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Method for synthesizing large-size lead telluride monocrystalline thermovoltaic material

A synthesis method and technology of lead telluride, applied in polycrystalline material growth, chemical instruments and methods, single crystal growth, etc. Micron, nanometer level and other issues, to achieve the effect of low loss, high conversion efficiency and stable performance

Inactive Publication Date: 2018-07-20
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing lead telluride is generally a polycrystalline material, and there is no lead telluride single crystal thermovoltaic material that can be applied on a large scale, which cannot meet the quality requirements of the ever-growing science and technology for thermovoltaic materials
In recent years, although the research on lead telluride single-crystal thermovoltaic materials has been reported, single-crystal thermovoltaic materials are still mainly focused on the growth process and photoelectric properties of nanorods, nanocrystals, nanowires, thin films and other small-scale materials. , the size of the single crystal thermovoltaic materials involved is only micron or nanometer level, and there is no report on the performance parameters of single crystal thermovoltaic materials

Method used

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  • Method for synthesizing large-size lead telluride monocrystalline thermovoltaic material
  • Method for synthesizing large-size lead telluride monocrystalline thermovoltaic material
  • Method for synthesizing large-size lead telluride monocrystalline thermovoltaic material

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Embodiment 1

[0045] In this embodiment, the high-temperature solid-phase reaction method uses the same process to prepare lead telluride polycrystalline positive and negative thermal volt materials.

[0046] Attached figure 2 The best process for preparing lead telluride polycrystalline positive and negative thermovoltaic materials by high-temperature solid-phase reaction method is given: the first heating section starts from room temperature, and after 8 hours, the temperature is increased to 500°C, and then enters the first constant temperature. After keeping it for 24 hours, it enters the second heating section, which takes 24 hours to raise the temperature to 1000°C, and then enters the second constant temperature section. The polycrystalline lead telluride positive electrode and negative electrode thermal volt materials were obtained respectively.

Embodiment 2

[0048] In this embodiment, the high-temperature solid-phase reaction method uses the same process to prepare lead telluride polycrystalline positive and negative thermal volt materials.

[0049] Attached image 3 Gives another best synthesis process for preparing lead telluride polycrystalline positive and negative thermovoltaic materials by high-temperature solid-phase reaction: the first heating stage starts from room temperature, and after 5 hours, the temperature is raised to 480°C, and then enters The first constant temperature section is kept for 20 hours, and then it enters the second temperature rise section, which takes 30 hours to heat up to 950°C, and then enters the second constant temperature section when the temperature is reached. After 30 hours of heat preservation, it enters the temperature drop section and cools to 150°C / hour. At room temperature, the polycrystalline lead telluride positive electrode and negative electrode thermal volt materials were obtained res...

Embodiment 3

[0054] See attached Figure 5 .

[0055] In this embodiment, the same process is used to make large-size lead telluride single crystal positive and negative thermal volt materials.

[0056] The polycrystalline positive electrode and negative electrode thermal source materials prepared in Example 1 were respectively packed into large-size quartz growth ampoules with an inner diameter of 50 mm and a length of 350 mm. After the temperature rises, the high temperature zone is around 1010°C, and the gradient zone drops from 1010°C to around 830°C, and then maintains around 830°C. During operation, first place the bottom end of the growth ampoule at 45cm in the furnace. After 50 hours of rest, slowly lower the growth ampoule at a rate of 0.5mm / hour. When the bottom end of the quartz ampoule reaches 75cm, stop the drop and take out the growth ampoule by cooling down. , To obtain large-size lead telluride single crystal positive and negative thermal volt materials. The lead telluride sin...

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Abstract

The invention relates to a method for synthesizing a large-size lead telluride monocrystalline thermovoltaic material. According to the method, elemental tellurium and lead are served as raw materials, lead telluride polycrystalline positive and negative thermovoltaic materials are prepared firstly, and then, the large-size lead telluride thermovoltaic material is synthesized. During the preparation of the polycrystalline positive and negative thermovoltaic materials, the stoichiometric ratio of lead and the stoichiometric ratio of tellurium are 0.99: 1 and 1: 0.998 separately. During the synthesis of lead telluride, the polycrystalline positive and negative thermovoltaic materials are separately loaded into a large-size quartz growth ampule, and the large-size quartz growth ampule is vacuumized and sealed and then placed into a growth furnace. The bottommost end of the growth ampule is placed at a position of 30cm to 50cm of the furnace firstly, is slowly lowered at a rate of 0.3mm / hto 0.5mm / h after 30 to 50 hours of standing, is stopped lowering until the bottommost end of the quartz ampule reaches a position of 60cm to 80cm and is cooled, the growth ampule is taken out, the growth ampule goes through a high-temperature area, a gradient area and a low-temperature area along with change of a furnace-inside position, and the temperature range is 830 DEG C to 1,020 DEG C. According to the method, the blank in the prior art that lead telluride monocrystalline thermovoltaic materials cannot be produced in a large-size and large-scale manner is filled up. The product performance is stable and reliable, and the thermoelectric figure of merit (ZT value) reaches up to 1 or more.

Description

Technical field [0001] The invention belongs to the category of compound synthesis, and relates to a lead telluride thermoelectric single crystal synthesis, in particular to a large-size lead telluride thermoelectric material synthesis method. Background technique [0002] As a new compound semiconductor material, lead telluride is used in many high-tech fields, such as thermoelectric field, with its excellent characteristics. However, the existing lead telluride is generally a polycrystalline material, and there is no single crystal lead telluride thermovoltaic material that can be applied on a large scale, which cannot meet the quality requirements of the increasingly developed science and technology for thermovoltaic materials. In recent years, although research on lead telluride single crystal thermovoltaic materials has been reported, single crystal thermovoltaic materials are mainly focused on the growth process and photoelectric performance of small-sized materials such as...

Claims

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Application Information

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IPC IPC(8): C30B29/46C30B28/02C30B11/02
CPCC30B11/02C30B28/02C30B29/46
Inventor 昂然唐明静尹聪刘航天康彬
Owner SICHUAN UNIV
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