阅读说明：本技术 一种非晶GeH的高压制备方法 (High-pressure preparation method of amorphous GeH ) 是由 李全军 荆晓玲 赵海洋 杜轶 刘冰冰 于 2019-12-02 设计创作，主要内容包括：本发明提供了一种非晶GeH的制备方法,属于非晶GeH制备技术领域。本发明提供的制备方法,包括以下步骤：将晶体GeH、压力标定物和传压介质密封在金刚石对顶砧压机的腔体内,调节腔体内的压力,得到非晶GeH。本发明在密封的金刚石对顶砧压机中,对GeH施加压力,使GeH的非晶化过程在室温条件下能够实现,且在制备过程中不易引入杂质,能够获得纯净的非晶态GeH。且本发明提供的方法操作简单,重复性好。(The invention provides a preparation method of amorphous GeH, belonging to the technical field of amorphous GeH preparation. The preparation method provided by the invention comprises the following steps: and sealing the crystal GeH, the pressure calibration material and the pressure transmission medium in a cavity of the diamond anvil cell pressing machine, and adjusting the pressure in the cavity to obtain the amorphous GeH. In the invention, pressure is applied to GeH in a sealed diamond anvil cell press, so that the GeH non-crystallization process can be realized at room temperature, impurities are not easy to introduce in the preparation process, and pure amorphous GeH can be obtained. The method provided by the invention is simple to operate and good in repeatability.)

1. The high-pressure preparation method of amorphous GeH is characterized by comprising the following steps:

and sealing the crystal GeH, the pressure calibration material and the pressure transmission medium in a cavity of the diamond anvil cell pressing machine, and adjusting the pressure in the cavity to obtain the amorphous GeH.

2. The method of claim 1, wherein the adjusting the pressure in the chamber is accomplished by adjusting a compression screw of a diamond anvil press.

3. The method according to claim 2, wherein the pressing speed of the pressing screw is 0.2-0.5 GPa/min.

4. The production method according to claim 1 or 2, wherein the pressure is 0.5 to 40 GPa.

5. The method according to claim 1, wherein the diameter of the anvil surface of the diamond anvil cell press is 300 to 400 μm.

6. The method of claim 1, wherein the cavity of the diamond anvil cell press has a diameter of 130 to 150 μm and a height of 40 to 60 μm.

7. The method of manufacturing of claim 1, wherein the pad of the diamond anvil press is a T301 steel sheet.

8. The method according to claim 1, further comprising an X-ray diffraction of GeH and an in-situ detection of GeH amorphization during the preparation process.

Technical Field

The invention belongs to the technical field of amorphous GeH preparation, and particularly relates to a high-pressure preparation method of amorphous GeH.

Background

At present, most of various electronic devices use single crystal semiconductors, particularly single crystal silicon, as substrates. However, single crystal silicon has two significant disadvantages: firstly, the manufacturing process from growth to cutting, grinding and polishing of a wafer to becoming a device is quite complex, and the loss is large; secondly, the diameter of the silicon wafer is small, and the manufacture of large-area devices is difficult, while the amorphous semiconductor can just solve the problems.

Currently, the most studied amorphous semiconductors fall into two categories: one is a chalcogenide amorphous semiconductor; another class is group IV semiconductors such as amorphous silicon. The amorphous silicon solar cell is the most widely applied field of amorphous silicon at present, compared with the crystalline silicon solar cell, the amorphous silicon solar cell has the advantages of less raw material loss, relatively simple process and relatively low price, and when the amorphous GeH is used as a solar cell material, the conversion efficiency of the solar cell can be effectively improved.

The traditional method for synthesizing amorphous GeH generally comprises the steps of heating GeH for more than 4 hours at 75-175 ℃ in argon, carrying out non-crystallizing treatment, and naturally cooling to room temperature to obtain an amorphous GeH sample. However, the method is long in time consumption and high in cost, is not energy-saving and environment-friendly, and impurities are easily introduced due to impure argon in the preparation process of the amorphous GeH.

Disclosure of Invention

In view of the above, the present invention is directed to a method for preparing amorphous GeH, which is short in time consumption, capable of amorphizing GeH at room temperature, and less prone to impurity introduction during the preparation process.

In order to achieve the purpose, the invention provides the following technical scheme:

the invention provides a high-pressure preparation method of amorphous GeH, which comprises the following steps:

and sealing the crystal GeH, the pressure calibration material and the pressure transmission medium in a cavity of the diamond anvil cell pressing machine, and adjusting the pressure in the cavity to obtain the amorphous GeH.

Preferably, the pressure in the adjusting cavity is realized by adjusting a pressurizing screw of the diamond anvil cell press.

Preferably, the pressurizing speed of the pressurizing screw is 0.2-0.5 GPa/min.

Preferably, the pressure is 0.5-40 GPa.

Preferably, the diameter of the anvil surface of the diamond anvil cell press is 300-400 μm.

Preferably, the diameter of the cavity of the diamond anvil cell press is 130-150 μm, and the height of the cavity is 40-60 μm.

Preferably, the pad of the diamond anvil press is a T301 steel sheet.

Preferably, the method further comprises X-ray diffraction of GeH and in-situ detection of GeH amorphization process.

The invention provides a high-pressure preparation method of amorphous GeH, which comprises the following steps: and sealing the crystal GeH, the pressure calibration material and the pressure transmission medium in a cavity of the diamond anvil cell pressing machine, and adjusting the pressure in the cavity to obtain the amorphous GeH. The invention applies pressure to the crystal GeH in the sealed diamond anvil cell press, so that the non-crystallization process of the crystal GeH can be realized at room temperature, the preparation period is short, the prepared amorphous GeH is not easy to introduce impurities, pure amorphous GeH can be obtained, and the problems in the prior art can be effectively solved. The method provided by the invention is simple to operate and good in repeatability.

Drawings

FIG. 1 is an X-ray diffraction pattern of a GeH sample under different pressures;

FIG. 2 is an X-ray diffraction pattern of the amorphized GeH obtained in example 1 during pressure relief;

FIG. 3 is a selected area electron diffraction pattern of the amorphized GeH obtained in example 1;

FIG. 4 is a high resolution TEM photograph of the amorphized GeH obtained in example 1;

FIG. 5 is a high resolution TEM photograph of the amorphized GeH obtained in example 2.

Detailed Description

The invention provides a high-pressure preparation method of amorphous GeH, which comprises the following steps:

and sealing the crystal GeH, the pressure calibration material and the pressure transmission medium in a cavity of the diamond anvil cell pressing machine, and adjusting the pressure in the cavity to obtain the amorphous GeH. In the invention, the pressure calibration object is preferably ruby, the grain size of the ruby is preferably 10-20 microns, the using amount of the ruby is preferably 1-2, and the ruby is preferably placed at the edge in the cavity. In the invention, the grain size of the crystal GeH is preferably 100-110 μm, and the crystal GeH is preferably placed at the center in the cavity. The dosage of the crystal GeH is not specially limited, and the crystal GeH can be filled in a cavity of a diamond anvil cell press. In the present invention, the pressure transmission medium is preferably silicone oil, and the amount of the silicone oil is preferably 1 drop.

In the present invention, the diamond anvil press is preferably a symmetric Diamond Anvil Cell (DAC). In the invention, the diameter of the anvil surface of the diamond anvil cell press is preferably 300-400 μm; the diameter of a cavity of the diamond anvil cell press is preferably 130-150 micrometers, the height of the cavity is preferably 40-60 micrometers, and the center of the cavity is preferably formed by laser drilling; the pad of the diamond anvil press is preferably a T301 steel sheet. The invention adopts the T301 steel sheet as the sealing gasket, can generate hydrostatic pressure when raw materials are filled in the cavity, and has a protection effect on the diamond. The invention can generate higher pressure in the cavity by adopting the anvil surface of the diamond with a specific area. The invention is not particularly limited to the operation of the diamond anvil press, and may be performed in a manner well known to those skilled in the art.

In the invention, the pressure in the adjusting cavity is preferably realized by adjusting a pressurizing screw of the diamond anvil cell press, and the pressurizing speed of the pressurizing screw is preferably 0.2-0.5 GPa/min, more preferably 0.2-0.4 GPa/min, and even more preferably 0.2 GPa/min. The invention adopts specific pressurizing rate to uniformly and slowly apply pressure to the cavity of the anvil cell pressing machine by the diamond, and takes silicon oil as a pressure transmission medium to uniformly transmit the applied pressure to the crystal GeH, so that the non-crystallization process of the crystal GeH can be realized at room temperature, and the process is carried out under the sealing condition, and impurities are not easily introduced into the prepared amorphous GeH.

In the present invention, the pressure is preferably 0.5 to 40GPa, and more preferably 0.5 to 35 GPa. According to the invention, after initial pressure of 0.5-1 GPa is preferably applied to the cavity of the diamond anvil cell press, the pressure is uniformly applied to the pressure cavity by rotating the pressure screw of the diamond anvil cell press. According to the invention, the initial pressure of 0.5-1 GPa is applied to the cavity of the diamond anvil cell press, the viscosity of the silicone oil is increased, the silicone oil is completely solidified, and the crystal GeH, the ruby and the silicone oil are completely sealed in the cavity of the diamond anvil cell press.

The invention also includes the X-ray diffraction of GeH and the in-situ detection of the GeH amorphization process. The invention realizes the purpose of detecting the X-ray diffraction of the GeH and the amorphization process of the GeH on line by detecting the X-ray diffraction pattern of the GeH and the fluorescence pattern of the ruby changing along with the pressure in situ in the amorphization process.

The following will explain the preparation method of amorphous GeH provided by the present invention in detail with reference to the examples, but they should not be construed as limiting the scope of the present invention.