CN111926391A - Quartz tube high-vacuum exhaust system and method - Google Patents
Quartz tube high-vacuum exhaust system and method Download PDFInfo
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- CN111926391A CN111926391A CN202010827541.7A CN202010827541A CN111926391A CN 111926391 A CN111926391 A CN 111926391A CN 202010827541 A CN202010827541 A CN 202010827541A CN 111926391 A CN111926391 A CN 111926391A
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- quartz tube
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- vacuum exhaust
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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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
- C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The application discloses quartz capsule high vacuum exhaust system, including the quartz capsule, the open end of quartz capsule is connected to the vacuum pump body, the inside of open end has held the sleeve pipe, during exhaust the sleeve pipe with the space has between the quartz capsule inner wall, exhaust completion back the sleeve pipe with the quartz capsule inner wall sinters into encapsulated situation, the blind end the inside of quartz capsule holds the mercury source, the outside of blind end utilizes cooling device to surround for keep mercury source temperature is below 0 ℃, moreover the quartz capsule is inside still to be fixed with the wafer. The application also discloses a quartz tube high vacuum exhaust method, which comprises the steps of pumping the quartz tube to high vacuum by using the quartz tube high vacuum exhaust system; and sintering the quartz tube and the sleeve together to form a sealed space. The system and the method disclosed by the application can inhibit the volatilization of mercury, improve the vacuum degree of the quartz tube and shorten the exhaust time.
Description
Technical Field
The invention belongs to the technical field of heat treatment equipment, and particularly relates to a quartz tube high-vacuum exhaust system and a quartz tube high-vacuum exhaust method.
Background
The mercury cadmium telluride is an important infrared detection material, and has the advantages of adjustable forbidden band width, detection spectral range extending from a short wave band to a very long wave band, high photoelectric detection efficiency and the like, so the mercury cadmium telluride is widely applied to military and civil fields such as early warning detection, infrared reconnaissance, imaging guidance and the like. The mercury cadmium telluride infrared focal plane device develops rapidly, wherein the implantation of B + ions to form an n-on-p junction is a common mode for preparing a mercury cadmium telluride photovoltaic detector, and the development of the n-on-p technology has formed a stable process technology, high device reliability and high yield so far. It should be noted that mercury cadmium telluride is a ternary compound, and after the material growth is completed, the stoichiometric ratio and components of the material are usually adjusted by adopting a mercury source heat treatment process, so that the performance of the material meets the requirements of devices, and the defects of the material are reduced, thereby achieving the purpose of improving pn junctions. In the closed tube heat treatment process, firstly, the processed tellurium-cadmium-mercury material and mercury are respectively placed in a quartz tube, the quartz tube is pumped to high vacuum through exhaust, and then the quartz tube and a sleeve are sealed by adopting a vacuum tube sealing technology. The heat treatment of the mercury source of the closed tube provides a process environment which is balanced at a certain temperature and a certain mercury vapor pressure for the mercury cadmium telluride material, the adopted heat treatment process has high requirement on the vacuum degree in the quartz tube, otherwise, an oxide layer is formed on the surface of the material, although the oxidation degree is possibly light, the barrier effect of the oxide layer on the internal and external atom communication of the surface layer is very obvious, therefore, the oxygen content in the quartz tube must be reduced as much as possible, and the high vacuum degree in the quartz tube is ensured.
In addition, the vacuum exhaust table usually exhausts gas to a plurality of quartz tubes at the same time, the problem caused by mercury volatilization is more prominent, the vacuum degree of the quartz tubes cannot be ensured, and the efficiency of the process is also influenced by longer exhaust time.
Disclosure of Invention
In order to solve the problems, the invention provides a high-vacuum exhaust system and method for a quartz tube, which can inhibit the volatilization of mercury, improve the vacuum degree of the quartz tube and shorten the exhaust time.
The invention provides a quartz tube high vacuum exhaust system which comprises a quartz tube, wherein an opening end of the quartz tube is connected to a vacuum pump body, a sleeve is accommodated in the opening end, a gap is formed between the sleeve and the inner wall of the quartz tube during exhaust, the sleeve and the inner wall of the quartz tube are sintered into a sealed state after the exhaust is finished, a mercury source is accommodated in a closed end of the quartz tube, the outer side of the closed end is surrounded by a cooling device and used for keeping the temperature of the mercury source below 0 ℃, and a wafer is further fixed in the quartz tube.
Preferably, in the quartz tube high-vacuum exhaust system, the cooling device is a cooling tank filled with an ice-water mixture.
Preferably, in the quartz tube high-vacuum exhaust system, the cooling device includes a cooling tank filled with a cooling liquid and a refrigerator connected to the cooling tank.
Preferably, in the above quartz tube high vacuum exhaust system, the cooling device includes a cooling tank filled with liquid nitrogen.
Preferably, in the high vacuum exhaust system for the quartz tube, a flat-head pressure ring is sleeved on the periphery of the open end of the quartz tube, a wedge-shaped pressure ring is arranged at the tail end of the connecting tube of the vacuum pump body, a sealing ring is arranged between the flat-head pressure ring and the wedge-shaped pressure ring, and the quartz tube and the vacuum pump body are hermetically connected by extrusion of the flat-head pressure ring and the wedge-shaped pressure ring.
Preferably, in the quartz tube high vacuum exhaust system, the inner layer of the cooling tank is a stainless steel layer, the outer layer of the cooling tank is a polytetrafluoroethylene layer, the middle layer of the cooling tank is a heat insulating material layer, and a cover plate is arranged above the cooling tank.
Preferably, in the quartz tube high vacuum exhaust system, the wafer is a mercury cadmium telluride wafer.
The invention provides a high vacuum exhaust method for a quartz tube, which comprises the following steps:
pumping a high vacuum to the quartz tube by using any one of the quartz tube high vacuum exhaust systems;
and sintering the quartz tube and the sleeve together to form a sealed space.
Preferably, in the above method of exhausting the high vacuum of the quartz tube, the evacuating the high vacuum of the quartz tube includes:
opening a dry pump, and vacuumizing to below 10 Pa;
opening the valve of the molecular pump, and vacuumizing to 10 DEG-2Pa below;
the ion pump was turned on and the vacuum was pulled high.
Preferably, in the above high vacuum exhaust method for a quartz tube, the quartz tube and the sleeve are sintered together by using an oxyhydrogen flame to form a sealed space.
As can be seen from the above description, according to the quartz tube high vacuum exhaust system provided by the present invention, since the mercury source is accommodated in the closed end of the quartz tube, and the outer side of the closed end is surrounded by the cooling device for maintaining the temperature of the mercury source below 0 ℃, the volatilization of mercury can be suppressed during the high vacuum exhaust process, the vacuum degree of the quartz tube can be increased, and the exhaust time can be shortened. According to the high-vacuum exhaust method for the quartz tube, due to the adoption of the exhaust system, the vacuum degree of the quartz tube can be improved, and the exhaust time is shortened.
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 diagram of an embodiment of a quartz tube high vacuum exhaust system provided by the present invention;
FIG. 2 is a schematic view of a wedge-shaped compression ring;
FIG. 3 is a schematic view of the connection of a wedge-shaped compression ring and a flat compression ring;
FIG. 4 is a schematic diagram of an embodiment of a high vacuum exhaust method for a quartz tube according to the present invention.
Detailed Description
The core of the invention is to provide a quartz tube high vacuum exhaust system and a method, which can inhibit the volatilization of mercury, improve the vacuum degree of the quartz tube, shorten the exhaust time and can be particularly used for an n-type heat treatment process in the preparation process of a mercury cadmium telluride infrared focal plane detector chip.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
An embodiment of a quartz tube high vacuum exhaust system provided by the present invention is shown in fig. 1, and fig. 1 is a schematic diagram of an embodiment of a quartz tube high vacuum exhaust system provided by the present invention, the system includes a quartz tube 1, an open end 101 of the quartz tube 1 is connected to a vacuum pump body 2, the vacuum pump body 2 can include, but is not limited to, a molecular pump, a dry pump and an ion pump, a sleeve 3 is accommodated inside the open end 101, a gap is formed between the sleeve 3 and an inner wall of the quartz tube 1 during exhaust, the sleeve 3 and the inner wall of the quartz tube 1 are sintered into a sealed state after exhaust is completed, so as to ensure that the inside of the quartz tube 1 is always in a high vacuum state in a subsequent process, a mercury source 4 is accommodated inside a closed end 102 of the quartz tube 1, the outside of the closed end 102 is surrounded by a cooling device 5 for keeping the temperature of the mercury source 4 below 0 ℃, so that, further, a wafer 6 is fixed inside the quartz tube 1.
It should be noted that, when operating the above system, a proper amount of mercury source 4 is weighed by balance, the amount of mercury source 4 must meet the saturated mercury vapor pressure in the quartz tube 1 at a set temperature, then the wafer 6 is blown clean by a nitrogen gun and placed in the quartz tube 1, then the sleeve 3 is placed in the quartz tube 1, the sleeve 3 is preferably a quartz sleeve, so as to be more matched with the quartz tube and achieve a better combination effect, then the quartz tube 1 is vertically installed on an exhaust platform, the mercury source 4 is located at the lowest end of the quartz tube 1, then a sealing ring and a lower flat head pressure ring are installed to ensure that the vacuum pump body 2 of the exhaust platform and the quartz tube 1 form a good seal, then the mercury source 4 is placed in a cooling device 5, the mercury source 4 is cooled to inhibit the volatilization of mercury, and corresponding cooling media can be selected according to different vacuum degree requirements, that is, the higher the degree of vacuum pumping is required, the lower the corresponding cooling temperature is, after the vacuum pumping is performed to the preset vacuum degree, the oxyhydrogen flame can be opened, the proper flame can be adjusted, the quartz tube 1 and the sleeve 3 are sintered together, and finally, the quartz tube 1 can be placed into an annealing furnace for annealing.
As can be seen from the above description, in the embodiment of the quartz tube high vacuum exhaust system provided by the present invention, the mercury source is accommodated in the closed end of the quartz tube, and the outer side of the closed end is surrounded by the cooling device for keeping the temperature of the mercury source below 0 ℃, so that the volatilization of mercury can be suppressed during the high vacuum exhaust process, the vacuum degree of the quartz tube can be increased, and the exhaust time can be shortened.
In one embodiment of the quartz tube high vacuum exhaust system, the cooling device 5 may be a cooling tank filled with an ice-water mixture, which is set for a general high vacuum requirement, that is, in a situation where the vacuum requirement is not high, the temperature of the mercury source may be controlled to 0 degree celsius by using the ice-water mixture, which is simple and easy to operate.
In another embodiment of the above-described quartz tube high vacuum exhaust system, with continued reference to fig. 1, the cooling device 5 may comprise a cooling tank filled with a cooling liquid and a refrigerator 501 connected to the cooling tank, which is for the case where a higher vacuum degree is required, and the refrigerator is adapted to refrigerate the cooling liquid to a temperature lower than 0 degrees celsius of the ice-water mixture, thereby controlling the non-volatilization of the mercury source at the higher vacuum degree.
In another embodiment of the above-mentioned quartz tube high vacuum exhaust system, the cooling device 5 may comprise a cooling tank filled with liquid nitrogen, which is specific to the case where ultra-high vacuum is required, and the mercury source may be directly changed into a solid state by adding liquid nitrogen into the cooling tank, so as to avoid the problem of volatilization of the mercury source during ultra-high vacuum pumping.
In an embodiment of the above high vacuum exhaust system for a quartz tube, a flat head press ring is sleeved on the periphery of the open end of the quartz tube 1, a wedge-shaped press ring is arranged at the end of a connecting pipe of a vacuum pump body, the wedge-shaped press ring is shown in fig. 2, fig. 2 is a schematic diagram of the wedge-shaped press ring, a wedge-shaped position 7 therein forms an inclined plane structure from top to bottom, referring to fig. 3, fig. 3 is a schematic diagram of the connection of the wedge-shaped press ring and the flat head press ring, a seal ring 303 is further arranged between the flat head press ring 301 and the wedge-shaped press ring 302, the flat head press ring 301 and the seal ring 303 can be extruded into the wedge-shaped position 7 of the wedge-shaped press ring 302 by utilizing the extrusion of the three, the sealing connection of.
In another preferred embodiment of the above-mentioned quartz tube high vacuum exhaust system, the inner layer of the cooling tank 5 may be a stainless steel layer, the outer layer may be a polytetrafluoroethylene layer, the middle layer may be a thermal insulation material layer, and a cover plate may be provided above the cooling tank 5. Of course, this is only a preferred solution, and other cooling slots may be selected according to actual needs, and the present invention is not limited herein.
In addition, in the quartz tube high vacuum exhaust system, the wafer can be a mercury cadmium telluride wafer.
To sum up, the system inhibits the volatilization of mercury through the mode of cooling the mercury source on the one hand, can solve the problem that the vacuum degree of the quartz tube is not high because of the continuous evaporation of mercury, avoid a large amount of oxygen atoms in the quartz tube to react with the mercury cadmium telluride on the surface of the material at high temperature to form an oxide layer, hinder the atom exchange inside and outside the surface layer, on the other hand, through optimizing the interface of the vacuum pump body and the quartz tube, adopt the design of single wedge-shaped compression ring, guarantee that the sealing ring can be closely connected with the vacuum pump body and the quartz tube under the extrusion of two compression rings, through the above improvement, not only can shorten the exhaust time, promote the process efficiency, and simultaneously can realize better n type heat treatment.
Fig. 4 shows an embodiment of a high vacuum exhaust method for a quartz tube according to the present invention, and fig. 4 is a schematic diagram of an embodiment of a high vacuum exhaust method for a quartz tube according to the present invention, the method including the following steps:
s1: pumping the quartz tube to high vacuum by using any one of the quartz tube high vacuum exhaust systems;
s2: the quartz tube and the sleeve are sintered together to form a sealed space.
Specifically, a clean quartz tube can be taken firstly, a proper amount of mercury source is weighed by using a balance, the amount of the mercury source can meet the saturated mercury vapor pressure in the quartz tube at a set temperature, then a wafer is blown clean by using a nitrogen gun and placed in the quartz tube, then a sleeve is placed in the quartz tube, the sleeve is preferably a quartz sleeve, so that the quartz tube can be matched with the quartz tube better in combination effect, then the quartz tube is vertically arranged on an exhaust table, the mercury source is positioned at the lowest end of the quartz tube, then a sealing ring and a lower flat head pressure ring are arranged, the vacuum pump body of the exhaust table is ensured to form good sealing with the quartz tube, then the mercury source is placed in a cooling device, the volatilization of mercury is inhibited by adopting a mercury source cooling method, a corresponding cooling medium can be selected according to different vacuum degree requirements, namely, the higher the degree of vacuumizing is required, the corresponding cooling temperature is lower, after the vacuum is pumped to the preset vacuum degree, oxyhydrogen flame can be opened, proper flame is adjusted, the quartz tube and the sleeve are sintered together, and finally the quartz tube can be placed into an annealing furnace for annealing process.
In one specific embodiment of the above method for high vacuum exhaust of a quartz tube, the step of pulling a high vacuum on the quartz tube may include:
opening a dry pump, and vacuumizing to below 10 Pa;
opening the valve of the molecular pump, and vacuumizing to 10 DEG-2Pa below;
the ion pump was turned on and the vacuum was pulled high.
In another embodiment of the above-described high vacuum exhaust method for a quartz tube, the quartz tube and the sleeve may be sintered together to form a sealed space using an oxyhydrogen flame.
By using the method, the volatilization of mercury can be inhibited in the high vacuum exhaust process, the vacuum degree of the quartz tube is improved, and the exhaust time is shortened.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A quartz tube high vacuum exhaust system is characterized by comprising a quartz tube, wherein an open end of the quartz tube is connected to a vacuum pump body, a sleeve is accommodated in the open end, a gap is reserved between the sleeve and the inner wall of the quartz tube during exhaust, the sleeve and the inner wall of the quartz tube are sintered into a sealed state after the exhaust is finished, a mercury source is accommodated in a closed end of the quartz tube, the outer side of the closed end is surrounded by a cooling device and used for keeping the temperature of the mercury source below 0 ℃, and a wafer is further fixed in the quartz tube.
2. The quartz tube high vacuum exhaust system according to claim 1, wherein the cooling device is a cooling tank filled with an ice-water mixture.
3. The quartz tube high-vacuum exhaust system according to claim 1, wherein the cooling device includes a cooling tank filled with a cooling liquid and a refrigerator connected to the cooling tank.
4. The quartz tube high vacuum exhaust system according to claim 1, wherein the cooling device comprises a cooling tank filled with liquid nitrogen.
5. The quartz tube high vacuum exhaust system according to any one of claims 1 to 4, wherein a flat-head press ring is sleeved on the periphery of the open end of the quartz tube, a wedge-shaped press ring is arranged at the tail end of the connecting tube of the vacuum pump body, and a sealing ring is arranged between the flat-head press ring and the wedge-shaped press ring, so that the quartz tube and the vacuum pump body are connected in a sealing manner by extrusion of the flat-head press ring and the wedge-shaped press ring.
6. The quartz tube high vacuum exhaust system according to any one of claims 2 to 4, wherein the cooling tank has an inner layer of stainless steel, an outer layer of polytetrafluoroethylene, an intermediate layer of thermal insulation material, and a cover plate above the cooling tank.
7. The quartz tube high vacuum exhaust system of any of claims 1-4, wherein the wafer is a mercury cadmium telluride wafer.
8. A high vacuum exhaust method for a quartz tube is characterized by comprising the following steps:
pumping a high vacuum to the quartz tube by using the quartz tube high vacuum exhaust system according to any one of claims 1 to 7;
and sintering the quartz tube and the sleeve together to form a sealed space.
9. The quartz tube high vacuum exhaust method according to claim 8,
the pumping the quartz tube to high vacuum comprises the following steps:
opening a dry pump, and vacuumizing to below 10 Pa;
opening the valve of the molecular pump, and vacuumizing to 10 DEG-2Pa below;
the ion pump was turned on and the vacuum was pulled high.
10. The quartz tube high vacuum exhaust method according to claim 8, wherein the quartz tube and the sleeve are sintered together with an oxyhydrogen flame to form a sealed space.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010827541.7A CN111926391A (en) | 2020-08-17 | 2020-08-17 | Quartz tube high-vacuum exhaust system and method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010827541.7A CN111926391A (en) | 2020-08-17 | 2020-08-17 | Quartz tube high-vacuum exhaust system and method |
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| CN111926391A true CN111926391A (en) | 2020-11-13 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113172215A (en) * | 2021-03-27 | 2021-07-27 | 兰州交通大学 | Alloy vacuum directional solidification device |
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| CN1178391A (en) * | 1997-09-17 | 1998-04-08 | 中国科学院上海技术物理研究所 | Heat treating apparatus for mercury self sealed mercury-cadmium tellurid for switching transistors |
| CN101159211A (en) * | 2007-10-22 | 2008-04-09 | 陈卫 | Mercury gun |
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2020
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Patent Citations (4)
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| DE1944985A1 (en) * | 1968-09-27 | 1970-05-27 | Ibm | Method and device for growing ternary epitaxial layers |
| CN2252819Y (en) * | 1996-01-19 | 1997-04-23 | 中国科学院上海技术处理研究所 | Te, Cd, Hg crystal heat treatment appts |
| CN1178391A (en) * | 1997-09-17 | 1998-04-08 | 中国科学院上海技术物理研究所 | Heat treating apparatus for mercury self sealed mercury-cadmium tellurid for switching transistors |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113172215A (en) * | 2021-03-27 | 2021-07-27 | 兰州交通大学 | Alloy vacuum directional solidification device |
| CN113172215B (en) * | 2021-03-27 | 2022-06-28 | 兰州交通大学 | Alloy vacuum directional solidification device |
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Application publication date: 20201113 |