CN112374471A - Impurity removing device and method for ultra-high-purity tellurium - Google Patents
Impurity removing device and method for ultra-high-purity tellurium Download PDFInfo
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- CN112374471A CN112374471A CN202011268006.9A CN202011268006A CN112374471A CN 112374471 A CN112374471 A CN 112374471A CN 202011268006 A CN202011268006 A CN 202011268006A CN 112374471 A CN112374471 A CN 112374471A
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- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 73
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 239000012535 impurity Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000010453 quartz Substances 0.000 claims abstract description 172
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 172
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 125
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 89
- 239000010439 graphite Substances 0.000 claims abstract description 89
- 238000010438 heat treatment Methods 0.000 claims abstract description 51
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 239000002296 pyrolytic carbon Substances 0.000 claims description 5
- 239000010813 municipal solid waste Substances 0.000 claims 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 abstract description 24
- 229910052760 oxygen Inorganic materials 0.000 abstract description 8
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 38
- 238000000576 coating method Methods 0.000 description 11
- 238000002791 soaking Methods 0.000 description 10
- 239000000047 product Substances 0.000 description 8
- 238000004857 zone melting Methods 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 239000004744 fabric Substances 0.000 description 5
- 239000007888 film coating Substances 0.000 description 5
- 238000009501 film coating Methods 0.000 description 5
- 239000012467 final product Substances 0.000 description 5
- 238000009461 vacuum packaging Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000005034 decoration Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical class O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides an impurity removing device for ultra-high pure tellurium, which comprises a quartz tube, a heating device, a quartz boat and a graphite boat, wherein the heating device surrounds the outside of the quartz tube, and the quartz boat and the graphite boat are arranged in the quartz tube; the graphite boat is erected above the quartz boat through a support, a baffle with a hole at the bottom is arranged in the quartz boat along the length direction, the quartz boat is divided into a region A and a region B by the baffle, and the length of the region A is smaller than that of the region B; the bottom of the graphite boat is provided with a hole. The method of the invention is used for removing impurities from the ultra-high pure tellurium, and carbon powder impurities, carbon powder and oxides in the ultra-high pure tellurium are blocked at the A side of the quartz boat. According to the method, after the quartz boat is plated with carbon, tellurium cannot be adhered to the quartz boat, impurities in the quartz boat cannot enter a tellurium product, the surface of the produced product is bright, no oxide exists, the tellurium is in the form of tellurium metal, and the C, O content is less than 100 ppb.
Description
Technical Field
The invention belongs to the technical field of semiconductor materials, and particularly relates to an impurity removing device and method for 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.
The main preparation method of the ultra-high purity tellurium adopts a zone melting method, materials are placed in a graphite boat, and the production is carried out in an induction heating or resistance heating mode, and the method has the main defects that: CTZ and MCT crystals have high requirement on C, O content in materials, and a graphite boat is easy to decarbonize into products in the production process, so that the produced products have more carbon powder on the surfaces. Meanwhile, the graphite boat easily absorbs water vapor in the air, and part of tellurium can be oxidized in the production process, so that the purity of the ultra-high-purity tellurium product is influenced.
Disclosure of Invention
The invention aims to provide an impurity removing device and method for ultra-high-purity tellurium, which can effectively remove carbon and oxides and have the advantages of simple process, low cost, high efficiency and good purification effect.
The invention provides an impurity removing device for ultra-high pure tellurium, which comprises a quartz tube, a heating device, a quartz boat and a graphite boat, wherein the heating device surrounds the quartz tube and is arranged outside the quartz tube;
the graphite boat is erected above the quartz boat through a support, a baffle with a hole at the bottom is arranged in the quartz boat along the length direction, the quartz boat is divided into a region A and a region B by the baffle, and the length of the region A is smaller than that of the region B;
and the bottom of the graphite boat is provided with a hole for dripping the molten tellurium in the graphite boat into an area A in the quartz boat.
Preferably, the baffle is located at 1/4-1/5 of the length of the quartz boat.
Preferably, the aperture of the bottom of the baffle is 1-3 mm.
Preferably, the inner surface of the quartz boat is plated with a pyrolytic carbon film.
Preferably, the aperture of the hole at the bottom of the graphite boat is 1-3 mm.
Preferably, the support for erecting the graphite boat is a graphite support.
The invention provides an impurity removing method for ultra-high purity tellurium, which comprises the following steps:
A) using the preparation device of the ultra-high pure tellurium, putting the 7N tellurium raw material into a graphite boat, introducing reducing gas, and heating to melt the 7N tellurium raw material;
B) and stopping heating when the 7N tellurium raw materials are completely melted and completely dripped into the area A of the quartz boat, and obtaining the 7N tellurium subjected to impurity removal in the area B of the quartz boat.
Preferably, the reducing gas is hydrogen, and the flow rate of the reducing gas is 2-4L/min.
Preferably, the heating temperature is 500-550 ℃.
Preferably, the quartz boat is soaked in hydrofluoric acid, and after being washed, the surface of the quartz boat is plated with a pyrolytic carbon film.
The invention provides an impurity removing device for ultra-high pure tellurium, which comprises a quartz tube, a heating device, a quartz boat and a graphite boat, wherein the heating device surrounds the outside of the quartz tube, and the quartz boat and the graphite boat are arranged in the quartz tube; the graphite boat is erected above the quartz boat through a support, a baffle with a hole at the bottom is arranged in the quartz boat along the length direction, the quartz boat is divided into a region A and a region B by the baffle, and the length of the region A is smaller than that of the region B; and the bottom of the graphite boat is provided with a hole for dripping the molten tellurium in the graphite boat into an area A in the quartz boat. The method provided by the invention is used for removing impurities from the ultra-high purity tellurium, after the material is melted, the carbon powder floats and is isolated from the surface of the molten liquid by the baffle, the tellurium flows to the other side of the quartz boat through the small hole at the bottom of the baffle, and simultaneously, under the atmosphere of introducing hydrogen, the oxide in the tellurium is reduced, so that the carbon and oxygen removal effect is achieved. Carbon powder, impurity carbon powder and oxide in the ultra-high pure tellurium are blocked at the A side of the quartz boat. According to the method, after the quartz boat is plated with carbon, tellurium cannot be adhered to the quartz boat, meanwhile, impurities in the quartz boat cannot enter a tellurium product, the surface of the produced product is bright, no oxide exists, the tellurium is a tellurium metal, the C, O content is less than 100ppb, and the use requirements of customers are met.
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 structural diagram of an impurity removing device in the present invention, in FIG. 1, 1 is a quartz tube, 2 is a heating device, 3 is a quartz boat, 4 is a graphite support, 5 is a graphite boat, 6 is a quartz tube cap, and 7 is a furnace body;
FIG. 2 is a schematic structural diagram of the quartz boat of the present invention, wherein a is a side view of the quartz boat, b is a top view of the quartz boat, 3-1 is a baffle, and 3-1-1 is a through hole;
FIG. 3 is a schematic structural view of a graphite boat in the present invention, wherein a in FIG. 3 is a side view of the graphite boat, b is a cross-sectional view of the graphite boat, and 5-1 is a through hole.
Detailed Description
The invention provides an impurity removing device for ultra-high pure tellurium, which comprises a quartz tube, a heating device, a quartz boat and a graphite boat, wherein the heating device surrounds the outside of the quartz tube, and the quartz boat and the graphite boat are arranged in the quartz tube;
the graphite boat is erected above the quartz boat through a support, a baffle with a hole at the bottom is arranged in the quartz boat along the length direction, the quartz boat is divided into a region A and a region B by the baffle, and the length of the region A is smaller than that of the region B;
and the bottom of the graphite boat is provided with a hole for dripping the molten tellurium in the graphite boat into an area A in the quartz boat.
In the invention, the quartz tube is provided with a tube body and a tube cap, the quartz tube can be sealed, and a heating device is arranged outside the quartz tube and used for providing heat energy for melting raw materials in the quartz tube. The present invention is not particularly limited in size of the quartz tube, and a quartz tube having a size commonly used in the art may be used.
The quartz tube is internally provided with a quartz boat and a graphite boat, the quartz boat is arranged below the quartz tube, and the graphite boat is arranged above the quartz boat.
The inner surface of the quartz boat is plated with a pyrolytic carbon film at least so as to prevent impurities in the quartz boat from entering the tellurium product and prevent the tellurium from being adhered to the quartz boat. However, according to the process characteristics of the carbon coating film, the inner surface and the outer surface of the quartz boat can be completely coated with carbon.
In the invention, the inner part of the quartz boat is provided with a baffle plate along the length direction, the quartz boat is divided into a region A and a region B from the length direction, and the bottom of the baffle plate is provided with a through hole for enabling molten tellurium to flow into the region B from the region A and blocking carbon powder impurities in the region A. The aperture of the through hole at the bottom of the baffle is preferably 1-3 mm, and more preferably 1-2 mm.
In the present invention, the length of the region a is smaller than that of the region B, and more preferably, the ratio of the length of the region a to the length of the region B is preferably (3-5): 1, more preferably 4:1, i.e. the baffle is preferably arranged at 1/5 of the length direction of the quartz boat.
In the invention, the graphite boat is erected above the quartz boat, and the bottom of the graphite boat is provided with at least one through hole for dripping the melted ultra-high pure tellurium into the area A of the graphite boat, so the bottom through hole of the graphite boat should be arranged above the area A of the graphite boat.
The aperture of the through hole at the bottom of the graphite boat is preferably 1-3 mm, and more preferably 1-2 mm.
The invention has no special limitation on the specific sizes of the graphite boat and the quartz boat, and can be matched with the size of the quartz tube.
Based on the impurity removal device, the invention also provides a method for removing impurities from the ultra-high pure tellurium obtained by zone melting by using the impurity removal device, which comprises the following steps:
A) using the preparation device of the ultra-high pure tellurium, putting the 7N tellurium raw material into a graphite boat, introducing reducing gas, and heating to melt the 7N tellurium raw material;
B) and stopping heating when the 7N tellurium raw materials are completely melted and completely dripped into the area A of the quartz boat, and obtaining the 7N tellurium subjected to impurity removal in the area B of the quartz boat.
In the invention, the 7N tellurium raw material is preferably 7N ultra-high pure tellurium prepared by a zone melting method, and contains carbon powder impurities and oxides.
The preferable reducing gas is hydrogen, the preferable flow rate of the reducing gas is 2-4L/min, and more preferable flow rate is 3-3.5L/min, and the preferable ventilation time of the reducing gas is 2-4 hours, and more preferable ventilation time is 3-3.5 hours; the purity of the hydrogen gas is preferably 6N or more.
The heating temperature is preferably 500-550 ℃; the heating time is not specially limited, the heating time can be correspondingly adjusted according to the quantity of the raw materials, and the heating can be stopped when the 7N tellurium raw materials in the graphite boat are completely melted and completely drip into the area A of the quartz boat.
The melted materials are dripped into the area A and flow into the area B from the through hole of the baffle, carbon powder and oxides are blocked in the area A of the quartz boat, and the materials in the area B are cooled to obtain the 7N ultra-high pure tellurium after impurity removal.
The invention provides an impurity removing device for ultra-high pure tellurium, which comprises a quartz tube, a heating device, a quartz boat and a graphite boat, wherein the heating device surrounds the outside of the quartz tube, and the quartz boat and the graphite boat are arranged in the quartz tube; the graphite boat is erected above the quartz boat through a support, a baffle with a hole at the bottom is arranged in the quartz boat along the length direction, the quartz boat is divided into a region A and a region B by the baffle, and the length of the region A is smaller than that of the region B; and the bottom of the graphite boat is provided with a hole for dripping the molten tellurium in the graphite boat into an area A in the quartz boat. The method of the invention is used for removing impurities from the ultra-high pure tellurium, and carbon powder impurities, carbon powder and oxides in the ultra-high pure tellurium are blocked at the A side of the quartz boat. According to the method, after the quartz boat is plated with carbon, tellurium cannot be adhered to the quartz boat, meanwhile, impurities in the quartz boat cannot enter a tellurium product, the surface of the produced product is bright, no oxide exists, the tellurium is a tellurium metal, the C, O content is less than 100ppb, and the use requirements of customers are met.
In order to further illustrate the present invention, the following detailed description of the apparatus for removing impurities of ultra-high purity tellurium is provided in connection with the examples, which should not be construed as limiting the scope of the present invention.
Example 1
Soaking the required quartz boat for more than 8 hours by using 2-5% hydrofluoric acid, removing impurities on the surface of the quartz boat, cleaning the quartz boat by using pure water after soaking, and finally performing film coating operation on the surface of the quartz boat by using a carbon coating furnace according to a carbon coating process;
wiping the required auxiliary materials (baffle quartz boat, graphite boat and the like) and the quartz tube of the heating furnace with dust-free cloth and UP-grade absolute ethyl alcohol for later use;
combining a graphite boat and a quartz boat according to the figure 1, aligning the A side of the graphite boat with the A side of the quartz boat, putting 7N zone-melting tellurium into the graphite boat, then putting the whole graphite boat into a quartz tube of a heating furnace, and covering a tube cap;
introducing hydrogen (6N or more) into the quartz tube, wherein the flow rate is 4L/min, and the introducing time is 4 h;
starting heating, setting the heating temperature to be 550 ℃, observing the melting condition of the materials in the graphite boat, completely dripping the materials into the quartz boat after the materials in the graphite boat are melted, and stopping heating;
and when the material is cooled to room temperature, taking out the material in the quartz boat, keeping the carbon powder and the oxide on the side A, taking out the side B of the quartz boat as a final product, and carrying out vacuum packaging.
Example 2
Soaking the required quartz boat for more than 8 hours by using 2-5% hydrofluoric acid, removing impurities on the surface of the quartz boat, cleaning the quartz boat by using pure water after soaking, and finally performing film coating operation on the surface of the quartz boat by using a carbon coating furnace according to a carbon coating process;
wiping the required auxiliary materials (baffle quartz boat, graphite boat and the like) and the quartz tube of the heating furnace with dust-free cloth and UP-grade absolute ethyl alcohol for later use;
combining a graphite boat and a quartz boat according to the figure 1, aligning the A side of the graphite boat with the A side of the quartz boat, putting 7N zone-melting tellurium into the graphite boat, then putting the whole graphite boat into a quartz tube of a heating furnace, and covering a tube cap;
introducing hydrogen (6N or more) into the quartz tube, wherein the flow rate is 2L/min, and the introducing time is 4 h;
starting heating, setting the heating temperature to be 500 ℃, observing the melting condition of the materials in the graphite boat, completely dripping the materials into the quartz boat after the materials in the graphite boat are melted, and stopping heating;
and when the material is cooled to room temperature, taking out the material in the quartz boat, keeping the carbon powder and the oxide on the side A, taking out the side B of the quartz boat as a final product, and carrying out vacuum packaging.
Example 3
Soaking the required quartz boat for more than 8 hours by using 2-5% hydrofluoric acid, removing impurities on the surface of the quartz boat, cleaning the quartz boat by using pure water after soaking, and finally performing film coating operation on the surface of the quartz boat by using a carbon coating furnace according to a carbon coating process;
wiping the required auxiliary materials (baffle quartz boat, graphite boat and the like) and the quartz tube of the heating furnace with dust-free cloth and UP-grade absolute ethyl alcohol for later use;
combining a graphite boat and a quartz boat according to the figure 1, aligning the A side of the graphite boat with the A side of the quartz boat, putting 7N zone-melting tellurium into the graphite boat, then putting the whole graphite boat into a quartz tube of a heating furnace, and covering a tube cap;
introducing hydrogen (6N or more) into the quartz tube, wherein the flow rate is 3L/min, and the introducing time is 3 h;
starting heating, setting the heating temperature to 520 ℃, observing the melting condition of the materials in the graphite boat, completely dripping the materials into the quartz boat after the materials in the graphite boat are melted, and stopping heating;
and when the material is cooled to room temperature, taking out the material in the quartz boat, keeping the carbon powder and the oxide on the side A, taking out the side B of the quartz boat as a final product, and carrying out vacuum packaging.
Example 4
Soaking the required quartz boat for more than 8 hours by using 2-5% hydrofluoric acid, removing impurities on the surface of the quartz boat, cleaning the quartz boat by using pure water after soaking, and finally performing film coating operation on the surface of the quartz boat by using a carbon coating furnace according to a carbon coating process;
wiping the required auxiliary materials (baffle quartz boat, graphite boat and the like) and the quartz tube of the heating furnace with dust-free cloth and UP-grade absolute ethyl alcohol for later use;
combining a graphite boat and a quartz boat according to the figure 1, aligning the A side of the graphite boat with the A side of the quartz boat, putting 7N zone-melting tellurium into the graphite boat, then putting the whole graphite boat into a quartz tube of a heating furnace, and covering a tube cap;
introducing hydrogen (6N or more) into the quartz tube, wherein the flow rate is 3L/min, and the introducing time is 2 h;
starting heating, setting the heating temperature to be 540 ℃, observing the melting condition of the materials in the graphite boat, completely dripping the materials into the quartz boat after the materials in the graphite boat are melted, and stopping heating;
and when the material is cooled to room temperature, taking out the material in the quartz boat, keeping the carbon powder and the oxide on the side A, taking out the side B of the quartz boat as a final product, and carrying out vacuum packaging.
Example 5
Soaking the required quartz boat for more than 8 hours by using 2-5% hydrofluoric acid, removing impurities on the surface of the quartz boat, cleaning the quartz boat by using pure water after soaking, and finally performing film coating operation on the surface of the quartz boat by using a carbon coating furnace according to a carbon coating process;
wiping the required auxiliary materials (baffle quartz boat, graphite boat and the like) and the quartz tube of the heating furnace with dust-free cloth and UP-grade absolute ethyl alcohol for later use;
combining a graphite boat and a quartz boat according to the figure 1, aligning the A side of the graphite boat with the A side of the quartz boat, putting 7N zone-melting tellurium into the graphite boat, then putting the whole graphite boat into a quartz tube of a heating furnace, and covering a tube cap;
introducing hydrogen (6N or more) into the quartz tube, wherein the flow rate is 4L/min, and the introducing time is 3 h;
starting heating, setting the heating temperature to be 540 ℃, observing the melting condition of the materials in the graphite boat, completely dripping the materials into the quartz boat after the materials in the graphite boat are melted, and stopping heating;
and when the material is cooled to room temperature, taking out the material in the quartz boat, keeping the carbon powder and the oxide on the side A, taking out the side B of the quartz boat as a final product, and carrying out vacuum packaging.
TABLE 1 statistical table of carbon and oxygen contents and surface condition of ultra-high purity tellurium
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Carbon content (ppb) | <100 | <100 | <100 | <100 | <100 |
| Oxygen content (ppb) | <50 | 85 | 77 | 64 | 56 |
| Surface condition of the surface | Light brightness | Light brightness | Light brightness | Light brightness | Light brightness |
As can be seen from the table above, after the treatment by the method, the carbon and oxygen contents in the material are both less than 200ppb, and the use requirements of customers are met.
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 (10)
1. An impurity removing device for ultra-high pure tellurium comprises a quartz tube, a heating device surrounding the outside of the quartz tube, a quartz boat and a graphite boat arranged in the quartz tube;
the graphite boat is erected above the quartz boat through a support, a baffle with a hole at the bottom is arranged in the quartz boat along the length direction, the quartz boat is divided into a region A and a region B by the baffle, and the length of the region A is smaller than that of the region B;
and the bottom of the graphite boat is provided with a hole for dripping the molten tellurium in the graphite boat into an area A in the quartz boat.
2. The trash removal device of claim 1, wherein the baffle is located 1/4-1/5 of the length of the quartz boat.
3. The impurity removing device according to claim 1, wherein the aperture of the bottom of the baffle is 1-3 mm.
4. The impurity removing device according to claim 1, wherein the inner surface of the quartz boat is coated with a pyrolytic carbon film.
5. The impurity removing device according to claim 1, wherein the diameter of the hole at the bottom of the graphite boat is 1-3 mm.
6. The trash removal device of claim 1, wherein the support on which the graphite boat is mounted is a graphite support.
7. An impurity removal method for ultra-high purity tellurium comprises the following steps:
A) the apparatus for producing ultra-high purity tellurium as claimed in any one of claims 1 to 5, wherein 7N tellurium as a raw material is placed in a graphite boat, and a reducing gas is introduced into the boat and heated to melt the 7N tellurium;
B) and stopping heating when the 7N tellurium raw materials are completely melted and completely dripped into the area A of the quartz boat, and obtaining the 7N tellurium subjected to impurity removal in the area B of the quartz boat.
8. An impurity removal method according to claim 7, wherein the reducing gas is hydrogen, and a flow rate of the reducing gas is 2 to 4L/min.
9. An impurity removal method according to claim 7, wherein the heating temperature is 500 to 550 ℃.
10. The method according to claim 7, wherein the quartz boat is immersed in hydrofluoric acid, and the pyrolytic carbon film is coated on the surface of the quartz boat after washing.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113957543A (en) * | 2021-10-22 | 2022-01-21 | 广东先导微电子科技有限公司 | Method for removing surface impurities of ultra-high-purity tellurium |
| CN115477322A (en) * | 2022-09-29 | 2022-12-16 | 云南驰宏国际锗业有限公司 | Ultra-high purity GeCl 4 Preparation method |
| CN115609002A (en) * | 2022-09-29 | 2023-01-17 | 云南驰宏国际锗业有限公司 | Preparation method of high-purity superfine metal germanium powder |
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