CN113120957B - Deoxidizing method of cadmium arsenide - Google Patents
Deoxidizing method of cadmium arsenide Download PDFInfo
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- CN113120957B CN113120957B CN202110445420.0A CN202110445420A CN113120957B CN 113120957 B CN113120957 B CN 113120957B CN 202110445420 A CN202110445420 A CN 202110445420A CN 113120957 B CN113120957 B CN 113120957B
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Abstract
The invention provides a method for deoxidizing cadmium arsenide, and belongs to the field of material preparation. The method for deoxidizing the cadmium arsenide does not need to adopt specific implementation environment and equipment, and the pressure and the flow of the hydrogen in the atmosphere environment are controlled in the hydrogen reduction process, and the deoxidization is implemented by a two-section heating and heat-preserving procedure, so that the decomposition of the cadmium arsenide in the process can be avoided, the high-temperature hydrogenation effect is improved, and the loss rate of the whole material can be reduced. The cadmium arsenide treated by the method has the oxygen content of less than 100ppm and the material loss rate of less than 0.07 percent.
Description
Technical Field
The invention belongs to the field of material preparation, and particularly relates to a method for deoxidizing cadmium arsenide.
Background
Cadmium arsenide (CAS No. 12006-15-4, melting point about 716 ℃, vapour pressure at the melting point temperature about 0.8 atm) is generally produced by chemical combination of arsenic and cadmium, and in the existing industry, the initially synthesized cadmium arsenide has a high oxygen content, and the product contains a large amount of arsenic oxide and cadmium oxide, which greatly reduces the quality and performance of the material, so that oxygen removal by hydrogen reduction is required for the product. At normal pressure, higher temperature is needed for reduction with hydrogen, but cadmium arsenide gradually decomposes at a temperature of more than 500 ℃ in a hydrogen atmosphere, and a temperature less than this leads to poor hydrogenation and oxygen removal effects.
Disclosure of Invention
Based on the defects in the prior art, the invention aims to provide the cadmium arsenide deoxidizing method which has low requirements on equipment and environment, the prepared cadmium arsenide has the oxygen content of less than 100ppm, and the material loss rate is less than 0.07%.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for removing oxygen from cadmium arsenide comprises the following steps:
(1) crushing the cadmium arsenide primary material, then placing the crushed material into an atmosphere pressure furnace, introducing inert atmosphere to replace air in the atmosphere pressure furnace, raising the temperature and boosting the pressure to maintain the temperature in the furnace between 300 and 450 ℃ and the pressure between 2 and 3 atmospheric pressures, then introducing hydrogen and carrying out primary heat preservation, wherein the pressure is maintained between 2 and 3 atmospheric pressures during the heat preservation;
(2) after the primary heat preservation is finished, heating the furnace body to 680-710 ℃, carrying out secondary heat preservation, cooling to be less than or equal to 500 ℃ after the secondary heat preservation is finished, then removing the pressure of hydrogen, and introducing inert atmosphere to replace the hydrogen in the furnace;
(3) and after the furnace body is cooled to the room temperature, the deoxidization of the cadmium arsenide is finished.
In the deoxidization method, hydrogen is used as a deoxidization reducing agent, and also serves as a pressure maintaining agent in a reaction environment at a certain high temperature, the same pressure value is maintained during the temperature rise and the heat preservation, cadmium arsenide can be effectively ensured not to be decomposed at the high temperature, and the deoxidization efficiency of the cadmium arsenide can be effectively ensured by maintaining the flow.
The method for deoxidizing the cadmium arsenide does not need to adopt specific implementation environment and equipment, controls the pressure of hydrogen in the atmosphere environment in the hydrogen reduction process, and implements deoxidization by a two-section heating and heat-preserving procedure, so that the decomposition of the cadmium arsenide in the process can be avoided, the high-temperature hydrogenation effect is improved, and the loss rate of the whole material can be reduced.
Preferably, the flow rate of the introduced hydrogen in the step (1) is 3-5L/min.
Preferably, the cadmium arsenide primary material in the step (1) is crushed to the particle size of-100 meshes.
The surface contact area of the cadmium arsenide primary material which is crushed to-100 meshes (namely the particle size of the primary material is crushed to be below the corresponding size of 100 meshes) is obviously increased, the cadmium arsenide primary material is fully contacted with hydrogen, and the hydrogenation and oxygen removal effect is improved.
Preferably, the temperature rise rate in the step (1) is 5-10 ℃/min, and the heat preservation time is 30-60 min.
Before the deoxidization reaction, the temperature rise rate of the furnace body is controlled, hydrogen is introduced, and the temperature is kept for a certain time, so that redundant impurity gas in the furnace body can be effectively removed, the stability of the cadmium arsenide primary material is kept, and unnecessary side reactions are avoided.
Preferably, the temperature rising rate in the step (2) is 3-6 ℃/min, and the heat preservation time is 6-10 h.
The furnace body can ensure the stability of pressure during two-stage temperature rise through strict temperature rise rate, effectively avoid cadmium arsenide from decomposing due to too fast temperature rise or unstable furnace body pressure, and simultaneously, hydrogen can fully react with arsenic oxide and cadmium oxide in sufficient heat preservation time.
The invention also aims to provide the application of the cadmium arsenide deoxidization method in the preparation of cadmium arsenide materials.
The invention has the beneficial effects that the invention provides the method for deoxidizing the cadmium arsenide, no specific implementation environment and equipment are needed, the pressure and the flow of hydrogen in the atmosphere environment are controlled in the hydrogen reduction process, and the deoxidization is implemented by a two-section heating and heat-preserving procedure, so that the decomposition of the cadmium arsenide in the process can be avoided, the high-temperature hydrogenation effect is improved, and the loss rate of the whole material can be reduced. The cadmium arsenide oxygen content treated by the method is less than 100ppm, and the material loss rate is less than 0.07%.
Detailed Description
In order to better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples and comparative examples, which are intended to be understood in detail, but not intended to limit the invention. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of protection of the present invention.
Example 1
One embodiment of the cadmium arsenide deoxygenation method of the present invention comprises the following steps:
(1) crushing the cadmium arsenide primary material to 100 meshes, putting the crushed material into an atmosphere pressure furnace, introducing inert atmosphere to replace the air in the furnace, heating the interior of the furnace to 450 ℃ at the speed of 5 ℃/min, and maintaining the pressure in the furnace to be 2 atmospheric pressures; then preserving the heat for 30min and introducing hydrogen simultaneously, and maintaining the pressure in the furnace at 2 atmospheric pressures; the flow rate of the hydrogen is 5L/min;
(2) heating the furnace body to 710 ℃ at the speed of 5 ℃/min, preserving heat for 7 hours, cooling to be less than or equal to 500 ℃ after heat preservation is finished, then removing the pressure of hydrogen and introducing inert atmosphere to replace the hydrogen in the furnace;
(3) and after the furnace body is cooled to the room temperature, the deoxidization of the cadmium arsenide is finished.
Example 2
One embodiment of the cadmium arsenide deoxygenation method of the present invention comprises the following steps:
(1) crushing the cadmium arsenide primary material to 200 meshes, putting the crushed material into an atmosphere pressure furnace, introducing inert atmosphere to replace the air in the furnace, heating the interior of the furnace to 400 ℃ at the speed of 10 ℃/min, and maintaining the pressure in the furnace to be 3 atmospheric pressures; then preserving the heat for 50min and introducing hydrogen simultaneously, and maintaining the pressure in the furnace at 3 atmospheric pressures; the flow rate of the hydrogen is 3L/min;
(2) heating the furnace body to 680 ℃ at the speed of 3 ℃/min, preserving heat for 6 hours, cooling to be less than or equal to 500 ℃ after heat preservation is finished, then removing the pressure of hydrogen, and introducing inert atmosphere to replace the hydrogen in the furnace;
(3) and after the furnace body is cooled to the room temperature, the deoxidization of the cadmium arsenide is finished.
Example 3
One embodiment of the cadmium arsenide deoxygenation method of the present invention comprises the following steps:
(1) crushing the cadmium arsenide primary material to 100 meshes, putting the crushed material into an atmosphere pressure furnace, introducing inert atmosphere to replace the air in the furnace, heating the interior of the furnace to 300 ℃ at the speed of 8 ℃/min, and maintaining the pressure in the furnace to be 2.5 atmospheric pressure; then preserving the heat for 30min and introducing hydrogen simultaneously, and maintaining the pressure in the furnace at 2.5 atmospheric pressures; the flow rate of the hydrogen is 4L/min;
(2) heating the furnace body to 700 ℃ at the speed of 6 ℃/min, preserving heat for 8 hours, cooling to be less than or equal to 500 ℃ after heat preservation is finished, then removing the pressure of hydrogen, and introducing inert atmosphere to replace the hydrogen in the furnace;
(3) and after the furnace body is cooled to the room temperature, the deoxidization of the cadmium arsenide is finished.
Comparative example 1
A comparative example of the cadmium arsenide deoxygenation method of the present invention includes the following steps:
(1) crushing the cadmium arsenide primary material to 100 meshes, then placing the crushed material into an atmosphere pressure furnace, introducing inert atmosphere to replace the air in the furnace, heating the interior of the furnace to 400 ℃ at the speed of 8 ℃/min, and maintaining the pressure in the furnace to be 0.5 atmospheric pressure; then preserving the heat for 50min and introducing hydrogen simultaneously, and maintaining the pressure in the furnace at 0.5 atmospheric pressure; the flow rate of the hydrogen is 4L/min;
(2) heating the furnace body to 710 ℃ at the speed of 5 ℃/min, preserving heat for 8 hours, cooling to be less than or equal to 500 ℃ after heat preservation is finished, then removing the pressure of hydrogen, and introducing inert atmosphere to replace the hydrogen in the furnace;
(3) and after the furnace body is cooled to the room temperature, the deoxidization of the cadmium arsenide is finished.
Comparative example 2
A comparative example of the cadmium arsenide deoxygenation method of the present invention includes the following steps:
(1) crushing the cadmium arsenide primary material to 100 meshes, putting the crushed material into an atmosphere pressure furnace, introducing inert atmosphere to replace the air in the furnace, heating the interior of the furnace to 400 ℃ at the speed of 8 ℃/min, and maintaining the pressure in the furnace to be 2 atmospheric pressures; then preserving the heat for 50min and introducing hydrogen simultaneously, and maintaining the pressure in the furnace at 2 atmospheric pressures; the flow rate of the hydrogen is 2L/min;
(2) heating the furnace body to 700 ℃ at the speed of 5 ℃/min, preserving heat for 8 hours, cooling to be less than or equal to 500 ℃ after heat preservation is finished, then removing the pressure of hydrogen, and introducing inert atmosphere to replace the hydrogen in the furnace;
(3) and when the furnace body is cooled to the room temperature, the deoxidization of the cadmium arsenide is finished.
Effect example 1
In order to verify the deoxidizing effect of the cadmium arsenide deoxidizing method, the cadmium arsenide samples treated by the methods of examples 1-3 and comparative examples 1-2 are subjected to front and back element analysis to obtain the oxygen content change of the cadmium arsenide before and after hydrogenation, and meanwhile, the material loss rate of the process ((the mass of the cadmium arsenide before hydrogenation-the mass of the cadmium arsenide after hydrogenation)/the mass of the cadmium arsenide before hydrogenation x 100%) is calculated, and the test results are shown in table 1.
TABLE 1
| Test items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
| Oxygen content before hydrogenation (ppm) | 409 | 468 | 580 | 505 | 498 |
| Oxygen content after hydrogenation (ppm) | 89 | 78 | 91 | 83 | 230 |
| Percentage of Material loss (%) | 0.06 | 0.05 | 0.06 | 3.4 | 0.05 |
As can be seen from Table 1, the cadmium arsenide deoxidization method can effectively reduce the oxygen content of the cadmium arsenide product to be below 100ppm, and simultaneously controls the economic benefit of the process, so that the material loss rate is lower than 0.07%; the method of the comparative example 1 has more material loss due to insufficient furnace body air pressure, and the economic benefit is obviously reduced; the process described in comparative example 2 results in a lower oxygen removal efficiency due to insufficient hydrogen content.
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 (3)
1. The method for removing oxygen from cadmium arsenide is characterized by comprising the following steps:
(1) crushing the cadmium arsenide primary material, then placing the crushed material into an atmosphere pressure furnace, introducing inert atmosphere to replace air in the atmosphere pressure furnace, raising the temperature and raising the pressure at a temperature raising rate of 5-10 ℃/min to maintain the temperature in the furnace between 300-450 ℃ and the pressure between 2-3 atmospheric pressures, then introducing hydrogen and carrying out primary heat preservation for 30-60 min, wherein the pressure is maintained between 2-3 atmospheric pressures during the heat preservation period; the flow rate of the introduced hydrogen is 3-5L/min;
(2) after the primary heat preservation is finished, heating the furnace body to 680-710 ℃ at a heating rate of 3-6 ℃/min, carrying out secondary heat preservation for 6-10 h, cooling to be less than or equal to 500 ℃ after the secondary heat preservation is finished, then removing the pressure of hydrogen, and introducing inert atmosphere to replace the hydrogen in the furnace;
(3) and after the furnace body is cooled to the room temperature, the deoxidization of the cadmium arsenide is finished.
2. The method for removing oxygen from cadmium arsenide as claimed in claim 1, wherein the cadmium arsenide starting material in step (1) is crushed to a particle size of-100 mesh.
3. The use of the cadmium arsenide deoxygenation method of any of claims 1-2 in the preparation of a cadmium arsenide material.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112125285A (en) * | 2020-09-18 | 2020-12-25 | 先导薄膜材料（广东）有限公司 | Arsenic or compound thereof doped cadmium selenide and preparation method thereof, thin film solar cell and preparation method thereof |
| CN112125286A (en) * | 2020-09-18 | 2020-12-25 | 先导薄膜材料（广东）有限公司 | Arsenic or compound thereof doped cadmium selenide and preparation method thereof, thin film solar cell and preparation method thereof |
| CN112301239A (en) * | 2020-09-30 | 2021-02-02 | 广东先导稀材股份有限公司 | Preparation method of cadmium arsenide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112125285A (en) * | 2020-09-18 | 2020-12-25 | 先导薄膜材料（广东）有限公司 | Arsenic or compound thereof doped cadmium selenide and preparation method thereof, thin film solar cell and preparation method thereof |
| CN112125286A (en) * | 2020-09-18 | 2020-12-25 | 先导薄膜材料（广东）有限公司 | Arsenic or compound thereof doped cadmium selenide and preparation method thereof, thin film solar cell and preparation method thereof |
| CN112301239A (en) * | 2020-09-30 | 2021-02-02 | 广东先导稀材股份有限公司 | Preparation method of cadmium arsenide |
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