Nanoscale black phosphorus as well as preparation method and application thereof

Abstract

The invention provides nanoscale black phosphorus as well as a preparation method and application thereof. The preparation method comprises the following steps that in protective gas, adding bulk red phosphorus of which the dimension is greater than 0.1cm and stainless steel balls of which the diameters are 6mm-12mm to a high energy ball milling pot in the mass ratio of the bulk red phosphorus to the stainless steel balls being 1 to (20-60), performing sealing, and then performing a ball milling reaction, so as to prepare the nanoscale black phosphorus. The temperature of the ball milling reaction is from room temperature to 60 DEG C, the ball milling rotational speed is 1100r / min-1500r / min, and the ball milling time is 2h-8h. The invention further provides the nanoscale black phosphorus prepared by the preparation method, the particle diameters of the nanoscale black phosphorus are 1nm-5nm. The invention further provides an application of the nanoscale black phosphorus in photoelectric devices, solar batteries, lithium batteries and biomedical science.

Description

technical field

[0001] The invention belongs to the field of novel nanomaterials, and relates to a nanoscale black phosphorus and its preparation method and application, in particular to a method for efficiently and rapidly converting large-scale preparation of nanoscale black phosphorus. Background technique

[0002] Black phosphorus, as the most stable of phosphorus allotropes, is a semiconductor with a natural wrinkled layered structure. This unique wrinkled structure endows black phosphorus with many unique physical and chemical properties, such as black phosphorus has a direct band gap, Possesses electron mobility beyond that of transition metals, up to 1,000cm 2 ·V -1 ·s -1 , and its spectral range covers the entire visible and near-infrared regions. Therefore, black phosphorus has broad application prospects in the fields of optoelectronic devices, sensors, biomedicine, solar cells, and lithium batteries. Especially nano-scale black phosphorus (usually <100nm), ...

Examples

Embodiment 1

[0046] The present embodiment provides a kind of preparation method of nanoscale black phosphorus, it comprises the following steps:

[0047] Weigh 5 grams of red phosphorus blocks with a size of 0.1-0.3 cm in an argon-filled glove box, fill them with stainless steel balls with a diameter of 10 mm in a mass ratio of 1:20 into a 50 ml high-energy ball mill jar and Seal; the high-energy ball mill jar is placed in the high-energy ball mill, and the highest temperature is set to 60 degrees Celsius, the lowest temperature is set to 25 degrees Celsius, and then ball milled at 1500r / min for 2 hours to obtain 4.92 grams of nano-scale black phosphorus.

[0048] The nano-scale black phosphorus prepared in this embodiment is characterized, and compared with the red phosphorus raw material, the results are as follows Figure 1A-Figure 2B As shown, among them, Figure 1A and Figure 1B Respectively show the XRD figure of red phosphorus raw material and the black phosphorus that the presen...

Embodiment 2

[0050] The present embodiment provides a kind of preparation method of nanoscale black phosphorus, it comprises the following steps:

[0051] Weigh 3 grams of red phosphorus blocks with a size of 0.3-0.6 cm in an argon-filled glove box, fill them with stainless steel balls with a diameter of 10 mm in a mass ratio of 1:60 into a 50 ml high-energy ball mill jar and Seal; the high-energy ball mill jar is placed in a high-energy ball mill, and the highest temperature is set to 40 degrees Celsius, and the lowest temperature is set to 25 degrees Celsius, and then ball milled at 1200r / min for 5 hours to obtain 2.95 grams of nano-scale black phosphorus.

[0052] The nanoscale black phosphorus that present embodiment is made characterizes, and its result is as follows image 3 as shown, image 3 The Raman spectrum in shows that after the red phosphorus is ball-milled by the method of this example, the Raman peak at 390 wavenumber completely disappears, and a new Raman peak appears at ...

Embodiment 3

[0054] The present embodiment provides a kind of preparation method of nanoscale black phosphorus, it comprises the following steps:

[0055] Weigh 5 grams of red phosphorus blocks with a size of 0.3-0.6 cm in an argon-filled glove box, fill them with stainless steel balls with a diameter of 12 mm in a mass ratio of 1:30 into a 50 ml high-energy ball mill jar and Sealing; the high-energy ball mill jar is placed in the high-energy ball mill, and the highest temperature is set to 45 degrees Celsius, the lowest temperature is set to 25 degrees Celsius, and then ball milled at 1300r / min for 3.5 hours to obtain 4.96 grams of nano-scale black phosphorus.

[0056] The nanoscale black phosphorus that present embodiment is made characterizes, and its result is as follows Figure 4 , Figure 5 as shown, Figure 4 The Raman spectrum in shows that after the red phosphorus is ball-milled by the method of this example, the Raman peak at 390 wavenumber completely disappears, and a new Rama...

technical field

[0001] The invention belongs to the field of novel nanomaterials, and relates to a nanoscale black phosphorus and its preparation method and application, in particular to a method for efficiently and rapidly converting large-scale preparation of nanoscale black phosphorus. Background technique

[0002] Black phosphorus, as the most stable of phosphorus allotropes, is a semiconductor with a natural wrinkled layered structure. This unique wrinkled structure endows black phosphorus with many unique physical and chemical properties, such as black phosphorus has a direct band gap, Possesses electron mobility beyond that of transition metals, up to 1,000cm 2 ·V -1 ·s -1 , and its spectral range covers the entire visible and near-infrared regions. Therefore, black phosphorus has broad application prospects in the fields of optoelectronic devices, sensors, biomedicine, solar cells, and lithium batteries. Especially nano-scale black phosphorus (usually <100nm), ...

Examples

Embodiment 1

[0046] The present embodiment provides a kind of preparation method of nanoscale black phosphorus, it comprises the following steps:

[0047] Weigh 5 grams of red phosphorus blocks with a size of 0.1-0.3 cm in an argon-filled glove box, fill them with stainless steel balls with a diameter of 10 mm in a mass ratio of 1:20 into a 50 ml high-energy ball mill jar and Seal; the high-energy ball mill jar is placed in the high-energy ball mill, and the highest temperature is set to 60 degrees Celsius, the lowest temperature is set to 25 degrees Celsius, and then ball milled at 1500r / min for 2 hours to obtain 4.92 grams of nano-scale black phosphorus.

[0048] The nano-scale black phosphorus prepared in this embodiment is characterized, and compared with the red phosphorus raw material, the results are as follows Figure 1A-Figure 2B As shown, among them, Figure 1A and Figure 1B Respectively show the XRD figure of red phosphorus raw material and the black phosphorus that the presen...

Embodiment 2

[0050] The present embodiment provides a kind of preparation method of nanoscale black phosphorus, it comprises the following steps:

[0051] Weigh 3 grams of red phosphorus blocks with a size of 0.3-0.6 cm in an argon-filled glove box, fill them with stainless steel balls with a diameter of 10 mm in a mass ratio of 1:60 into a 50 ml high-energy ball mill jar and Seal; the high-energy ball mill jar is placed in a high-energy ball mill, and the highest temperature is set to 40 degrees Celsius, and the lowest temperature is set to 25 degrees Celsius, and then ball milled at 1200r / min for 5 hours to obtain 2.95 grams of nano-scale black phosphorus.

[0052] The nanoscale black phosphorus that present embodiment is made characterizes, and its result is as follows image 3 as shown, image 3 The Raman spectrum in shows that after the red phosphorus is ball-milled by the method of this example, the Raman peak at 390 wavenumber completely disappears, and a new Raman peak appears at ...

Embodiment 3

[0054] The present embodiment provides a kind of preparation method of nanoscale black phosphorus, it comprises the following steps:

[0055] Weigh 5 grams of red phosphorus blocks with a size of 0.3-0.6 cm in an argon-filled glove box, fill them with stainless steel balls with a diameter of 12 mm in a mass ratio of 1:30 into a 50 ml high-energy ball mill jar and Sealing; the high-energy ball mill jar is placed in the high-energy ball mill, and the highest temperature is set to 45 degrees Celsius, the lowest temperature is set to 25 degrees Celsius, and then ball milled at 1300r / min for 3.5 hours to obtain 4.96 grams of nano-scale black phosphorus.

[0056] The nanoscale black phosphorus that present embodiment is made characterizes, and its result is as follows Figure 4 , Figure 5 as shown, Figure 4 The Raman spectrum in shows that after the red phosphorus is ball-milled by the method of this example, the Raman peak at 390 wavenumber completely disappears, and a new Rama...

Images