Selenium bismuth oxide compound as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of materials, and particularly relates to a selenium bismuth oxide compound and a preparation method and application thereof. The chemical formula of the selenium bismuth oxide compound is Bi18SeO29, and the molecular weight of the selenium bismuth oxide compound is 4304.6. The invention also provides a preparation method and application of the selenium bismuth oxide compound. The selenium bismuth oxide compound provided by the invention has good optical properties, excellent stability and low thermal conductivity, and the preparation method is simple, easy to form and process, low in cost and convenient for large-scale production and application.

Description

Technical Field

[0001] The invention belongs to the technical field of materials, and in particular relates to a bismuth selenium oxide compound and a preparation method and application thereof. Background Art

[0002] In modern optical technology, controlling and modulating the intensity, phase, frequency and other characteristics of light is crucial for many applications. Especially in the field of lasers, the modulation of laser pulses and the generation of ultrashort pulses rely on efficient and reliable optical materials. Among them, saturable absorbers have become key materials for realizing these functions due to their unique nonlinear optical properties.

[0003] A saturated absorber is an optical material with nonlinear absorption properties. When the incident light intensity is low, the saturated absorber has a high absorption coefficient and absorbs the photons entering the laser cavity, suppressing laser oscillation. When the incident light intensity increases to a certain level, the absorption coefficient of the saturated absorber decreases and the transmittance increases significantly, allowing laser photons to accumulate rapidly in the laser cavity, ultimately generating strong laser pulses.

[0004] Although existing saturable absorber materials have made significant progress in many applications, there are still some problems and challenges. For example, organic dye-based saturable absorbers are prone to degradation during long-term use, resulting in performance degradation. The high manufacturing cost of some high-performance materials limits their large-scale application. Summary of the invention

[0005] In order to solve the problems existing in the prior art, the present invention provides a selenium bismuth oxide compound, which can be used as an optical material due to its excellent stability, low thermal conductivity, high temperature stability and other characteristics.

[0006] One of the technical solutions provided by the present invention is: a selenium bismuth oxide compound, the chemical formula of which is Bi 18 SeO 29 , molecular weight is 4304.6.

[0007] The present invention also provides a preparation method of the bismuth selenium oxide compound, comprising the following steps: mixing Bi2O3 and Bi2Se3 raw materials evenly, putting them into a crucible, and then putting the crucible into a chemical vapor deposition reaction chamber or a muffle furnace, and obtaining the bismuth selenium oxide compound after chemical vapor deposition or high-temperature calcination treatment.

[0008] Preferably, the chemical vapor deposition processing method is: use argon gas for multiple purges; after the purge is completed, oxygen and argon are used as carrier gases with flow rates of 15 sccm and 100 sccm respectively, and the chemical vapor deposition temperature is increased to 750°C at 5°C / min, and after keeping warm for 2.5 hours, it is cooled to room temperature.

[0009] Preferably, the high temperature calcination treatment method is: starting temperature 22°C, heating rate 4°C / min, heating to 750°C, keeping time 10h, cooling rate 1.25°C / min, cooling to room temperature.

[0010] Preferably, the purity of Bi2O3 and Bi2Se3 is 99.99%.

[0011] Preferably, in the chemical vapor deposition process, the molar ratio of Bi2O3 to Bi2Se is 7-8:1.

[0012] Preferably, during the high temperature calcination treatment, the molar ratio of Bi2O3 to Bi2Se3 is 21-22:1.

[0013] The present invention further provides a use of the bismuth selenium oxide compound, wherein the bismuth selenium oxide compound is used as an optical material to realize the modulation or generation of laser pulses.

[0014] Preferably, the bismuth selenium oxide compound is used as a low thermal conductivity material in materials science, chemical engineering or mechanical engineering.

[0015] The bismuth selenium oxide compound provided by the present invention has good optical properties, excellent stability, and low thermal conductivity, and the preparation method is simple, easy to shape and process, low cost, and convenient for large-scale production and application. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 is the XRD spectrum of the bismuth selenium oxide compound powder prepared in Example 1; Figure 2 This is a physical picture of the bismuth selenium oxide compound powder prepared in Example 1; Figure 3 is a crystal photograph (micrometer scale) of the bismuth selenium oxide compound prepared in Example 1; Figure 4 is the absorption spectrum of the bismuth selenium oxide compound prepared in Example 1; Figure 5 This is a diagram of the experimental setup of a 1-micron passive Q-switched laser using the bismuth selenium oxide saturable absorber prepared in Example 1. (Inset: actual image) From left to right are the fiber-coupled 808nm semiconductor laser, coupling lens, input mirror, Nd:YAG, Bi 18 SeO 29 , and output mirror; Figure 6 is the variation of the average output power of the passively Q-switched laser with the pump power in Example 1; Figure 7 is the relationship between the passive Q-switched laser pulse width and repetition frequency and the pump power in Example 1; Figure 8 is the variation of the single pulse energy and peak power of the passively Q-switched laser with the pump power in Example 1; Fig. 9 The passive Q-switched laser single pulse shape and sequence in Example 1; Fig.10 is the thermal conductivity of the bismuth selenium oxide compound prepared in Example 1; Fig.11 is the Seebeck coefficient of the bismuth selenium oxide compound prepared in Example 1; Fig.12 is the XRD spectrum of the bismuth selenium oxide compound powder prepared in Example 2; Fig.13 This is a physical picture of the selenium bismuth oxide compound powder prepared in Example 2. DETAILED DESCRIPTION

[0017] The present invention is further described below in conjunction with specific embodiments and the accompanying drawings. More details are set forth in the following description to facilitate a full understanding of the present invention. However, the present invention is obviously capable of being implemented in a variety of other ways different from the description herein. For those skilled in the art, any substitution, improvement or change made to the embodiments of the present invention is within the protection scope of the present invention, and the protection scope of the present invention should not be limited by the content of this specific embodiment.

[0018] Example 1 The bismuth selenium oxide compound provided in this example is prepared by the following method: (a) Bi2O3 and Bi2Se3 raw materials with a molar ratio of 21:1 are mixed evenly and placed in a corundum crucible, and then the corundum crucible with a cover is placed in a muffle furnace; (b) Program settings: starting temperature 22 °C, heating rate 4 °C / min, heating to 750 °C, holding time 10 h, cooling rate 1.25 °C / min, cooling to 22 °C to obtain Bi 18 SeO 29 powder.

[0019] In this embodiment, the purity of Bi2O3 is 99.99%, and the purity of Bi2Se3 is 99.99%. The prepared bismuth selenium oxide compound has the chemical formula Bi 18 SeO 29 , molecular weight 4304.6, which is a yellow opaque pure sample of bismuth selenium oxide, such as Figure 1 , 2 , 3, and 4.

[0020] The bismuth selenium oxide prepared in this example is used as a saturable absorber to conduct a passive Q-switched laser experiment. The experimental device is as follows: Figure 5As shown, from left to right are fiber-coupled 808nm semiconductor laser, coupling lens, input mirror, Nd:YAG, Bi 18 SeO 29 , and output mirror.

[0021] like Figure 6 As shown, in the CW laser operation stage, the output power is almost linearly related to the pump power.

[0022] like Figure 7 As shown in Figure 2, with the continuous increase of incident pump power, Bi 18 SeO 29 The pulse width was reduced from 673.2ns to 424.8ns, and the repetition rate was increased from 101.6kHz to 234.3kHz. At a pump power of 2.04W, the shortest pulse width of 424.8ns was obtained.

[0023] like Figure 8 As shown in Figure 5, with the increase of pump power, the single pulse energy increases from 39.3 nJ to 136.6 nJ, and the peak power increases from 6 mW to 32 mW.

[0024] Passively Q-switched laser single pulse shape and sequence Fig. 9 shown.

[0025] The thermal conductivity of the bismuth selenium oxide compound prepared in this example is as follows Fig.10 As shown, the test temperature range is 400~600℃, and the thermal conductivity increases slightly with increasing temperature.

[0026] Example 2 The bismuth selenium oxide compound provided in this example is prepared by the following method: (a) Bi2O3 and Bi2Se3 raw materials with a molar ratio of 8:1 were mixed evenly and placed in a quartz crucible, and then the quartz crucible was placed in a chemical vapor deposition (CVD) process and purged three times with argon gas; (b) Program setting: After the purge, oxygen and argon were used as carrier gases with flow rates of 20 sccm and 100 sccm respectively. Chemical vapor deposition (CVD) was heated to 750°C at 5°C / min. After being kept at this temperature for 2 h, the temperature was cooled to room temperature to obtain bismuth selenium oxide. The sample was taken out and ground in a mortar to obtain Bi 18 SeO 29 powder.

[0027] In this embodiment, the purity of Bi2O3 is 99.99%, the purity of Bi2Se3 is 99.99%, and the purity of O2 is 99.999%.

[0028] The bismuth selenium oxide compound prepared in this example is a white powder, and its XRD spectrum is as follows: Fig.12As shown in the actual picture Fig.13 shown.

Claims

1. A bismuth selenium oxide compound, characterized in that: The chemical formula of this compound is Bi 18 SeO 29 , molecular weight is 4304.

6.

2. The method for preparing the bismuth selenium oxide compound according to claim 1, characterized in that: The method comprises the following steps: mixing Bi2O3 and Bi2Se3 raw materials uniformly, putting the materials into a crucible, and then putting the crucible into a chemical vapor deposition reaction chamber or a muffle furnace, and obtaining a selenium bismuth oxide compound after chemical vapor deposition or high-temperature calcination.

3. The method for preparing the bismuth selenium oxide compound according to claim 2, characterized in that: The chemical vapor deposition treatment method is: use argon gas for multiple purges; after the purge is completed, oxygen and argon are used as carrier gases with flow rates of 15 sccm and 100 sccm respectively, and the chemical vapor deposition temperature is increased to 750°C at 5°C / min, and after keeping warm for 2.5 hours, it is cooled down to room temperature.

4. The method for preparing the bismuth selenium oxide compound according to claim 2, characterized in that: The high temperature calcination treatment method is: starting temperature 22°C, heating rate 4°C / min, heating to 750°C, holding time 10h, cooling rate time 1.25°C / min, cooling to room temperature.

5. The method for preparing the bismuth selenium oxide compound according to claim 2, characterized in that: In the chemical vapor deposition process, the molar ratio of Bi2O3 to Bi2Se is 7-8:

1.

6. The method for preparing the bismuth selenium oxide compound according to claim 2, characterized in that: In the high temperature calcination treatment, the molar ratio of Bi2O3 to Bi2Se3 is 21-22:

1.

7. The method for preparing the bismuth selenium oxide compound according to any one of claims 2 to 6, characterized in that: The purity of Bi2O3 and Bi2Se3 is 99.99%.

8. The use of the bismuth selenium oxide compound according to claim 1, characterized in that: The bismuth selenium oxide compound is used as a saturable absorber optical material to achieve modulation or generation of laser pulses.

9. The use of the bismuth selenium oxide compound according to claim 1, characterized in that: The bismuth selenium oxide compound is used as a low thermal conductivity material in materials science, chemical engineering or mechanical engineering.

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