Universal preparation method for ternary layered compound MPS3
By synthesizing the ternary layered compound MPS3 in one step from metal powder, phosphorus powder and sulfur powder, the problems of low synthesis efficiency and cumbersome post-processing are solved, and efficient and low-cost preparation of MPS3 is achieved, which is suitable for ion transport, electrochemical energy storage and catalysis.
Patent Information
- Application Number
- CN202410262472.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-03-07
- Publication Date
- 2025-09-09
AI Technical Summary
The synthesis efficiency of the ternary layered compound MPS3 in the existing technology is low and the post-processing is cumbersome. In particular, the chemical vapor transfer method has slow synthesis speed and difficulty in removing the reaction medium iodine.
Using metal powder or alloy powder, phosphorus powder and sulfur powder as reactants, the ternary layered MPS3 powder is synthesized in a one-step process of cold pressing, vacuum packaging and heat treatment, avoiding the use of elemental iodine as a synthesis medium.
The efficient synthesis of the ternary layered compound MPS3 was achieved, with fast synthesis speed, small grain size, low raw material cost, simplified post-processing process, and suitability for industrial production.
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Figure CN120607274A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of nanomaterials, in particular to a general preparation method for a ternary layered compound MPS3. Background Art
[0002] MPS3 is a general term for a class of ternary layered compounds, where M primarily includes elements such as Mg, Ca, Sc, Ba, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Cd, and Sn. MPS3 shows promising applications in a wide range of fields, including ion transport, electrochemical energy storage, catalysis, and sensors. Currently, MPS3 is synthesized using methods such as chemical vapor transfer (CVT), chemical vapor deposition (CVD), high-energy ball milling, liquid-phase synthesis, and microwave-assisted synthesis, with CVT being the most widely used. However, CVT methods suffer from low synthesis efficiency and cumbersome post-processing. Therefore, developing efficient, simple, and versatile methods for preparing MPS3 is of great significance. Summary of the Invention
[0003] The purpose of the present invention is to provide a universal preparation method for the ternary layered compound MPS3, which solves the problems of low synthesis efficiency and complicated post-processing in the commonly used synthesis methods.
[0004] The technical solution of the present invention:
[0005] A general preparation method for a ternary layered compound MPS3 comprises the following steps:
[0006] (1) uniformly mixing metal powder, phosphorus powder and sulfur powder;
[0007] (2) cold pressing the mixed powder;
[0008] (3) vacuum packaging the formed powder;
[0009] (4) The encapsulated powder is heated to a specified temperature and then kept warm.
[0010] The general preparation method for the ternary layered compound MPS3, in step (1), the metal powder uses one or more of the metal elements Mg, Ca, Sc, Ba, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Cd, Sn and their alloys.
[0011] In the general preparation method for the ternary layered compound MPS3, the atomic ratio of M:P:S in the powder after the metal powder, phosphorus powder and sulfur powder are mixed is (1:0.8:2.5) to (1:1.2:3.5).
[0012] In the general preparation method for the ternary layered compound MPS3, in step (2), the diameter of the molding die is between 5 mm and 200 mm, and the molding pressure is between 2 kN and 100 kN to mold the powder.
[0013] In the general preparation method for the ternary layered compound MPS3, in step (3), the packaging container is a reactor made of quartz, polytetrafluoroethylene or a precious metal liner, and the inner wall of the packaging container is an inert material that does not react with the three components M, P and S, and its diameter is between 5 mm and 250 mm.
[0014] The general preparation method for the ternary layered compound MPS3 is characterized in that, in step (3), the vacuum is evacuated to a pressure of 10 -9 Pa~10 3 Pa.
[0015] In the general preparation method for the ternary layered compound MPS3, in step (4), the heating rate is between 1°C / min and 100°C / min.
[0016] In the general preparation method for the ternary layered compound MPS3, in step (4), the insulation temperature is between 100° C. and 1000° C., and the insulation time is between 1 minute and 1000 hours.
[0017] The design concept of the present invention:
[0018] The present invention overcomes the problems of slow synthesis speed and the need to remove iodine from the reaction medium in traditional chemical vapor transport methods, and proposes a method for directly synthesizing ternary layered MPS3 powder using metal powder or alloy powder and phosphorus powder and sulfur powder as reactants.
[0019] The advantages and beneficial effects of the present invention are:
[0020] 1. The present invention uses metal or alloy powder, phosphorus powder, and sulfur powder as reactants to directly produce the ternary layered compound MPS3 through a one-step process. This method has the advantages of low raw material cost, fast synthesis speed, and small grain size.
[0021] 2. Compared with the traditional CVT synthesis method, this method has significant advantages in synthesis efficiency, which is more than five times that of the CVT method.
[0022] 3. The present invention does not require elemental iodine as a synthesis medium in the preparation of MPS3, so there is no need for post-processing to remove iodine, and the powder can be used directly after simple grinding.
[0023] The present invention has low requirements on equipment in the process of preparing MPS3, does not require a dual-temperature zone furnace, is easy to scale up, and is of great significance to the industrial production of MPS3. BRIEF DESCRIPTION OF THE DRAWINGS
[0024] Figure 1 :(a) is the scanning morphology of CdPS3; (b) is the XRD spectrum of CdPS3, where the horizontal axis 2θ represents the diffraction angle (degree) and the vertical axis Intensity represents the relative intensity (arb units).
[0025] Figure 2 :(a) is the scanning morphology of MnPS3; (b) is the XRD spectrum of MnPS3, where the horizontal axis 2θ represents the diffraction angle (degree) and the vertical axis Intensity represents the relative intensity (arb units).
[0026] Figure 3 :(a) is the scanning morphology of FePS3; (b) is the XRD spectrum of FePS3, where the horizontal axis 2θ represents the diffraction angle (degree), and the vertical axis Intensity represents the relative intensity (arb units).
[0027] Figure 4 :(a) is the scanning morphology of NiPS3; (b) is the XRD spectrum of NiPS3, where the horizontal axis 2θ represents the diffraction angle (degree), and the vertical axis Intensity represents the relative intensity (arb units).
[0028] Figure 5 This is the scanning morphology of ZnPS3; Figure 6 This is the XRD pattern of ZnPS3, where the horizontal axis 2θ represents the diffraction angle (degree), and the vertical axis Intensity represents the relative intensity (arb units). DETAILED DESCRIPTION
[0029] In a specific implementation process, the present invention proposes a general preparation method for the ternary layered compound MPS3, comprising the following steps:
[0030] (1) uniformly mixing metal powder (one or more metal element powders or alloy powders thereof) with phosphorus powder and sulfur powder;
[0031] (2) cold pressing the evenly mixed powder into a mold;
[0032] (3) vacuum packaging the formed powder;
[0033] (4) The vacuum-encapsulated powder is heated to a specified temperature and then subjected to heat preservation heat treatment to synthesize layered MPS3 powder.
[0034] The feasibility of the present invention is further demonstrated below by examples.
[0035] Example 1
[0036] In this example, Cd powder was mixed with P powder and S powder and then loaded into a mold with a diameter of 10 mm. The atomic ratio of Cd:P:S in the powder after mixing Cd powder, P powder and S powder was 1:1:3. Then, a pressure of 5 kN was applied to the mold to form the powder. After the powder was formed, it was loaded into a quartz tube with an inner diameter of 12 mm and vacuumed to a pressure of 10 -2 The sealed quartz tube was sealed with Pa. The powder was placed in a muffle furnace and heated to 700°C at 5°C / min. After holding for 5 hours, it was cooled to room temperature in the furnace. Finally, the quartz tube was cut open to obtain the sample.
[0037] like Figure 1 As shown in (a), the scanning morphology of CdPS3 shows that the sample is a micron-sized powder with relatively regular morphology.
[0038] like Figure 1 As shown in (b), the XRD pattern of CdPS3 shows that the phase is composed of relatively pure CdPS3.
[0039] Example 2
[0040] In this embodiment, Mn powder was mixed with P powder and S powder and then loaded into a mold with a diameter of 10 mm. The atomic ratio of Mn:P:S in the powder after mixing Mn powder, P powder and S powder was 1:1:3. Then, a pressure of 5 kN was applied to the mold to form the powder. After the powder was formed, it was loaded into a quartz tube with an inner diameter of 12 mm and vacuumed to a pressure of 10 -2 The sealed quartz tube was sealed with Pa. The powder was placed in a muffle furnace and heated to 700°C at 5°C / min. After holding for 5 hours, it was cooled to room temperature in the furnace. Finally, the quartz tube was cut open to obtain the sample.
[0041] like Figure 2 As shown in (a), the scanning morphology of MnPS3 shows that the sample is a micron-sized powder with relatively regular morphology.
[0042] like Figure 2 As shown in (b), the XRD pattern of MnPS3 shows that the phase is composed of MnPS3 and a small amount of MnS.
[0043] Example 3
[0044] In this embodiment, Fe powder, P powder, and S powder were mixed evenly and then loaded into a mold with a diameter of 10 mm. The atomic ratio of Fe:P:S in the powder after the Fe powder, P powder, and S powder were mixed was 1:1:3. Then, a pressure of 5 kN was applied to the mold to form the powder. After the powder was formed, it was loaded into a quartz tube with an inner diameter of 12 mm and vacuumed to a pressure of 10 -2The sealed quartz tube was sealed with Pa. The powder was placed in a muffle furnace and heated to 700°C at 5°C / min. After holding for 5 hours, it was cooled to room temperature in the furnace. Finally, the quartz tube was cut open to obtain the sample.
[0045] like Figure 3 As shown in (a), the scanning morphology of FePS3 shows that the sample is a micron-sized powder with relatively regular morphology.
[0046] like Figure 3 As shown in (b), it can be seen from the XRD pattern of FePS3 that the phase is composed of relatively pure FePS3.
[0047] Example 4
[0048] In this embodiment, Ni powder was mixed with P powder and S powder and then loaded into a mold with a diameter of 10 mm. The atomic ratio of Ni:P:S in the powder after Ni powder, P powder and S powder were 1:1:3. Then, a pressure of 5 kN was applied to the mold to form the powder. After the powder was formed, it was loaded into a quartz tube with an inner diameter of 12 mm and vacuumed to a pressure of 10 -2 The sealed quartz tube was sealed with Pa. The powder was placed in a muffle furnace and heated to 700°C at 5°C / min. After holding for 5 hours, it was cooled to room temperature in the furnace. Finally, the quartz tube was cut open to obtain the sample.
[0049] like Figure 4 As shown in (a), the scanning morphology of NiPS3 shows that the sample is a micron-sized powder with relatively regular morphology.
[0050] like Figure 4 As shown in (b), the XRD pattern of NiPS3 shows that the phase is composed of relatively pure NiPS3.
[0051] Example 5
[0052] In this embodiment, Zn powder, P powder, and S powder were mixed uniformly and then loaded into a mold with a diameter of 10 mm. The atomic ratio of Zn:P:S in the powder after the Zn powder, P powder, and S powder were mixed was 1:1:3. Then, a pressure of 5 kN was applied to the mold to form the powder. After the powder was formed, it was loaded into a quartz tube with an inner diameter of 12 mm and vacuumed to a pressure of 10 -2 The sealed quartz tube was sealed with Pa. The powder was placed in a muffle furnace and heated to 700°C at 5°C / min. After holding for 5 hours, it was cooled to room temperature in the furnace. Finally, the quartz tube was cut open to obtain the sample.
[0053] like Figure 5 As shown in the figure, it can be seen from the scanning morphology of ZnPS3 that the sample is a micron-sized powder with relatively regular morphology.
[0054] like Figure 6As shown, it can be seen from the XRD pattern of ZnPS3 that the phase is composed of ZnPS3 and a small amount of ZnS.
[0055] The implementation results show that the MPS3 powder preparation method described in the present invention has the advantages of simple process, high efficiency, low cost, good crystallinity, and no need for post-processing. It is expected to be widely used in the fields of ion transport, electrochemical energy storage, catalysis, sensors, etc.
Claims
1. A general method for preparing a ternary layered compound MPS3, characterized in that: The steps include: (1) uniformly mixing metal powder, phosphorus powder and sulfur powder; (2) cold pressing the mixed powder; (3) vacuum packaging the formed powder; (4) The encapsulated powder is heated to a specified temperature and then kept warm.
2. The general preparation method for the ternary layered compound MPS3 according to claim 1, characterized in that In step (1), the metal powder uses one or more of the metal elements Mg, Ca, Sc, Ba, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Cd, Sn and their alloys.
3. The general preparation method for the ternary layered compound MPS3 according to claim 1, characterized in that In the powder obtained by mixing the metal powder, phosphorus powder and sulfur powder, the atomic ratio of M:P:S is (1:0.8:2.5) to (1:1.2:3.5).
4. The general preparation method for the ternary layered compound MPS3 according to claim 1, characterized in that In step (2), the diameter of the molding die is between 5 mm and 200 mm, and the molding pressure is between 2 kN and 100 kN to mold the powder.
5. The general preparation method for the ternary layered compound MPS3 according to claim 1, characterized in that: In step (3), the packaging container is a reactor made of quartz, polytetrafluoroethylene or a noble metal liner, and its diameter is between 5 mm and 250 mm.
6. The general preparation method for the ternary layered compound MPS3 according to claim 1 or 5, characterized in that: In step (3), the vacuum is pumped to a pressure of 10 -9 Pa~10 3 Pa.
7. The general preparation method for the ternary layered compound MPS3 according to claim 1, characterized in that In step (4), the heating rate is 1°C / min to 100°C / min.
8. The general preparation method for the ternary layered compound MPS3 according to claim 1 or 7, characterized in that In step (4), the holding temperature is between 100° C. and 1000° C., and the holding time is between 1 minute and 1000 hours.