CN113957543B - Method for removing surface impurities of ultra-high-purity tellurium - Google Patents
Method for removing surface impurities of ultra-high-purity tellurium Download PDFInfo
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- CN113957543B CN113957543B CN202111232500.4A CN202111232500A CN113957543B CN 113957543 B CN113957543 B CN 113957543B CN 202111232500 A CN202111232500 A CN 202111232500A CN 113957543 B CN113957543 B CN 113957543B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
- C30B35/007—Apparatus for preparing, pre-treating the source material to be used for crystal growth
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/02—Elemental selenium or tellurium
Abstract
The invention provides a method for removing surface impurities of ultra-high purity tellurium, which comprises the following steps: A) cleaning a quartz container by using a glass cleaning agent, aqua regia, dilute nitric acid and pure water in sequence, and finally performing ultrasonic treatment in the pure water to obtain a pretreated quartz container; B) placing tellurium ingots obtained by zone melting into a pretreated quartz container, loading into sublimation equipment, and sublimating under the condition of continuously introducing protective gas; the sublimation pressure is 100-1000 pa, the sublimation temperature is 350-420 ℃, and the sublimation time is 2-6 hours; C) and after sublimation is finished, cooling the system, filling protective gas into the system to normal pressure, and taking out the tellurium ingot. The method can effectively solve the problem of surface pollution of the ultrahigh pure tellurium zone melting ingot caused by containers or other reasons, makes up the defects of the prior art, greatly improves the qualification rate of products, has stable product quality, and can meet the requirements of producing CZT and MCT crystal materials.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to a method for removing impurities on the surface of ultra-high-purity tellurium.
Background
The purity of the ultra-high pure tellurium reaches 99.99999 percent (7N), and the tellurium-zinc-Cadmium (CZT) nuclear radiation detector and tellurium-cadmium-Mercury (MCT) infrared detector substrate materials prepared from the ultra-high pure tellurium are widely applied to the fields of national defense, security protection, positioning, guidance infrared detection and the like. Impurities in tellurium directly influence the service performance of CZT and MCT crystal materials, and further influence the detection range and the detection precision of the two detectors, so that the research and preparation of an ultrahigh-purity tellurium product with ultrahigh purity and stable quality and performance has great significance;
at present, the main preparation method of the ultra-high pure tellurium adopts a zone melting method, materials are placed in a graphite boat or a carbon-plated quartz boat, and the production is carried out by an induction heating or resistance heating mode, and the method has the main defects that the quality of the ultra-high pure tellurium product is unstable, because the surface pollution exists in the ultra-high pure tellurium produced by the method: (1) at present, the purity of the graphite boat can only reach 5ppm to the maximum, and trace graphite boat powder is attached to an ultra-high pure tellurium ingot after zone melting, so that pollution is caused; (2) the carbon-plated quartz boat is adopted, and cracks of different degrees can appear on the carbon film in the zone melting process, so that the surface pollution of the ultra-high-purity tellurium is caused; however, the tellurium ingot has a large number of gaps due to physical properties, and cannot be subjected to acid corrosion to remove surface impurities.
Disclosure of Invention
The invention aims to provide a method for removing surface impurities of ultra-high pure tellurium, which can remove surface pollution existing in the ultra-high pure tellurium, make up for the defects of the prior art, greatly improve the qualification rate of products and meet the requirements of producing CZT and MCT crystal materials.
The invention provides a method for removing surface impurities of ultra-high purity tellurium, which comprises the following steps:
A) cleaning a quartz container by using a glass cleaning agent, aqua regia, dilute nitric acid and pure water in sequence, and finally performing ultrasonic treatment in the pure water to obtain a pretreated quartz container;
B) placing tellurium ingots obtained by zone melting into a pretreated quartz container, loading into sublimation equipment, and sublimating under the condition of continuously introducing protective gas;
the sublimation pressure is 100-1000 pa, the sublimation temperature is 350-420 ℃, and the sublimation time is 2-6 hours;
C) and after sublimation is finished, cooling the system, filling protective gas into the system to normal pressure, and taking out the tellurium ingot.
Preferably, the aqua regia cleaning is to soak a quartz container in aqua regia for 2-8 hours.
Preferably, the dilute nitric acid cleaning is to soak a quartz container cleaned by aqua regia in dilute nitric acid solution for 5-20 min;
the mass concentration of the dilute nitric acid is 2-5%.
Preferably, the conductivity of the ultrasound to pure water is less than 0.5. mu.S/cm.
Preferably, the tellurium ingots obtained by zone melting and the zone melting boat are placed in the quartz container with the contact surface facing upwards.
Preferably, after the quartz container is placed in the sublimation equipment, high-purity nitrogen is introduced for 2-8 hours from an air inlet of the sublimation equipment, then the vacuum is pumped from a vacuum port of the sublimation equipment, and the flow of protective gas is adjusted to maintain the system pressure at 100-1000 pa.
Preferably, the vacuum port of the sublimation apparatus is disposed downstream in the gas flow direction.
Preferably, during the sublimation process, the sublimated impurities are condensed in the collecting quartz tube.
Preferably, the gas flow direction of the protective gas filled in the step C) is consistent with the gas direction of the sublimation gas flow.
The invention provides a method for removing surface impurities of ultra-high purity tellurium, which comprises the following steps: A) cleaning a quartz container by using a glass cleaning agent, aqua regia, dilute nitric acid and pure water in sequence, and finally performing ultrasonic treatment in the pure water to obtain a pretreated quartz container; B) placing tellurium ingots obtained by zone melting into a pretreated quartz container, loading into sublimation equipment, and sublimating under the condition of continuously introducing protective gas; the sublimation pressure is 100-1000 pa, the sublimation temperature is 350-420 ℃, and the sublimation time is 2-6 hours; C) and after sublimation is finished, cooling the system, filling protective gas into the system to normal pressure, and taking out the tellurium ingot. The method can effectively solve the problem of surface pollution of the ultrahigh pure tellurium zone ingots caused by containers or other reasons, makes up the defects of the prior art, greatly improves the qualification rate of products, has stable product quality, and can meet the requirements of producing CZT and MCT crystal materials.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic view of the apparatus for removing impurities on the surface of ultra-high purity tellurium according to the present invention;
FIG. 2 is a schematic cross-sectional view of a quartz container according to the present invention;
FIG. 3 is a schematic side view of the quartz container of the present invention;
1 is an air inlet, 2 is a heater, 3 is a quartz container, 4 is a collecting quartz tube, 5 is a baffle plate, and 6 is a vacuum port.
Detailed Description
The invention provides a method for removing surface impurities of ultra-high purity tellurium, which comprises the following steps:
A) cleaning a quartz container by using a glass cleaning agent, aqua regia, dilute nitric acid and pure water in sequence, and finally performing ultrasonic treatment in the pure water to obtain a pretreated quartz container;
B) placing tellurium ingots obtained by zone melting into a pretreated quartz container, loading into sublimation equipment, and sublimating under the condition of continuously introducing protective gas;
the sublimation pressure is 100-1000 pa, the sublimation temperature is 350-420 ℃, and the sublimation time is 2-6 hours;
C) and after sublimation is finished, cooling the system, filling protective gas into the system to normal pressure, and taking out the tellurium ingot.
Firstly, pretreating a quartz container used for sublimation, firstly, soaking the quartz container in a glass cleaning agent for more than 4 hours to remove oily substances on the surface of quartz, and then, washing the quartz container clean by pure water. The glass cleaning agent is preferably 901 glass cleaning agent.
And then soaking the quartz container cleaned by the glass cleaning agent in aqua regia to remove metal impurities, preferably soaking in the aqua regia for 2-8 hours, more preferably 3-7 hours, and most preferably 4-6 hours.
In order to prevent residual impurities caused by hydrolysis reaction caused by directly washing quartz which is just taken out of aqua regia, formed precipitates and attached to the surface, the method preferably uses dilute nitric acid for soaking treatment after the aqua regia is washed, and then uses flowing pure water for washing for 1-2 min. In the invention, the concentration of the dilute nitric acid is preferably 2-5%, and more preferably 3-4%; the soaking time in the dilute nitric acid is preferably 5-20 min, and more preferably 10-15 min.
And placing the quartz container washed by the dilute nitric acid in pure water for ultrasonic treatment to remove acid residues until the conductivity of the pure water after ultrasonic treatment is less than 0.5 mu S/cm.
After the pretreatment of the quartz container is finished, tellurium ingots obtained by zone melting are placed in the pretreated quartz container and are placed in sublimation equipment for sublimation and impurity removal.
In the invention, the sublimation equipment has the structure shown in figure 1, and in the invention, the sublimation equipment is a tubular cavity, and the outer side of one end of the tubular cavity is provided with a heater; the other end of the tubular cavity is provided with a collecting quartz tube for condensing sublimed impurities brought out along with the airflow.
In the invention, the tubular cavity is provided with an air inlet at one end provided with the heater for introducing protective gas, and the tubular cavity is provided with a vacuum port at one end provided with the collecting quartz tube for vacuumizing the tubular cavity.
In the invention, one end of the collection quartz tube, which is close to the vacuum port, is provided with a baffle plate for preventing tellurium powder from entering a vacuum system.
The invention preferably places the tellurium ingots obtained by zone melting and the zone-melting boat in the quartz container with the contact surface facing upwards. The contact surface of the tellurium ingot obtained by zone melting and the zone-melting boat refers to the contact surface of the tellurium ingot and the zone-melting boat in the zone melting process, the surface impurity problem is most obvious because the contact surface is directly contacted with the zone-melting boat, and the contact surface is placed upwards, namely the contact surface is not contacted with the carrying surface of the quartz container, so that the impurity removal in the sublimation process is facilitated.
Firstly, introducing protective gas such as high-purity nitrogen into a gas inlet of sublimation equipment, and emptying a tubular cavity to reduce the oxygen content of a system in the subsequent sublimation process; the high-purity nitrogen is nitrogen with the purity of 7N, and the time for introducing the nitrogen is preferably 2-8 hours, more preferably 3-7 hours, and most preferably 4-6 hours.
After protective gas is introduced and exhausted, the vacuum port of the sublimation equipment is vacuumized, and the pressure in the tubular cavity is always kept at 100-1000 Pa by adjusting the flow of the protective gas at the gas inlet.
In the sublimation process of the invention, easily sublimed impurities (compared with tellurium) are heated and sublimated, and then condensed in the collecting quartz tube, thus being removed; the impurities which are difficult to sublimate (compared with tellurium) are physically carried to a collecting quartz tube by virtue of the tellurium sublimation process, so that the impurities are separated from the tellurium ingot. And keep letting in certain flow's protective gas in the sublimation in-process, can improve the efficiency that physics was smugglied secretly under the air current effect, be favorable to getting rid of difficult sublimation impurity. Meanwhile, the sublimation efficiency is improved, and less tellurium is lost on the premise of achieving the same impurity removal effect.
In the present invention, the sublimation pressure is preferably 100 to 1000Pa, more preferably 200 to 900Pa, such as 100Pa, 200Pa, 300Pa, 400Pa, 500Pa, 600Pa, 700Pa, 800Pa, 900Pa, 1000Pa, and is preferably a range value with any of the above values as an upper limit or a lower limit; the sublimation temperature is slightly lower than the melting point of tellurium, preferably 350-420 ℃, such as 350 ℃, 360 ℃, 370 ℃, 380 ℃, 390 ℃, 400 ℃, 410 ℃ and 420 ℃, and preferably ranges with any value as the upper limit or the lower limit; the sublimation time is preferably 2 to 6 hours, such as 2 hours, 3 hours, 4 hours, 5 hours or 6 hours, and is preferably a range value in which any of the above values is an upper limit or a lower limit.
And after sublimation is finished, stopping adding, cooling to normal temperature, stopping vacuumizing, increasing the flow of protective gas at the gas inlet, and pressurizing the tubular cavity to normal pressure. The invention fills protective gas from the gas inlet to supplement gas to normal pressure, namely the gas supplementing direction is consistent with the direction of sublimation airflow when discharging, thus avoiding secondary pollution caused by back blowing of sublimated tellurium powder or impurities in the collected quartz tube onto a tellurium ingot.
The invention provides a method for removing surface impurities of ultra-high purity tellurium, which comprises the following steps: A) cleaning a quartz container by using a glass cleaning agent, aqua regia, dilute nitric acid and pure water in sequence, and finally performing ultrasonic treatment in the pure water to obtain a pretreated quartz container; B) placing tellurium ingots obtained by zone melting into a pretreated quartz container, loading into sublimation equipment, and sublimating under the condition of continuously introducing protective gas; the sublimation pressure is 100-1000 pa, the sublimation temperature is 350-420 ℃, and the sublimation time is 2-6 hours; C) and after sublimation is finished, cooling the system, filling protective gas into the system to normal pressure, and taking out the tellurium ingot. The method can effectively solve the problem of surface pollution of the ultrahigh pure tellurium zone melting ingot caused by containers or other reasons, makes up the defects of the prior art, greatly improves the qualification rate of products, has stable product quality, and can meet the requirements of producing CZT and MCT crystal materials.
In order to further illustrate the present invention, the following will describe the method for removing surface impurities of ultra-high purity tellurium in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Example 1
Washing sublimed quartz by using pure water, a, soaking the sublimed quartz in a 901 glass cleaning agent solution for 6 hours, washing the sublimed quartz by using the pure water, b, soaking the sublimed quartz in king water for 4 hours, c, soaking the sublimed quartz in a 3% dilute nitric acid solution for 10 minutes, d, finally, washing the sublimed quartz for 1 minute by using flowing pure water, placing the rinsing water in a pp groove, adding the pure water until the rinsing water submerges a quartz container, carrying out ultrasonic treatment for 1 minute, and repeating the step d until the conductivity of the ultrasonic pure water is less than 0.5 mu S/cm; after drying, packaging for later use;
wiping the visible dust on the surface of the zone-melted tellurium ingot by using a dust-free cloth, and sampling;
placing the tellurium ingot on a quartz container, enabling the contact surface of the tellurium ingot and the zone-melting boat to be upward, and loading the tellurium ingot into a sublimation furnace;
introducing high-purity nitrogen (7N) for 4 hours from an air inlet to evacuate, then vacuumizing from a vacuum port, and keeping the pressure of the system at 800-1000 pa all the time by adjusting the flow rate of the nitrogen;
heating for sublimation, controlling the temperature to be 400 ℃, and keeping the temperature for 2.5 hours; then the heating is turned off;
after cooling to normal temperature, stopping vacuumizing, increasing the nitrogen flow, and pressurizing the system to normal pressure;
taking out the tellurium ingot, immediately putting the tellurium ingot into a glove box, removing the head and the tail, and sampling and analyzing;
example 2
Washing sublimed quartz by using pure water, a, soaking the sublimed quartz in a 901 glass cleaning agent solution for 8 hours, washing the sublimed quartz by using the pure water, b, soaking the sublimed quartz in king water for 4 hours, c, soaking the sublimed quartz in a 3% dilute nitric acid solution for 15 minutes, d, finally, washing the sublimed quartz for 1 minute by using flowing pure water, putting the sublimed quartz into a pp groove, adding the pure water until the sublimed quartz submerges in a quartz container, carrying out ultrasonic treatment for 1 minute, and repeating the step d until the conductivity of the ultrasonic pure water is less than 0.5 mu S/cm; after drying, packaging for later use;
wiping the visible dust on the surface of the zone-melted tellurium ingot by using a dust-free cloth, and sampling;
placing the tellurium ingot on a quartz container, enabling the contact surface of the tellurium ingot and the zone-melting boat to be upward, and loading the tellurium ingot into a sublimation furnace;
introducing high-purity nitrogen (7N) for 6h from the air inlet to evacuate, then vacuumizing from the vacuum port, and keeping the pressure of the system at 150-350 pa all the time by adjusting the flow rate of the nitrogen;
heating for sublimation, controlling the temperature to be 380 ℃, and preserving the heat for 3 hours; then the heating is turned off;
after cooling to normal temperature, stopping vacuumizing, increasing the nitrogen flow, and pressurizing the system to normal pressure;
taking out the tellurium ingot, immediately putting the tellurium ingot into a glove box, removing the head and the tail, and sampling and analyzing;
example 3
Washing sublimed quartz by using pure water, a, soaking the sublimed quartz in a 901 glass cleaning agent solution for 5 hours, washing the sublimed quartz by using the pure water, b, soaking the sublimed quartz in king water for 4 hours, c, soaking the sublimed quartz in a 3% dilute nitric acid solution for 8 minutes, d, finally, washing the sublimed quartz for 1 minute by using flowing pure water, putting the sublimed quartz into a pp groove, adding the pure water until the sublimed quartz submerges in a quartz container, carrying out ultrasonic treatment for 1 minute, and repeating the step d until the conductivity of the ultrasonic pure water is less than 0.5 mu S/cm; after drying, packaging for later use;
wiping the visible dust on the surface of the zone-melted tellurium ingot by using a dust-free cloth, and sampling;
placing the tellurium ingot on a quartz container, enabling the contact surface of the tellurium ingot and the zone-melting boat to be upward, and loading the tellurium ingot into a sublimation furnace;
introducing high-purity nitrogen (7N) for 5 hours from an air inlet to evacuate, then vacuumizing from a vacuum port, and keeping the pressure of the system at 400-600 pa all the time by adjusting the flow rate of the nitrogen;
heating for sublimation, controlling the temperature to be 410 ℃, and keeping the temperature for 2 hours; then the heating is turned off;
after cooling to normal temperature, stopping vacuumizing, increasing the nitrogen flow, and pressurizing the system to normal pressure;
taking out the tellurium ingot, immediately putting the tellurium ingot into a glove box, removing the head and the tail, and sampling and analyzing;
comparative example 1:
washing sublimed quartz by using pure water, then putting the sublimed quartz into 901 glass cleaner solution for soaking for 5 hours, washing the sublimed quartz by using the pure water, then soaking the sublimed quartz in aqua regia for 4 hours, washing the sublimed quartz by using flowing pure water for 1 minute, putting the sublimed quartz into a pp groove, adding the pure water until the sublimed quartz submerges in a quartz container, carrying out ultrasonic treatment for 1 minute, and repeating the ultrasonic treatment until the conductivity of the ultrasonic pure water is less than 0.5 mu S/cm; after drying, packaging for later use;
wiping the visible dust on the surface of the zone-melting tellurium ingots in the same batches as in the example 3 by using a dust-free cloth;
placing the tellurium ingot on a quartz container, enabling the contact surface of the tellurium ingot and the zone-melting boat to be upward, and loading the tellurium ingot into a sublimation furnace;
introducing high-purity nitrogen (7N) for 5 hours from an air inlet to evacuate, then vacuumizing from a vacuum port, and keeping the pressure of the system at 400-600 pa all the time by adjusting the flow rate of the nitrogen;
heating for sublimation, controlling the temperature to be 410 ℃, and keeping the temperature for 2 hours; then the heating is turned off;
after cooling to normal temperature, stopping vacuumizing, increasing the nitrogen flow, and pressurizing the system to normal pressure;
taking out the tellurium ingot, immediately putting the tellurium ingot into a glove box, removing the head and the tail, and sampling and analyzing;
comparative example 2:
washing sublimed quartz by using pure water, a, soaking the sublimed quartz in a 901 glass cleaning agent solution for 5 hours, washing the sublimed quartz by using the pure water, b, soaking the sublimed quartz in king water for 4 hours, c, soaking the sublimed quartz in a 3% dilute nitric acid solution for 8 minutes, d, finally, washing the sublimed quartz for 1 minute by using flowing pure water, putting the sublimed quartz into a pp groove, adding the pure water until the sublimed quartz submerges in a quartz container, carrying out ultrasonic treatment for 1 minute, and repeating the step d until the conductivity of the ultrasonic pure water is less than 0.5 mu S/cm; after drying, packaging for later use;
wiping the visible dust on the surface of the zone-melting tellurium ingots in the same batches as in the example 3 by using a dust-free cloth;
placing the tellurium ingot on a quartz container, enabling the contact surface of the tellurium ingot and the zone-melting boat to be upward, and loading the tellurium ingot into a sublimation furnace;
vacuumizing to below 50 Pa;
heating for sublimation, controlling the temperature to be 410 ℃, and keeping the temperature for 2 hours; then the heating is turned off;
after cooling to normal temperature, stopping vacuumizing, and supplementing air to normal pressure;
taking out the tellurium ingot, immediately putting the tellurium ingot into a glove box, removing the head and the tail, and sampling and analyzing;
TABLE 1 GDMS analysis results of tellurium ingots before and after sublimation
As can be seen from the above table, through 1 time of sublimation process, the impurity content of the ultra-high purity tellurium can be controlled below the standard, and the single impurity is in the standard range, which meets the requirements of the customer standard.
Comparative example 1 no impurity standard of ultra-high purity tellurium was achieved because nitric acid treatment was not used and comparative example 2 did not continue to inject nitrogen gas during sublimation.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A method for removing impurities on the surface of ultra-high purity tellurium comprises the following steps:
A) cleaning a quartz container by using a glass cleaning agent, aqua regia, dilute nitric acid and pure water in sequence, and finally performing ultrasonic treatment in the pure water to obtain a pretreated quartz container;
B) placing tellurium ingots obtained by zone melting into a pretreated quartz container, loading into sublimation equipment, and sublimating under the condition of continuously introducing protective gas;
the sublimation pressure is 100-1000 pa, the sublimation temperature is 350-420 ℃, and the sublimation time is 2-6 hours;
C) and after sublimation is finished, cooling the system, filling protective gas into the system to normal pressure, and taking out the tellurium ingot.
2. The method as claimed in claim 1, wherein the aqua regia cleaning is carried out by immersing a quartz container in aqua regia for 2-8 hours.
3. The method as claimed in claim 2, wherein the dilute nitric acid cleaning is carried out by immersing a quartz container cleaned by aqua regia in a dilute nitric acid solution for 5-20 min;
the mass concentration of the dilute nitric acid is 2-5%.
4. The method of claim 3, wherein the conductivity of the ultrasound to pure water is less than 0.5 μ S/cm.
5. The method as claimed in claim 1, wherein the tellurium ingot obtained by zone melting is placed in a quartz vessel with the contact surface of the zone melting boat facing upwards.
6. The method as claimed in claim 1, wherein after the quartz container is loaded into the sublimation apparatus, high-purity nitrogen gas is introduced from the gas inlet of the sublimation apparatus for 2 to 8 hours, and then vacuum is drawn from the vacuum port of the sublimation apparatus, and the flow rate of the protective gas is adjusted to maintain the system pressure at 100 to 1000 pa.
7. A method according to claim 6, wherein the vacuum port of the sublimation apparatus is disposed downstream in the direction of gas flow.
8. The method of claim 7, wherein during the sublimation, the sublimated impurities condense in a collection quartz tube.
9. The method according to claim 1, wherein the flow direction of the protective gas fed in step C) coincides with the gas direction of the sublimation gas flow.
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| US4869893A (en) * | 1987-08-10 | 1989-09-26 | Hughes Aircraft Company | Preparation of high purity compounds of sulfur, selenium, and tellurium |
| JP2512961B2 (en) * | 1987-10-20 | 1996-07-03 | 三菱マテリアル株式会社 | How to remove tellurium in selenium |
| JP4460236B2 (en) * | 2003-07-23 | 2010-05-12 | 新日本製鐵株式会社 | Silicon carbide single crystal wafer |
| WO2006070480A1 (en) * | 2004-12-27 | 2006-07-06 | Nippon Steel Corporation | Silicon carbide single crystal, silicon carbide single crystal wafer, and process for producing the same |
| TWI403461B (en) * | 2010-07-21 | 2013-08-01 | Masahiro Hoshino | Method and apparatus for improving yield and yield of metallurgical silicon |
| CN102139863A (en) * | 2011-05-03 | 2011-08-03 | 嘉兴市达泽光电技术有限公司 | Method for purifying tellurium by using crucible |
| CN103911665B (en) * | 2013-01-08 | 2016-03-09 | 广东先导稀材股份有限公司 | The impurity-removing method in tellurium-zincium-cadmium crystal process prepared by employing plating carbon quartz crucible |
| CN111809240B (en) * | 2020-06-12 | 2022-01-18 | 先导薄膜材料（广东）有限公司 | Preparation method of high-purity cadmium telluride |
| CN111924811A (en) * | 2020-07-02 | 2020-11-13 | 清远先导材料有限公司 | Preparation method of ultra-high-purity tellurium |
| CN112374471A (en) * | 2020-11-13 | 2021-02-19 | 清远先导材料有限公司 | Impurity removing device and method for ultra-high-purity tellurium |
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