CN113023688B - Preparation method of arsenic-doped cadmium telluride - Google Patents
Preparation method of arsenic-doped cadmium telluride Download PDFInfo
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- CN113023688B CN113023688B CN202110445496.3A CN202110445496A CN113023688B CN 113023688 B CN113023688 B CN 113023688B CN 202110445496 A CN202110445496 A CN 202110445496A CN 113023688 B CN113023688 B CN 113023688B
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Abstract
The invention discloses a preparation method of arsenic-doped cadmium telluride. The preparation method of the arsenic-doped cadmium telluride comprises the following steps: and uniformly mixing the deoxidized cadmium telluride powder and the deoxidized cadmium arsenide powder, and carrying out hot-pressing sintering at 650-850 ℃ to obtain the arsenic-doped cadmium telluride, wherein the hot-pressing sintering is carried out under the protection of vacuum or protective gas. Cadmium telluride and cadmium arsenide are used as raw materials instead of corresponding simple substances, and hot-pressing sintering is carried out at a lower temperature, so that the raw materials are solid in the whole process, segregation is avoided, and the obtained arsenic-doped cadmium telluride material is ensured to have good uniformity; meanwhile, the deoxidized cadmium telluride powder and cadmium arsenide powder are used as raw materials, and hot-pressing sintering is carried out under the protection of vacuum or protective gas, so that the obtained arsenic-doped cadmium telluride material has low oxygen content and high purity.
Description
Technical Field
The invention relates to the field of preparation of solar materials, in particular to a preparation method of arsenic-doped cadmium telluride.
Background
With the increasing exhaustion of energy sources such as coal, petroleum, natural gas and the like and the increasing aggravation of environmental pollution, people are urgently required to find clean renewable new energy sources. The solar cell is used as an unlimited and renewable pollution-free energy source of the earth, and the solar cell is increasingly attracting attention, so that the solar cell can convert solar energy into electric energy, and the development of the solar cell is rapidly developed. At present, commercial crystalline silicon solar cells have the highest photoelectric conversion efficiency, but are limited by material purity and preparation process, so that the cost is high, and the conversion efficiency is difficult to improve or the cost is difficult to reduce.
The thin-film solar cell can realize photoelectric conversion only with the thickness of a few microns, and is an ideal material for reducing cost and improving photon circulation. CdTe (cadmium telluride) is not only a semiconductor having a bandgap width of 1.45 eV, but also can be expressed as > 5X 10 -4 cm -1 The CdTe doping can increase the hole (carrier) density, extend the carrier lifetime, and thus improve the power generation efficiency.
However, the currently obtained arsenic-doped cadmium telluride material with good uniformity, low oxygen content and high purity still remains an urgent technical problem to be solved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of arsenic-doped cadmium telluride, and the prepared arsenic-doped cadmium telluride has good uniformity, low oxygen content and high purity.
In order to realize the aim, the invention provides a preparation method of arsenic-doped cadmium telluride, which comprises the following steps: uniformly mixing the deoxidized cadmium telluride powder and the deoxidized cadmium arsenide powder, and carrying out hot-pressing sintering at 650-850 ℃ to obtain the arsenic-doped cadmium telluride, wherein the hot-pressing sintering is carried out under the protection of vacuum or protective gas.
The preparation method adopts cadmium telluride and cadmium arsenide rather than corresponding simple substances as raw materials, and carries out hot-pressing sintering at the lower temperature of 650-850 ℃, so that the raw materials are solid in the whole process, segregation is avoided, and the obtained arsenic-doped cadmium telluride material is ensured to have good uniformity; meanwhile, the deoxidized cadmium telluride powder and the deoxidized cadmium arsenide powder are used as raw materials, and hot-pressed and sintered under the protection of vacuum or protective gas, so that the obtained cadmium telluride material doped with arsenic has lower oxygen content (such as less than 200 ppm) and higher purity (such as more than 5N).
Preferably, the procedure of the hot-pressing sintering is as follows: heating to 650-850 ℃, then preserving heat and pressurizing, preserving heat and pressure, and finally cooling and depressurizing to obtain the arsenic-doped cadmium telluride. Therefore, the raw material powder can be fully preheated before pressurization, and the protection of the die is facilitated.
More preferably, the procedure of the hot press sintering is as follows: heating to 650-850 deg.C, pressurizing at 650-850 deg.C, maintaining pressure at 650-850 deg.C, and cooling and depressurizing to obtain the arsenic-doped cadmium telluride.
Preferably, in the hot-pressing sintering process, the pressure is increased to 60-100 MPa, and the pressure maintaining time is 90-120 min.
Preferably, the mass of the cadmium arsenide powder after oxygen removal accounts for 0.1-30% of the total mass of the cadmium telluride powder after oxygen removal and the cadmium arsenide powder after oxygen removal.
Preferably, in the hot-pressing sintering process, the heating rate of heating to 650-850 ℃ is 6-10 ℃/min.
Preferably, the deoxidized cadmium telluride powder is prepared by hydrogenating and deoxidizing the cadmium telluride powder; the deoxidized cadmium arsenide powder is prepared by hydrogenating and deoxidizing the cadmium arsenide powder.
Preferably, the hydrogenation temperature is 750-950 ℃ when the cadmium telluride powder is hydrogenated and deoxidized; when the cadmium arsenide powder is hydrogenated and deoxidized, the hydrogenation temperature is 450-600 ℃.
Cadmium telluride has better oxygen removing effect at the hydrogenation temperature of 750-950 ℃; cadmium arsenide can be decomposed at high temperature, and the temperature for hydrogenation and oxygen removal is controlled within the range of 450-600 ℃, so that not only can decomposition be avoided, but also oxygen can be effectively removed.
Preferably, the particle size of the cadmium telluride powder and the particle size of the cadmium arsenide powder are both below 325 meshes, the hydrogen flow rate is 3-8L/min, and the hydrogenation time is 5-10 h.
Preferably, the cadmium telluride powder used for the hydrogenation and oxygen removal and the cadmium arsenide powder used for the hydrogenation and oxygen removal have a purity of 5N or more, so that the purity of the obtained arsenic-doped cadmium telluride can reach 5N or more.
Preferably, the mixing of the deoxidized cadmium telluride powder and the deoxidized cadmium arsenide powder is carried out under the protection of protective gas; before the hot-pressing sintering, the equipment is firstly vacuumized to less than 5 multiplied by 10 -2 Pa, and introducing protective gas.
In the present invention, the protective gas may be at least one of nitrogen and an inert gas.
Compared with the prior art, the invention has the following beneficial effects: cadmium telluride and cadmium arsenide are used as raw materials instead of corresponding simple substances, and hot-pressing sintering is carried out at the lower temperature of 650-850 ℃, so that the raw materials are solid in the whole process, segregation is avoided, and the obtained arsenic-doped cadmium telluride material is ensured to have good uniformity; meanwhile, the deoxidized cadmium telluride powder and the deoxidized cadmium arsenide powder are used as raw materials and are sintered in a hot pressing way under the protection of vacuum or protective gas, so that the obtained cadmium telluride material doped with arsenic has lower oxygen content and higher purity.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples. It will be understood by those skilled in the art that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
Example 1
The embodiment provides a preparation method of arsenic-doped cadmium telluride, which comprises the following steps:
(1) Cadmium telluride powder deoxidizing: crushing cadmium telluride (with the purity of 5N) into powder with the particle size of less than 325 meshes, and then putting the powder into a hydrogen atmosphere furnace to carry out hydrogenation and deoxidization to obtain the deoxidized cadmium telluride powder, wherein the hydrogen flow is 8L/min, the hydrogenation temperature is 750 ℃, and the hydrogenation time is 10h;
(2) Deoxidizing cadmium arsenide powder: crushing cadmium arsenide (with the purity of 5N) into powder with the particle size of below 325 meshes, and then putting the powder into a hydrogen atmosphere furnace for hydrogenation and deoxygenation to obtain the deoxidized cadmium arsenide powder, wherein the hydrogen flow is 3L/min, the hydrogenation temperature is 600 ℃, and the hydrogenation time is 5 hours;
(3) And mixing the deoxidized cadmium telluride powder and the deoxidized cadmium arsenide powder according to the ratio of cadmium telluride: the mass ratio of cadmium arsenide =99.9 is as follows, the mixture is put into a homogenizer under the protection of nitrogen and mixed evenly;
(4) Putting the mixed powder obtained in the step (3) into a mould, then placing the mould into an atmosphere hot-pressing furnace, closing a furnace door, and vacuumizing to less than 5 x 10 -2 And Pa, introducing inert gas for replacement, performing replacement back and forth for three times, introducing the inert gas for the last time, maintaining one atmospheric pressure, heating to 850 ℃ at the speed of 8 ℃/min, starting pressurizing and pressurizing to 80MPa, keeping the temperature and the pressure for 120min, then cooling and reducing the pressure, and discharging from the furnace to obtain the arsenic-doped cadmium telluride.
Segregation does not occur in the preparation process of the embodiment, the obtained arsenic-doped cadmium telluride has good uniformity, the purity is 5N, the oxygen content is shown as 1, and the impurity content is shown as table 2.
Example 2
The embodiment provides a preparation method of arsenic-doped cadmium telluride, which comprises the following steps:
(1) Deoxidizing the cadmium telluride powder: crushing cadmium telluride (with the purity of 5N) into powder with the particle size of below 325 meshes, and then putting the powder into a hydrogen atmosphere furnace for hydrogenation and deoxidization to obtain the deoxidized cadmium telluride powder, wherein the hydrogen flow is 3L/min, the hydrogenation temperature is 950 ℃, and the hydrogenation time is 5h;
(2) Deoxidizing cadmium arsenide powder: crushing cadmium arsenide (with the purity of 5N) into powder with the particle size of below 325 meshes, and then putting the powder into a hydrogen atmosphere furnace for hydrogenation and deoxygenation to obtain the deoxidized cadmium arsenide powder, wherein the hydrogen flow is 8L/min, the hydrogenation temperature is 450 ℃, and the hydrogenation time is 10 hours;
(3) And mixing the deoxidized cadmium telluride powder and the deoxidized cadmium arsenide powder according to the ratio of cadmium telluride: the mass ratio of cadmium arsenide =70 is put into a homogenizer under the protection of nitrogen for uniform mixing;
(4) Putting the mixed powder obtained in the step (3) into a mould, then placing the mould into an atmosphere hot-pressing furnace, closing a furnace door, and vacuumizing to less than 5 x 10 -2 And Pa, introducing inert gas for replacement, performing replacement back and forth for three times, introducing the inert gas for the last time, maintaining one atmospheric pressure, heating to 650 ℃ at the speed of 6 ℃/min, starting pressurizing and pressurizing to 100MPa, keeping the temperature and the pressure for 90min, then cooling and reducing the pressure, and discharging from the furnace to obtain the arsenic-doped cadmium telluride.
Segregation does not occur in the preparation process of the embodiment, the obtained arsenic-doped cadmium telluride has good uniformity, the purity is 5N, the oxygen content is shown as 1, and the impurity content is shown as table 2.
Example 3
The embodiment provides a preparation method of arsenic-doped cadmium telluride, which comprises the following steps:
(1) Cadmium telluride powder deoxidizing: crushing cadmium telluride (with the purity of 5N) into powder with the particle size of below 325 meshes, and then putting the powder into a hydrogen atmosphere furnace for hydrogenation and deoxidization to obtain the deoxidized cadmium telluride powder, wherein the hydrogen flow is 5L/min, the hydrogenation temperature is 800 ℃, and the hydrogenation time is 8h;
(2) Deoxidizing cadmium arsenide powder: crushing cadmium arsenide (with the purity of 5N) into powder with the particle size of below 325 meshes, and then putting the powder into a hydrogen atmosphere furnace for hydrogenation and deoxygenation to obtain the deoxidized cadmium arsenide powder, wherein the hydrogen flow is 6L/min, the hydrogenation temperature is 500 ℃, and the hydrogenation time is 6h;
(3) And mixing the deoxidized cadmium telluride powder and the deoxidized cadmium arsenide powder according to the ratio of cadmium telluride: the mass ratio of cadmium arsenide = 88;
(4) Putting the mixed powder obtained in the step (3) into a mould, then placing the mould into an atmosphere hot-pressing furnace, closing a furnace door, and vacuumizing to less than 5 x 10 -2 And Pa, introducing inert gas for replacement, performing replacement for three times back and forth, introducing the inert gas for the last time, keeping the atmospheric pressure, heating to 700 ℃ at the speed of 10 ℃/min, starting pressurizing and pressurizing to 70MPa, keeping the temperature and the pressure for 100min, then cooling and depressurizing, and discharging from the furnace to obtain the arsenic-doped cadmium telluride.
Segregation does not occur in the preparation process of the embodiment, the obtained arsenic-doped cadmium telluride has good uniformity, the purity is 5N, the oxygen content is shown as 1, and the impurity content is shown as table 2.
TABLE 1 oxygen content/ppm of As-doped cadmium telluride obtained in the examples
| Test item | Example 1 | Example 2 | Example 3 |
| Oxygen content | 158 | 137 | 128 |
TABLE 2 impurity content/ppm of As-doped cadmium telluride obtained in each example
| Content of impurities | Example 1 | Example 2 | Example 3 |
| Na | ＜0.5 | ＜0.5 | ＜0.5 |
| Mg | ＜0.1 | ＜0.1 | ＜0.1 |
| Ca | ＜0.2 | ＜0.2 | ＜0.2 |
| Fe | 0.23 | 0.25 | 0.22 |
| Zn | 0.1 | ＜0.1 | ＜0.1 |
| Cu | 0.1 | ＜0.1 | ＜0.1 |
| Ni | 0.12 | 0.15 | 0.13 |
| Sb | 0.1 | ＜0.1 | ＜0.1 |
| Pb | 0.1 | ＜0.1 | ＜0.1 |
| Al | 0.1 | ＜0.1 | ＜0.1 |
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (1)
1. A preparation method of arsenic-doped cadmium telluride is characterized by comprising the following steps:
(1) Crushing cadmium telluride with the purity of 5N into powder with the particle size of below 325 meshes, and then putting the powder into a hydrogen atmosphere furnace to carry out hydrogenation and deoxidization to obtain the deoxidized cadmium telluride powder, wherein the hydrogen flow is 5L/min, the hydrogenation temperature is 800 ℃, and the hydrogenation time is 8h;
(2) Crushing cadmium arsenide with the purity of 5N into powder with the particle size of below 325 meshes, and then putting the powder into a hydrogen atmosphere furnace for hydrogenation and deoxygenation to obtain the deoxidized cadmium arsenide powder, wherein the hydrogen flow is 6L/min, the hydrogenation temperature is 500 ℃, and the hydrogenation time is 6 hours;
(3) And mixing the deoxidized cadmium telluride powder and the deoxidized cadmium arsenide powder according to the ratio of cadmium telluride: the mass ratio of cadmium arsenide = 88;
(4) Putting the mixed powder obtained in the step (3) into a mould, then placing the mould into an atmosphere hot-pressing furnace, closing a furnace door, and vacuumizing to less than 5 x 10 -2 And Pa, introducing inert gas for replacement, performing replacement for three times back and forth, introducing the inert gas for the last time, keeping the atmospheric pressure, heating to 700 ℃ at the speed of 10 ℃/min, starting pressurizing and pressurizing to 70MPa, keeping the temperature and the pressure for 100min, then cooling and depressurizing, and discharging from the furnace to obtain the arsenic-doped cadmium telluride.
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