Alpha-PbFz nano-rod, strip or piece and its manufacturing method and use

A nano-strip, nano-rod technology, applied in chemical instruments and methods, luminescent materials, lead halide and other directions, to achieve the effects of easy availability of raw materials, simple raw materials and mild conditions

Inactive Publication Date: 2006-06-14
NANJING UNIV +1
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Abstract

The present invention relates to an alpha-PbF2 nano material. It is a one-dimentional nano rod whose diameter is 100-500 nano and length is 1300-10000 nano or nano strip whose thickness is 100-160 nano, width is 500-10000 nano and length is 4500-20000 nano or nano sheet whose thickness is 100-200 nano and side lengths are 1200-1500 nano and 1200-2500 nano. The PL optical spectrum of the invented alpha-PbF2 nano material at room temperature is strong, so that it can be used for preparing fluorescent material. Its preparation method is an ultrasonic emulsion one which is created by organically-combining ultrasonic technique and microemulsion system.

Application Domain

Lead halidesLuminescent compositions

Technology Topic

FluorescenceEmulsion +5

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  • Alpha-PbFz nano-rod, strip or piece and its manufacturing method and use
  • Alpha-PbFz nano-rod, strip or piece and its manufacturing method and use
  • Alpha-PbFz nano-rod, strip or piece and its manufacturing method and use

Examples

  • Experimental program(3)

Example Embodiment

[0050] Example 1. α-PbF 2 Preparation of nanorods
[0051] Example 1-1 After successively adding 50ml cyclohexane, 10ml OP emulsifier (TRITONXT-10), 6ml n-pentanol, 10ml 0.1mol/L lead acetate aqueous solution to a 100mL round bottom flask, the system was placed in Ningbo, Zhejiang In the JY92-2D ultrasonic instrument (ultrasonic frequency 20kHz) produced by Zhike Institute of Devices, at room temperature and normal pressure, the power was set to 600W, and the quaternary emulsion was prepared by ultrasonication for 10 minutes. Then, 10ml of 0.2mol/L ammonium fluoride solution containing 0.5g PEG-6000 was added and allowed to stand for 24h. The product was separated by centrifugation, the precipitate was washed with distilled water and ethanol in sequence, and the resulting precipitate was vacuum-dried at room temperature to obtain a white powder, namely α-PbF 2 Nano stave. Powder XRD results show that it is pure orthorhombic α-PbF 2. The positions and intensities of the peaks matched literature values ​​[Ref: Joint Committee on Powder Diffraction Standards (JCPDS), File No 06-0288.]. No heterogeneous peaks were found, indicating that the purity of the product is relatively high. PbF was observed by TEM and SEM 2 Nanorod: diameter 100-500nm, length 1300-10000nm (see Figure 3-1(a)).
[0052] Example 1-2 After successively adding 50ml cyclohexane, 10ml OP emulsifier (TRITONXT-10), 6ml n-pentanol, 10ml 0.1mol/L lead acetate aqueous solution to a 100mL round bottom flask, the system was placed in a new In the JY92-2D ultrasonic instrument produced by Zhike Instrument Research Institute, at room temperature and normal pressure, the power was set to 600W, and the quaternary emulsion was prepared by ultrasonication for 10 minutes. Then, 10ml of 0.2mol/L ammonium fluoride solution containing 0.25g PEG-600 was added and allowed to stand for 12h. The product was separated by centrifugation, the precipitate was washed with distilled water and ethanol in sequence, and the resulting precipitate was vacuum-dried at room temperature to obtain a white powder, namely α-PbF 2 Nano stave. Products of similar size and shape were also obtained (see Figure 3-2(a)).
[0053] Example 1-3 After successively adding 50ml cyclohexane, 10ml OP emulsifier (TRITONXT-10), 6ml n-pentanol, 10ml 0.25mol/L lead acetate aqueous solution into a 100mL round-bottomed flask, the system was placed in a new In the JY92-2D ultrasonic instrument produced by Zhike Instrument Research Institute, at room temperature and normal pressure, the power was set to 600W, and the quaternary emulsion was prepared by ultrasonication for 10 minutes. Then, 10ml of 0.50mol/l ammonium fluoride solution containing 0.25g PEG-600 was added and allowed to stand for 12h. The product was separated by centrifugation, the precipitate was washed with distilled water and ethanol in sequence, and the resulting precipitate was vacuum-dried at room temperature to obtain a white powder, namely α-PbF 2 Nano stave. Products of similar size and shape were also obtained (see Figure 3-3(a)).
[0054] Example 1-4 After successively adding 50ml cyclohexane, 7ml OP emulsifier (TRITONXT-10), 4ml n-pentanol, 5ml 0.25mol/L lead acetate aqueous solution into a 100mL round-bottomed flask, the system was placed in Ningbo, Zhejiang In the JY92-2D ultrasonic instrument (ultrasonic frequency 20kHz) produced by Zhike Institute of Devices, at room temperature and normal pressure, the power was set to 600W, and the quaternary emulsion was prepared by ultrasonication for 10 minutes. Then, 10ml of 0.25mol/L ammonium fluoride solution containing 0.5g PEG-6000 was added and allowed to stand for 24h. The product was separated by centrifugation, the precipitate was washed with distilled water and ethanol in sequence, and the resulting precipitate was vacuum-dried at room temperature to obtain a white powder, namely α-PbF 2 Nano stave. Products of similar size and shape are also obtained. (See Figure 3-4(a)).

Example Embodiment

[0055] Example 2. α-PbF 2 Preparation of nanosheets
[0056] Example 2-1 After successively adding 50ml cyclohexane, 10ml OP emulsifier (TRITONXT-10), 6ml n-pentanol, 10ml 0.1mol/L lead acetate aqueous solution to a 100ml round bottom flask, the system was placed in a new In the JY92-2D ultrasonic instrument produced by Zhike Instrument Research Institute, at room temperature and normal pressure, the power was set to 600W, and the quaternary emulsion was prepared by ultrasonication for 10 minutes. Then, add 20 ml of 0.1 mol/L ammonium fluoride solution containing 1.0 g of PVP-K30, set the power to 400 W, continue ultrasonication for 5 min, and let stand for 1 h. The product was separated by centrifugation, the precipitate was washed with distilled water and ethanol in sequence, and the resulting precipitate was vacuum-dried at room temperature to obtain a white powder, namely α-PbF 2Nanosheets. Powder XRD results show that it is pure orthorhombic α-PbF2. The positions and intensities of the peaks matched literature values ​​[Ref: Joint Committee on Powder Diffraction Standards (JCPDS), File No 06-0288.]. No heterogeneous peaks were found, indicating that the purity of the product is relatively high. PbF was observed by TEM and SEM 2 Nanosheet: 100-200nm thick, 1200-1500nm long on the first side, and 1200-2500nm long on the second side (see Figure 3-1(b)).
[0057] Example 2-2 Add 50ml of cyclohexane, 10ml of OP emulsifier (TRITONXT-10), 6ml of n-pentanol, and 10ml of 0.25mol/L lead acetate aqueous solution to a 100ml round-bottomed flask, and place the system in a new In the JY92-2D ultrasonic instrument produced by Zhike Instrument Research Institute, at room temperature and normal pressure, the power was set to 600W, and the quaternary emulsion was prepared by ultrasonication for 10 minutes. Then, add 25 ml of 0.2 mol/L ammonium fluoride solution containing 2.0 g of PVP-K30, set the power to 400 W, continue ultrasonication for 5 min, and let stand for 1 h. The product was separated by centrifugation, the precipitate was washed with distilled water and ethanol in sequence, and the resulting precipitate was vacuum-dried at room temperature to obtain a white powder, namely PbF 2 Nanosheets. Products of similar size and shape were also obtained (see Figure 3-2(b)).
[0058] Example 2-3 Add 50ml of cyclohexane, 10ml of OP emulsifier (TRITONXT-10), 6ml of n-pentanol, and 5ml of 0.5mol/L lead acetate aqueous solution to a 100ml round-bottomed flask, and place the system in Ningbo, Zhejiang In the JY92-2D ultrasonic instrument produced by Zhike Instrument Research Institute, at room temperature and normal pressure, the power was set to 600W, and the quaternary emulsion was prepared by ultrasonication for 10 minutes. Then, add 5ml of 1.0mol/L ammonium fluoride solution and continue to sonicate for 20min, and let stand for 1h. The product was separated by centrifugation, the precipitate was washed with distilled water and ethanol in sequence, and the resulting precipitate was vacuum-dried at room temperature to obtain a white powder, namely α-PbF 2 Nanosheets. Products of similar size and shape were also obtained (see Figure 3-3(b)).
[0059] Example 2-4 After successively adding 50ml cyclohexane, 10ml OP emulsifier (TRITONXT-10), 6ml n-pentanol, 6ml 1.0mol/l ammonium fluoride aqueous solution into a 100ml round bottom flask, the system was placed in Zhejiang In the JY92-2D ultrasonic instrument produced by Ningbo Xinzhike Instrument Research Institute, at room temperature and normal pressure, the power was set to 600W, and the quaternary emulsion was prepared by ultrasonication for 10 minutes. Then, add 6ml of 0.5mol/L lead acetate solution and continue to sonicate for 20min, and let it stand for 1h. The product was separated by centrifugation, the precipitate was washed with distilled water and ethanol in sequence, and the resulting precipitate was vacuum-dried at room temperature to obtain a white powder, namely PbF 2 Nanosheets. Products of similar size and shape were also obtained (see Fig. 3-4(b)).

Example Embodiment

[0060] Example 3. α-PbF 2 Preparation of nanoribbons
[0061] Example 3-1 Add 50ml of cyclohexane, 7ml of OP emulsifier (TRITONXT-10), 4ml of n-pentanol, and 5ml of 0.5mol/L lead acetate aqueous solution to a 100ml round-bottomed flask, and place the system in Ningbo, Zhejiang Quaternary Emulsion A was prepared in JY92-2D Ultrasonic Apparatus produced by Zhike Institute, at room temperature and normal pressure, with the power set at 600W, and ultrasonication for 10 minutes.
[0062] Add 50ml of cyclohexane, 7ml of OP emulsifier (TRITON XT-10), 4ml of n-pentanol, and 5ml of 1.0mol/L ammonium fluoride aqueous solution into a 100ml round-bottomed flask, and place the system in Xinzhi, Ningbo, Zhejiang Quaternary Emulsion B was prepared in JY92-2D Ultrasonic Apparatus produced by Keqi Research Institute, at room temperature and pressure, with the power set at 600W, and ultrasonication for 10 minutes.
[0063] Put the prepared quaternary emulsion A and the prepared quaternary emulsion B into a 200ml beaker and let stand for 2h. The product was separated by centrifugation, the precipitate was washed with distilled water and ethanol in sequence, and the resulting precipitate was vacuum-dried at room temperature to obtain a white powder, namely α-PbF 2 Nanostrips. Powder XRD results show that it is pure orthorhombic α-PbF2. The positions and intensities of the peaks matched literature values. No heterogeneous peaks were found, indicating that the purity of the product is relatively high. PbF was observed by TEM and SEM 2 Nanostripes: 100-160nm thick, 500-1000nm wide, 4500-20000nm long (see Figure 3-1(c)).
[0064] Example 3-2 Add 50ml of cyclohexane, 10ml of OP emulsifier (TRITONXT-10), 6ml of n-pentanol, and 5ml of 0.50mol/L lead acetate aqueous solution to a 100ml round-bottomed flask, and place the system in a new Quaternary Emulsion A was prepared in JY92-2D Ultrasonic Apparatus produced by Zhike Institute, at room temperature and normal pressure, with the power set at 600W, and ultrasonication for 10 minutes.
[0065] Add 50ml of cyclohexane, 10ml of OP emulsifier (TRITON XT-10), 6ml of n-pentanol, and 5ml of 1.0mol/L ammonium fluoride aqueous solution into a 100ml round-bottomed flask, and place the system in Xinzhi, Ningbo, Zhejiang Quaternary Emulsion B was prepared in JY92-2D Ultrasonic Apparatus produced by Keqi Research Institute, at room temperature and pressure, with the power set at 600W, and ultrasonication for 10 minutes.
[0066] Put the prepared quaternary emulsion A and the prepared quaternary emulsion B into a 200ml beaker and let stand for 6h. The product was separated by centrifugation, the precipitate was washed with distilled water and ethanol in sequence, and the resulting precipitate was vacuum-dried at room temperature to obtain a white powder, namely PbF 2 Nanostrips. Products of similar size and shape were also obtained (see Figure 3-2(c)).
[0067] Example 3-3 Add 50ml of cyclohexane, 7ml of OP emulsifier (TRITONXT-10), 4ml of n-pentanol, and 5ml of 0.25mol/L lead acetate aqueous solution to a 100ml round-bottomed flask, and place the system in Ningbo, Zhejiang Quaternary Emulsion A was prepared in JY92-2D Ultrasonic Apparatus produced by Zhike Institute, at room temperature and normal pressure, with the power set at 600W, and ultrasonication for 10 minutes.
[0068] Add 50ml cyclohexane, 10ml OP emulsifier (TRITON XT-10), 6ml n-pentanol, 5ml 0.5mol/L ammonium fluoride aqueous solution to a 100mL round-bottomed flask, and place the system in Xinzhi, Ningbo, Zhejiang Quaternary Emulsion B was prepared in JY92-2D Ultrasonic Apparatus produced by Keqi Research Institute, at room temperature and pressure, with the power set at 600W, and ultrasonication for 10 minutes.
[0069] Put the prepared quaternary emulsion A and the prepared quaternary emulsion B into a 200ml beaker and let stand for 6h. The product was separated by centrifugation, the precipitate was washed with distilled water and ethanol in sequence, and the resulting precipitate was vacuum-dried at room temperature to obtain a white powder, namely PbF 2 Nanostrips. Products of similar size and shape were also obtained (see Fig. 3-3(c)).
[0070] Example 3-4 After successively adding 50ml cyclohexane, 10ml OP emulsifier (TRITONXT-10), 6ml n-pentanol, 5ml 0.25mol/L lead acetate aqueous solution into a 100ml round bottom flask, the system was placed in a new Quaternary Emulsion A was prepared in JY92-2D Ultrasonic Apparatus produced by Zhike Institute, at room temperature and normal pressure, with the power set at 600W, and ultrasonication for 10 minutes.
[0071] Add 50ml of cyclohexane, 10ml of OP emulsifier (TRITON XT-10), 6ml of n-pentanol, and 5ml of 0.5mol/L ammonium fluoride aqueous solution to a 100ml round-bottomed flask, and place the system in Xinzhi, Ningbo, Zhejiang. Quaternary Emulsion B was prepared in JY92-2D Ultrasonic Apparatus produced by Keqi Research Institute, at room temperature and pressure, with the power set at 600W, and ultrasonication for 10 minutes. Put the prepared quaternary emulsion A and the prepared quaternary emulsion B into a 200mL beaker and let it stand for 2h. The product was separated by centrifugation, the precipitate was washed with distilled water and ethanol in sequence, and the resulting precipitate was vacuum-dried at room temperature to obtain a white powder, namely α-PbF 2 Nanostrips. Products of similar size and shape were also obtained (see Fig. 3-4(c)).

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