A hydroxy samarium chloride nanosheet material and a preparation method thereof

Abstract

The invention discloses a samarium hydroxychloride nanosheet and a preparation method thereof, which belong to the technical field of preparation of rare earth element hydroxychloride nanomaterials. The samarium hydroxychloride material is composed of nanosheet-shaped samarium hydroxychloride, the thickness of the nanosheet is about 10-40nm, the side length is about 50-300nm, and the surface is smooth. The preparation method is as follows: pour samarium chloride hexahydrate and samarium oxide into a mortar, mix them thoroughly, grind them evenly, and then pour them into a reactor, set the temperature to 80-200℃, and set the time to 1-14h; after the reaction is completed, naturally cool to room temperature, grind the product again, and obtain white samarium hydroxychloride powder. The operation method of the invention is simple, easy to control, has good repeatability, high sample purity, and good crystallinity.

Description

Technical Field

[0001] The present invention belongs to the technical field of the preparation of rare earth element hydroxy chloride nanomaterials, and particularly relates to a simple, novel and efficient method for preparing nanosheet-shaped samarium hydroxy chloride materials. Background Art

[0002] Rare earth elements are typical metal elements. The orbital electrons of the 4f sublayer of the lanthanide elements are effectively shielded by the outer 5s and 5p electrons and cannot participate in bonding, resulting in their similar chemical properties and obvious differences in physical properties, creating various opportunities for the application and development of rare earth elements. The unique electronic structure of rare earth elements enables the compounds of rare earth elements to have excellent optical, electrical and magnetic properties. Magnetocaloric effect, magnetic refrigeration, magnetostriction and magneto-optical effect all fully demonstrate the individuality of rare earth elements. The metallic atomic radius of rare earth elements is larger than that of iron, and it is easy to fill in the grains and defects of steel and form a film that can hinder the continuous growth of grains, thereby refining the grains and improving the performance of steel. Using these characteristics of rare earth elements, many high-tech new materials can be prepared, opening up many doors for the application and development of rare earth elements.

[0003] The excellent optical properties of samarium elements have greatly increased the research interest of researchers. At present, the research on samarium compounds such as samarium hydroxide and samarium oxide has been very extensive and in-depth.

[0004] Samarium hydroxy chloride belongs to a new type of two-dimensional hydrogen bond compound and is a new member of the large family of two-dimensional hydrogen bond compounds. Due to the unique electronic structure of samarium elements, samarium hydroxy chloride exhibits excellent properties in aspects such as optics and electrochemistry and has great application prospects in the field of functional materials. Since samarium has good hydrogen storage capacity, the catalytic performance of samarium hydroxy chloride is also very prominent, so it can be used as a photocatalyst. Samarium hydroxy chloride can also be used to treat nuclear waste and protect the environment.

[0005] At present, the synthesis of samarium hydroxy chloride materials mostly uses the hydrothermal method: In 2001, Cyril Jouve et al. prepared Sm(OH)2Cl by the hydrothermal method, with a long reaction time and complex operation. The prepared Sm(OH)2Cl belongs to the orthorhombic system; Saburo Hosokawa et al. synthesized Sm(OH)2Cl by the hydrothermal method in 2006, and the required reaction temperature is relatively high; In 2018, Yin et al. prepared large-sized sheet-shaped samarium hydroxy chloride micron materials by the solvothermal synthesis method. The research on the preparation of nanosized samarium hydroxy chloride by the solid-phase synthesis method is very scarce.

[0006] Researchers have invested great enthusiasm in the research on the synthesis method of samarium hydroxy chloride. However, for the time being, there is little research on the synthesis of nanosheet-shaped samarium hydroxy chloride by the solid-phase method. Summary of the Invention

[0007] The technical problem to be solved by the present invention is to provide a new method for preparing nano-sheet hydroxy samarium chloride (Sm(OH)2Cl) material, which is simple, easy to control, has good repeatability, high sample purity and good crystallinity.

[0008] The specific technical solution is as follows:

[0009] A hydroxy samarium chloride nano-sheet material is composed of hydroxy samarium chloride nano-sheets, which is Sm(OH)2Cl formed by samarium, chlorine and hydroxyl in a stoichiometric ratio of 1:1:2, belonging to the monoclinic system.

[0010] The thickness of the nano-sheets is 10 - 40 nm, the side length is 50 - 300 nm, and the surface is smooth.

[0011] A method for preparing a hydroxy samarium chloride nano-sheet material uses samarium chloride hexahydrate and samarium oxide as raw materials. Put samarium chloride hexahydrate and samarium oxide into a mortar and grind for 30 minutes. Among them, the molar ratio of samarium chloride hexahydrate to samarium oxide is 1:1. Transfer the ground mixed powder to a polytetrafluoroethylene reaction kettle. Tighten the reaction kettle and put it into an electrothermal constant temperature drying oven. Set the temperature to 80°C - 200°C, and the reaction time is 1h - 14h. After the reaction is completed, wait for it to cool naturally to room temperature. Pour the product into the mortar and continue to grind for 15 minutes to obtain a white powder-like hydroxy samarium chloride sample.

[0012] The reaction temperature is preferably 190°C; the reaction time is preferably 6 hours.

[0013] Beneficial Effects:

[0014] The present invention synthesizes nano-sheet hydroxy samarium chloride material for the first time; the thickness of the nano-sheets is about 10 - 40 nm, the side length is about 50 - 300 nm, and the surface is smooth. The present invention uses the solid-phase synthesis method for the first time, which is simple in operation, has good repeatability and low cost; the yield and purity of the prepared hydroxy samarium chloride nano-sheets are high, laying a foundation for further research on the application of hydroxy chlorides. Description of the Drawings

[0015] Figure 1 It is the XRD spectrum of the Sm(OH)2Cl nano-sheets prepared in Example 1.

[0016] Figure 2 It is the SEM image of the Sm(OH)2Cl nano-sheets prepared in Example 1.

[0017] Figure 3 It is the XRD spectrum of the Sm(OH)2Cl nano-sheets prepared in Example 2.

[0018] Figure 4It is the SEM image of the Sm(OH)2Cl nanosheets prepared in Example 2.

[0019] Figure 5 It is the SEM image of the Sm(OH)2Cl nanosheets prepared in Example 3.

[0020] Figure 6 It is the XRD pattern of the Sm(OH)2Cl nanosheets prepared in Example 4.

[0021] Figure 7 It is the SEM image of the Sm(OH)2Cl nanosheets prepared in Example 4.

[0022] Figure 8 It is the XRD pattern of the Sm(OH)2Cl nanosheets prepared in Example 5. Detailed implementation manners

[0023] Example 1

[0024] Using samarium chloride hexahydrate and samarium oxide as raw materials, first put 0.221 g of samarium chloride hexahydrate (0.6 mmol) into a mortar, then put 0.211 g (0.6 mmol) of samarium oxide into the mortar as well. After mixing the two, grind them for 30 minutes; after grinding, pour the mixture into a reaction kettle, put the reaction kettle into an electrothermal constant temperature drying oven, set the temperature of the drying oven to 190 °C, and the reaction time is 6 h; wait for it to cool naturally to room temperature, then pour the product into the mortar and grind for 15 minutes to obtain a white powdery samarium hydroxy chloride sample, and the sample is samarium hydroxy chloride nanosheets.

[0025] This example is the optimal example.

[0026] Figure 1 The XRD pattern of the Sm(OH)2Cl nanosheets prepared under the above conditions is given. After comparing with the standard card, it is found that its crystallinity is good, the product is relatively pure, and there are no impurity peaks. Figure 2 The SEM image of the Sm(OH)2Cl nanosheets prepared under the above conditions is given. It can be seen that the side length of this kind of nanoblock is about 50 nm to 300 nm, the thickness is about 10 to 40 nm, and the surface is smooth.

[0027] Example 2

[0028] Using samarium chloride hexahydrate and samarium oxide as raw materials, first put 0.221 g of samarium chloride hexahydrate (0.6 mmol) into a mortar, then put 0.211 g (0.6 mmol) of samarium oxide into the mortar as well. After mixing the two, grind them for 30 minutes; after grinding, pour the medicine into a reaction kettle, put the reaction kettle into an electrothermal constant temperature drying oven, set the temperature of the drying oven to 80 °C, and the reaction time is 14 h; wait for it to cool naturally to room temperature, then pour the product into the mortar and grind for 15 minutes to obtain a white powdery samarium hydroxy chloride sample, and the sample is samarium hydroxy chloride nanosheets.

[0029] Figure 3 The XRD pattern of the prepared Sm(OH)₂Cl nanosheet crystals was given. By comparing with the standard card, it can be determined as samarium hydroxy chloride. However, the peak intensity is relatively low, indicating that the crystallinity of the sample prepared in this example is slightly worse than that in Example 1. Figure 4 The SEM image of the prepared Sm(OH)₂Cl nanosheets was given. It can be seen that the Sm(OH)₂Cl nanosheets are small in size, aggregated together, and the side length is only dozens of nanometers.

[0030] Example 3

[0031] Using samarium chloride hexahydrate and samarium oxide as raw materials, first put 0.221 g of samarium chloride hexahydrate (0.6 mmol) into a mortar, then put 0.211 g (0.6 mmol) of samarium oxide into the mortar as well. After mixing the two, grind them for 30 minutes; after the grinding is completed, pour the medicine into a reaction kettle, put the reaction kettle into an electrothermal constant temperature drying oven, set the temperature of the drying oven to 140 °C, and the reaction time is 2 h; wait for it to cool naturally to room temperature, pour the product into the mortar and grind for 15 minutes to obtain a white powdery samarium hydroxy chloride sample, and the sample is samarium hydroxy chloride nanosheets.

[0032] Figure 5 The SEM image of the prepared Sm(OH)₂Cl nanosheets was given.

[0033] Example 4

[0034] Using samarium chloride hexahydrate and samarium oxide as raw materials, first put 0.221 g of samarium chloride hexahydrate (0.6 mmol) into a mortar, then put 0.211 g (0.6 mmol) of samarium oxide into the mortar as well. After mixing the two, grind them for 30 minutes; after the grinding is completed, pour the medicine into a reaction kettle, put the reaction kettle into an electrothermal constant temperature drying oven, set the temperature of the drying oven to 170 °C, and the reaction time is 4 h; wait for it to cool naturally to room temperature, pour the product into the mortar and grind for 15 minutes to obtain a white powdery samarium hydroxy chloride sample, and the sample is samarium hydroxy chloride nanosheets.

[0035] Figure 6 The XRD pattern of the Sm(OH)₂Cl nanosheets prepared in this example was given. By comparing with the standard card, it can be determined as samarium hydroxy chloride, and the intensity is higher than that in Example 2; Figure 7 The SEM image of the Sm(OH)₂Cl nanosheets was given.

[0036] Example 5

[0037] Using samarium chloride hexahydrate and samarium oxide as raw materials, first place 0.221 g of samarium chloride hexahydrate (0.6 mmol) into a mortar, then add 0.211 g (0.6 mmol) of samarium oxide into the mortar as well. After mixing the two, grind them for 30 minutes. After the grinding is completed, pour the medicine into a reaction kettle, place the reaction kettle into an electrothermal constant temperature drying oven, set the temperature of the drying oven to 190 °C, and the reaction time is 1 h. Wait for it to cool naturally to room temperature, pour the product into a mortar and grind it for 15 minutes to obtain a white powdery samarium hydroxy chloride sample, and the sample is samarium hydroxy chloride nanosheets.

[0038] Figure 8 The XRD pattern of the Sm(OH)2Cl nanosheets prepared in this example is given, and it can be seen that the intensity is higher than that of Example 2 and Example 4.

Claims

1. A preparation method of a samarium hydroxy chloride nanosheet material, using samarium chloride hexahydrate and samarium oxide as raw materials, putting the samarium chloride hexahydrate and samarium oxide into a mortar and grinding for 30 minutes; wherein, The molar ratio of samarium chloride hexahydrate to samarium oxide is 1:

1. The ground mixed powder is transferred into a polytetrafluoroethylene reaction kettle, and the reaction kettle is tightened and placed in an electrothermal constant temperature drying oven. The temperature is set at 80 °C to 200 °C, and the reaction time is 1 to 14 hours. After the reaction is completed, it is allowed to cool naturally to room temperature. The product is poured into a mortar and ground for another 15 minutes to obtain a white powdery samarium hydroxy chloride sample; the samarium hydroxy chloride nanosheet material is composed of samarium hydroxy chloride nanosheets, and is Sm(OH)2Cl formed by samarium, chlorine and hydroxyl in a ratio of 1:1:2 by stoichiometry, belonging to the monoclinic system.

2. The preparation method of a samarium hydroxy chloride nanosheet material according to claim 1, characterized in that, The thickness of the nanosheets is 10 to 40 nm, the side length is 50 to 300 nm, and the surface is smooth.

3. The preparation method of a samarium hydroxy chloride nanosheet material according to claim 1, characterized in that, The reaction temperature in the constant temperature drying oven is 190 °C; the reaction time is 6 hours.

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