw material O in a quartz boat, and transferring the quartz boat into a single-temperature zone tube furnace; then carrying out vacuumizing treatment on the single-temperature-zone tubular furnace, filling nitrogen for protection, and finally carrying out heating treatment on the single-temperature-zone tubular furnace, heating to 240 ℃ at 10 ℃/min, and keeping for 160min to obtain FeOCl powder;
s2: 1g of FeOCl powder prepared by S1 is weighed and placed in an ampoule tube, and the ampoule tube is vacuumized to 10 -5 Sealing after Torr, and installingAmpoule tube is placed in the heating zone tube furnace, one end of ampoule tube is placed at cold end, and the other end is placed at hot end;
s3: heating the hot end and the cold end to 385 ℃ and 370 ℃ respectively, preserving heat for 40 hours, cooling to room temperature, breaking the ampoule tube, and stripping the ampoule tube wall at one end of a tubular container placed at the cold end to obtain the large-size layered FeOCl single crystal.
The large-size layered FeOCl single crystal obtained in this example had a size of about 2X 5mm 2 The yield was about 57%.
Example 4
A preparation method of a large-size layered FeOCl single crystal comprises the following steps:
s1: first, 1g of FeCl 3` 6H 2 Grinding the raw material O, then placing the raw material O in a quartz boat, and transferring the quartz boat into a single-temperature zone tube furnace; then carrying out vacuumizing treatment on the single-temperature-zone tubular furnace, filling nitrogen for protection, and finally carrying out heating treatment on the single-temperature-zone tubular furnace, heating to 250 ℃ at 10 ℃/min, and keeping for 180min to obtain FeOCl powder;
s2: 1g of FeOCl powder prepared by S1 is weighed and placed in an ampoule tube, and the ampoule tube is vacuumized to 10 -5 Sealing after Torr, placing the ampoule tube into a heating zone tube furnace, wherein one end of the ampoule tube is placed at a cold end, and the other end of the ampoule tube is placed at a hot end;
s3: heating the hot end and the cold end to 385 ℃ and 365 ℃ respectively, preserving heat for 40 hours, cooling to room temperature, breaking the ampoule tube, and stripping the ampoule tube wall at one end of a tubular container placed at the cold end to obtain the large-size layered FeOCl single crystal.
The large-size layered FeOCl single crystal obtained in this example had a size of about 1X 5mm 2 The yield was about 64%.
Example 5
A preparation method of a large-size layered FeOCl single crystal comprises the following steps:
s1: first, 1g of FeCl 3` 6H 2 Grinding the raw material O, then placing the raw material O in a quartz boat, and transferring the quartz boat into a single-temperature zone tube furnace; then for single temperature zone tube typeVacuumizing the furnace, filling nitrogen for protection, and finally heating the single-temperature-zone tubular furnace to 245 ℃ at 10 ℃/min, and keeping for 170min to obtain FeOCl powder;
s2: 1.5g of FeOCl powder prepared by S1 is weighed and placed in an ampoule tube, and the ampoule tube is vacuumized to 10 -5 Sealing after Torr, placing the ampoule tube into a heating zone tube furnace, wherein one end of the ampoule tube is placed at a cold end, and the other end of the ampoule tube is placed at a hot end;
s3: heating the hot end and the cold end to 380 ℃ and 365 ℃ respectively, preserving heat for 40 hours, cooling to room temperature, breaking the ampoule tube, and stripping the ampoule tube wall at one end of a tubular container placed at the cold end to obtain the large-size layered FeOCl single crystal.
The large-size layered FeOCl single crystal obtained in this example had a size of about 1X 10mm 2 The yield was about 55%.
Example 6
A preparation method of a large-size layered FeOCl single crystal comprises the following steps:
s1: first, 1g of FeCl 3` 6H 2 Grinding the raw material O, then placing the raw material O in a quartz boat, and transferring the quartz boat into a single-temperature zone tube furnace; then carrying out vacuumizing treatment on the single-temperature-zone tubular furnace, filling nitrogen for protection, and finally carrying out heating treatment on the single-temperature-zone tubular furnace, heating to 250 ℃ at 10 ℃/min, and keeping for 180min to obtain FeOCl powder;
s2: 0.5g of FeOCl powder prepared by S1 is weighed and placed in an ampoule tube, and the ampoule tube is vacuumized to 10 -5 Sealing after Torr, placing the ampoule tube into a heating zone tube furnace, wherein one end of the ampoule tube is placed at a cold end, and the other end of the ampoule tube is placed at a hot end;
s3: heating the hot end and the cold end to 385 ℃ and 365 ℃ respectively, preserving heat for 40 hours, cooling to room temperature, breaking the ampoule tube, and stripping the ampoule tube wall at one end of a tubular container placed at the cold end to obtain the large-size layered FeOCl single crystal.
The large-size layered FeOCl single crystal obtained in this example had a size of about 1X 8mm 2 The yield was about 67%.
Example 7
A preparation method of a large-size layered FeOCl single crystal comprises the following steps:
s1: first, 1g of FeCl 3` 6H 2 Grinding the raw material O, then placing the raw material O in a quartz boat, and transferring the quartz boat into a single-temperature zone tube furnace; then carrying out vacuumizing treatment on the single-temperature-zone tubular furnace, filling nitrogen for protection, and finally carrying out heating treatment on the single-temperature-zone tubular furnace, heating to 250 ℃ at 10 ℃/min, and keeping for 170min to obtain FeOCl powder;
s2: 0.5g of FeOCl powder prepared by S1 is weighed and placed in an ampoule tube, and the ampoule tube is vacuumized to 10 -5 Sealing after Torr, placing the ampoule tube into a heating zone tube furnace, wherein one end of the ampoule tube is placed at a cold end, and the other end of the ampoule tube is placed at a hot end;
s3: heating the hot end and the cold end to 395 ℃ and 370 ℃ respectively, preserving heat for 45h, cooling to room temperature, breaking the ampoule tube, and stripping the ampoule tube wall at one end of a tubular container placed at the cold end to obtain the large-size layered FeOCl single crystal.
The large-size layered FeOCl single crystal obtained in this example had a size of about 1X 8mm 2 The yield was about 67%.
Example 8
A preparation method of a large-size layered FeOCl single crystal comprises the following steps:
s1: first 2g FeCl 3` 6H 2 Grinding the raw material O, then placing the raw material O in a quartz boat, and transferring the quartz boat into a single-temperature zone tube furnace; then carrying out vacuumizing treatment on the single-temperature-zone tubular furnace, filling nitrogen for protection, and finally carrying out heating treatment on the single-temperature-zone tubular furnace, heating to 245 ℃ at 9 ℃/min, and keeping for 160min to obtain FeOCl powder;
s2: 1g of FeOCl powder prepared by S1 is weighed and placed in an ampoule tube, and the ampoule tube is vacuumized to 10 -5 Sealing after Torr, placing the ampoule tube into a heating zone tube furnace, wherein one end of the ampoule tube is placed at a cold end, and the other end of the ampoule tube is placed at a hot end;
s3: heating the hot end and the cold end to 390 ℃ and 375 ℃ respectively, preserving heat for 48 hours, cooling to room temperature, breaking the ampoule tube, and stripping the ampoule tube wall at one end of a tubular container placed at the cold end to obtain the large-size layered FeOCl single crystal.
The large-size layered FeOCl single crystal obtained in this example had a size of about 1X 10mm 2 The yield was about 64%.
Example 9
A preparation method of a large-size layered FeOCl single crystal comprises the following steps:
s1: first, 1g of FeCl 3` 6H 2 Grinding the raw material O, then placing the raw material O in a quartz boat, and transferring the quartz boat into a single-temperature zone tube furnace; then carrying out vacuumizing treatment on the single-temperature-zone tubular furnace, filling nitrogen for protection, and finally carrying out heating treatment on the single-temperature-zone tubular furnace, heating to 220 ℃ at 5 ℃/min, and keeping for 150min to obtain FeOCl powder;
s2: 1g of FeOCl powder prepared by S1 is weighed and placed in an ampoule tube, and the ampoule tube is vacuumized to 10 -5 Sealing after Torr, placing the ampoule tube into a heating zone tube furnace, wherein one end of the ampoule tube is placed at a cold end, and the other end of the ampoule tube is placed at a hot end;
s3: heating the hot end and the cold end to 385 ℃ and 365 ℃ respectively, preserving heat for 50 hours, cooling to room temperature, breaking the ampoule tube, and stripping the ampoule tube wall at one end of a tubular container placed at the cold end to obtain the large-size layered FeOCl single crystal.
The large-size layered FeOCl single crystal obtained in this example had a size of about 1X 10mm 2 The yield was about 70%.
FIG. 1 is an X-ray energy dispersive spectrum of a large-size layered FeOCl single crystal, wherein the Fe, O and Cl elements are uniformly distributed, and the stoichiometric ratio of the Fe, O and Cl elements is about 1:1:1.
FIG. 2 is an XRD pattern of a large-sized layered FeOCl single crystal, from which it can be seen that 5 peaks appear at 10.9 °, 33.7 °, 45.6 °, 58.0 ° and 71.3 °, indicating a high crystal quality and a preferential orientation of the growth direction along the [001] axis.
FIG. 3 is an x-ray of a large-size layered FeOCl single crystalFrom the photoelectron spectrum, the bond state of FeOCl crystal was measured by x-ray photoelectron spectrum, and it can be seen from FIGS. 3a to 3c that two main peaks at 711.1eV and 725.0eV correspond to Fe 2p, respectively 3/2 And Fe 2p 1/2 The presence of the Fe (III) state in FeOCl was confirmed by the presence of the Fe 2p peak and the satellite peak at 719.1eV, the peak at 530.0eV being the signal of Fe-O bonding, the other two peaks being 198.2eV and 199.8eV, respectively, corresponding to Cl 2p 3/2 And Cl 2p 1/2 。
FIG. 4 is a Raman spectrum of a large-sized layered FeOCl single crystal, from which it can be seen that FeOCl has no FeCl in the Raman spectrum 3 The signal, again, illustrates that the as-grown FeOCl has a higher crystal quality.
FIG. 5 is a graph showing the Raman spectrum of FeOCl before and after exposing large layered FeOCl single crystals to air for 9 months, and it can be seen from the graph that some layers of FeOCl can be stabilized for 9 months at room temperature, and have good stability.
The above is only for illustrating the technical idea of the present application, and the protection scope of the present application is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present application falls within the protection scope of the claims of the present application.
Claims (4)
1. The preparation method of the large-size layered FeOCl single crystal is characterized by comprising the following steps of:
s1: feCl is added 3` 6H 2 O is ground and then is placed in heating equipment for heating treatment, so that FeOCl powder is obtained;
in S1, the heating treatment includes the steps of: feCl is added 3` 6H 2 O is placed in heating equipment after grinding, then the heating equipment is vacuumized, nitrogen is filled in, then the heating equipment is heated to 220-250 ℃ at 5-10 ℃/min, and the temperature is kept for 120-180 min;
s2: placing the FeOCl powder obtained in the step S1 into a tubular container, and then placing the tubular container into a heating device with a hot end and a cold end, wherein one end of the tubular container is placed at the cold end, and the other end of the tubular container is placed at the hot end;
s2, placing FeOCl powder into a tubular container, vacuumizing the tubular container until the vacuum degree in the tubular container is less than or equal to 10 -5 Torr, sealing the tubular container, and then placing the tubular container in a heating apparatus having a hot end and a cold end;
s3: heating the hot end and the cold end respectively by a heating program, and obtaining a large-size layered FeOCl monocrystal on the container wall at one end of a tubular container placed at the cold end after the heating treatment is finished;
s3, the heating program of the hot end is as follows: heating the hot end to 380-395 ℃, preserving heat for 40-50 hours, and cooling to room temperature; the heating program of the cold end is as follows: and heating the cold end to 365-375 ℃, then preserving heat for 40-50 h, and cooling to room temperature.
2. The method for producing a large-sized layered FeOCl single crystal as defined in claim 1, wherein in S1, the heating apparatus is a single-temperature zone tube furnace.
3. The method for producing a large-sized layered FeOCl single crystal according to claim 1, wherein in S2, the tubular container is an ampoule.
4. The method for producing a large-sized layered FeOCl single crystal according to claim 1, wherein in S2, the heating apparatus having a hot end and a cold end is a double-temperature zone tube furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211166701.3A CN115323493B (en) | 2022-09-23 | 2022-09-23 | Large-size layered FeOCl single crystal and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211166701.3A CN115323493B (en) | 2022-09-23 | 2022-09-23 | Large-size layered FeOCl single crystal and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115323493A CN115323493A (en) | 2022-11-11 |
| CN115323493B true CN115323493B (en) | 2023-10-03 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491429A (en) * | 2011-11-16 | 2012-06-13 | 华东师范大学 | Preparation method of FeOCl |
| CN112337490A (en) * | 2020-11-10 | 2021-02-09 | 安徽舜禹水务股份有限公司 | Preparation of Mn-FeOCl material and application method of Mn-FeOCl material in catalytic degradation of malachite green in water |
| CN114314673A (en) * | 2021-12-30 | 2022-04-12 | 合肥学院 | Preparation method of flaky FeOCl nano material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491429A (en) * | 2011-11-16 | 2012-06-13 | 华东师范大学 | Preparation method of FeOCl |
| CN112337490A (en) * | 2020-11-10 | 2021-02-09 | 安徽舜禹水务股份有限公司 | Preparation of Mn-FeOCl material and application method of Mn-FeOCl material in catalytic degradation of malachite green in water |
| CN114314673A (en) * | 2021-12-30 | 2022-04-12 | 合肥学院 | Preparation method of flaky FeOCl nano material |
Non-Patent Citations (1)
| Title |
|---|
| 2D FeOCl：A Highly In-Plane Anisotropic Antiferromagnetic Semiconductor Synthesized via Temperature-Oscillation Chemical Vapor Transport;Yi Zeng等;ADVANCED MATERIALS;第34卷;2108847 * |
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