CN116588907A - Phosphorus recovery unit, system and recovery method for molecular beam epitaxy cavity - Google Patents
Phosphorus recovery unit, system and recovery method for molecular beam epitaxy cavity Download PDFInfo
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- CN116588907A CN116588907A CN202310880689.0A CN202310880689A CN116588907A CN 116588907 A CN116588907 A CN 116588907A CN 202310880689 A CN202310880689 A CN 202310880689A CN 116588907 A CN116588907 A CN 116588907A
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 141
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 136
- 239000011574 phosphorus Substances 0.000 title claims abstract description 136
- 238000011084 recovery Methods 0.000 title claims abstract description 112
- 238000001451 molecular beam epitaxy Methods 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000002955 isolation Methods 0.000 claims abstract description 47
- 239000003595 mist Substances 0.000 claims abstract description 24
- 238000005507 spraying Methods 0.000 claims abstract description 19
- 239000002826 coolant Substances 0.000 claims description 55
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 42
- 239000007788 liquid Substances 0.000 claims description 41
- 229910052757 nitrogen Inorganic materials 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 10
- 239000007921 spray Substances 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 17
- 238000004140 cleaning Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000005669 field effect Effects 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 125000006850 spacer group Chemical group 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- 231100000644 Toxic injury Toxicity 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/003—Phosphorus
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02538—Group 13/15 materials
- H01L21/02543—Phosphides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02631—Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a phosphorus recovery unit, a system and a recovery method for a molecular beam epitaxy cavity, wherein the phosphorus recovery unit for the molecular beam epitaxy cavity comprises: the phosphorus recovery module is internally provided with a phosphorus recovery cavity, the phosphorus recovery cavity is connected with a first channel, the first channel is used for being connected with the MBE system cavity, and a first isolation element is arranged on the first channel; a cold trap and a vacuum water mist spraying module are arranged in the phosphorus recovery cavity; a vacuum pump connected to the phosphorus recovery chamber through a second channel. According to the invention, after phosphorus is condensed on the surface of the cold trap, a layer of ice is covered outside the phosphorus material by the vacuum water mist spraying module, so that the effect of isolating air is achieved.
Description
Technical Field
The invention relates to the technical field of semiconductor manufacturing, in particular to a phosphorus recovery unit, a system and a recovery method for a molecular beam epitaxy cavity.
Background
In molecular beam epitaxy (molecular beam epitaxy, MBE) systems, materials are synthesized by evaporating a solid source under ultra-high vacuum and depositing directly onto a substrate.
The phosphorus source is a common source material for MBE growth, and MBE growth phosphide is widely applied to lasers, radars, detectors and high-frequency communication devices. However, MBE technology inevitably presents a problem in that a large amount of material is evaporated into the chamber and deposited on the chamber surfaces cannot be removed.
Phosphorus, especially white phosphorus, has very low burning points due to the characteristics of loose texture, so that MBE cavity in which phosphide grows is very difficult to maintain, and safety accidents are frequent; smoke generated by the combustion of the phosphorus material also causes physiological toxic injury to the use and maintenance personnel of the on-site MBE.
To solve this problem, the current mainstream method is to use a phosphorus recovery system on the MBE system, specifically as follows: before MBE finishes maintaining the growth open cavity, the redundant phosphorus material in the cavity is driven into a phosphorus recovery unit cooled by liquid nitrogen by high-temperature baking, the phosphorus recovery unit is isolated from the cavity by a valve after baking, and then the phosphorus recovery unit is treated independently.
However, this method has the following problems: when the phosphorus recovery unit is treated independently, a great amount of phosphorus material still cannot be prevented from contacting with air and knocking is generated, so that safety accidents are caused, and a more perfect mechanism for isolating the air is needed.
Therefore, the design of the more complete phosphide MBE cavity phosphorus recovery unit has important significance for equipment maintenance, EHS (Environment, health, safety, health, safety and environmental integrated management) protection and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention discloses a phosphorus recovery unit, a system and a recovery method for a molecular beam epitaxy cavity.
The technical scheme adopted by the invention is as follows:
a phosphorus recovery unit for use in a molecular beam epitaxy chamber, comprising:
the device comprises a phosphorus recovery module, wherein a phosphorus recovery cavity is formed in the phosphorus recovery module, the phosphorus recovery cavity is connected with a first channel, the first channel is used for being connected with an MBE system cavity, and a first isolation element is arranged on the first channel; a cold trap and a vacuum water mist spraying module are arranged in the phosphorus recovery cavity;
a vacuum pump connected to the phosphorus recovery chamber through a second channel.
In one embodiment of the invention, the cold trap comprises a cold trap pipe on which a coolant inlet and a coolant outlet are arranged, which coolant inlet and coolant outlet extend outside the phosphorus recovery module.
In one embodiment of the present invention, the cooling device further comprises a cooling agent supply module, wherein the cooling agent supply module comprises a gas-liquid separator, a gas containing space and a liquid containing space are formed inside the gas-liquid separator, a cooling agent circulation outlet, a cooling agent circulation inlet, a cooling agent supplementing port and an exhaust port are respectively arranged on the gas-liquid separator, and the cooling agent circulation outlet and the cooling agent circulation inlet are respectively connected with the cooling agent inlet and the cooling agent outlet of the cold trap; the coolant circulation outlet is communicated with the space containing liquid in the gas-liquid separator, and the exhaust port is communicated with the space containing gas in the gas-liquid separator.
In one embodiment of the invention, the coolant is liquid nitrogen.
In one embodiment of the invention, the coolant replenishment port is provided with a first control element.
In one embodiment of the invention, the vacuum water mist spraying module comprises an atomizer and a water source which are connected through a pipeline, the pipeline is provided with a second control element and a third control element, the second control element controls water mist to enter the phosphorus recovery cavity, and the third control element controls water inflow of the water source.
In one embodiment of the invention, a second spacer element is provided on the second channel.
In one embodiment of the invention, a third isolation element is provided between the vacuum pump and the phosphorus recovery module.
A method for a phosphorus recovery unit in a molecular beam epitaxy chamber based on the above, characterized by comprising the steps of:
s1, connecting a first channel of the phosphorus recovery unit with an outlet of an MBE system cavity, wherein a third isolation element is arranged on the outlet of the MBE system cavity;
s2, starting a vacuum pump to enable the pressure in the phosphorus recovery cavity to be lower than the atmospheric pressure; introducing a coolant into the cold trap in the phosphorus recovery cavity, and starting the first isolation element and the third isolation element to drive phosphorus in the MBE system cavity into the phosphorus recovery cavity through baking;
s3, closing the first isolation element and the third isolation element, stopping introducing the coolant into the cold trap, and spraying water mist to the phosphorus recovery cavity by the water mist spraying module to enable the surface of phosphorus on the cold trap to condense an ice layer;
s4, disconnecting the first channel of the phosphorus recovery unit from the molecular beam epitaxy cavity, and processing phosphorus in the phosphorus recovery unit.
A phosphorus recovery system for use in a molecular beam epitaxy chamber, comprising:
the cavity of the MBE system is provided with a cavity,
and a phosphorus recovery unit as described above for use in a molecular beam epitaxy chamber.
Compared with the prior art, the technical scheme of the invention has the following advantages:
the system for cleaning the phosphor material in the molecular beam epitaxy cavity can effectively solve the problems in the phosphor material treatment of the phosphide MBE cavity: the independent liquid nitrogen cooling recovery unit can effectively separate and capture the phosphide in the MBE cavity; the water spraying device can cover an ice layer on the surface of the captured phosphorus material, so that contact between phosphorus and air is effectively isolated, the risk of leakage of fire and harmful substances is greatly reduced, and the operation safety is greatly improved.
Drawings
In order that the invention may be more readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings.
FIG. 1 is a schematic diagram of a system for cleaning phosphor materials in a molecular beam epitaxy chamber in accordance with the present invention.
Fig. 2 is a schematic view of a phosphorus recovery module in accordance with the present invention.
Fig. 3 is a schematic view of a coolant supply module in accordance with the present invention.
Fig. 4 is a schematic view of a vacuum mist spray module.
Description of the specification reference numerals: 1. MBE system cavity; 2. a first isolation element; 3. a second isolation element; 4. a phosphorus recovery module; 5. a third isolation element; 6. a vacuum pump; 7. a phosphorus recovery cavity; 8. a cold trap; 9. a vacuum water mist spraying module; 10. a coolant circulation outlet; 11. a coolant circulation inlet; 12. a coolant supply module; 13. a coolant replenishment port; 14. an exhaust port; 15. a first control element; 16. a second control element; 17. a third control element; 18. and (3) a water source.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the invention and practice it.
The foregoing and other features, aspects and advantages of the present invention will become more apparent from the following detailed description of the embodiments, read in conjunction with the accompanying drawings. The directional terms mentioned in the following embodiments are, for example: upper, lower, left, right, front or rear, etc., are merely references to the directions of the drawings. Thus, directional terminology is used for the purpose of illustration and is not intended to be limiting of the invention, and furthermore, like reference numerals refer to like elements throughout the embodiments.
MBE (Molecular Beam Epitaxy ) is used as a vacuum evaporation form, has advantages in material chemical composition, growth rate control and the like, is very suitable for homojunction and heterojunction epitaxial growth of various compound semiconductors and alloy materials thereof, and plays an important role in preparation of microwave, millimeter wave devices, circuits and photoelectric devices such as technical semiconductor field effect transistors (MESFETs), high Electron Mobility Transistors (HEMTs), heterostructure Field Effect Transistors (HFETs), heterojunction Bipolar Transistors (HBTs) and the like.
Phosphorus sources are a common source material for MBE growth and are extremely reactive with oxygen due to the fact that phosphorus, especially white phosphorus. Compared with the traditional phosphorus recovery mode, such as using a cold pump or a diffusion pump with an MBE cavity to recover phosphorus, a large amount of phosphorus enters a vacuum pump, so that the service life of the vacuum pump is seriously lost; while vacuum pump maintenance is still subject to serious fire risks. The accidents of fire disaster caused by maintaining the phosphorus-containing cavity occur in a plurality of MBE epitaxial wafer production enterprises at home and abroad. The diffusion pump uses oil vapor as a vacuum maintaining medium, so that huge pollution hidden danger is brought to the MBE system cavity, and the diffusion pump is gradually eliminated at present. Similar problems can be completely avoided by using a separate liquid nitrogen cooled phosphorus recovery device. However, the existing independent liquid nitrogen cooling phosphorus recovery device still faces a certain risk of exposing air when the phosphorus recovery device is used for treatment.
To this end, the invention provides a phosphorus recovery unit, system and recovery method for use in a molecular beam epitaxy chamber.
Example 1:
referring to fig. 1 and 2, a phosphorus recovery unit for use in a molecular beam epitaxy chamber, comprising:
the phosphorus recovery module 4, the phosphorus recovery cavity 7 is formed in the phosphorus recovery module 4, the phosphorus recovery cavity 7 is connected with a first channel, the first channel is used for connecting the MBE system cavity 1, and the first channel is provided with a first isolation element 2; a cold trap 8 and a vacuum water mist spraying module 9 are arranged in the phosphorus recovery cavity 7;
a vacuum pump 6 connected to the phosphorus recovery chamber 7 through a second passage for maintaining a vacuum state of the phosphorus recovery module 4.
Wherein, when the cold trap 8 executes phosphorus recovery operation, liquid nitrogen is introduced to adsorb phosphorus vapor baked out from the MBE system cavity 1; the cold trap 8 is thus provided with a coolant circulation outlet 10 and a coolant circulation inlet 11, the arrows in fig. 2 indicating the direction of liquid nitrogen ingress and egress.
Specifically, as shown in fig. 4, the vacuum water mist spraying module 9 comprises an atomizer and a water source 18 which are connected through a pipeline, the pipeline is provided with a second control element 16 and a third control element 17, the second control element 16 controls water mist to enter the phosphorus recovery cavity 7, and the third control element 17 controls water inflow of the water source 18. Further, the second control element 16 and the third control element 17 are electrically controlled valves. The water source 18 is deionized water at a constant pressure.
The second channel is provided with a second spacer element 3.
A third isolation element 5 is provided between the vacuum pump 6 and the phosphorus recovery module 4. Further, the first isolation element 2 is an isolation gate valve, the second isolation element 3 is a vacuum isolation valve, and the third isolation element 5 is a vacuum isolation valve. The second and third insulating members 3 and 5 serve to maintain the vacuum state of the phosphorus recovery module 4 at the completion of the phosphorus material recovery work and to prevent the phosphorus material from leaking out. Generally, there is no need for ultra-high vacuum sealing between the MBE system cavity 1 and the phosphorus recovery module 4 and between the phosphorus recovery module 4 and the vacuum pump 6, and the use frequency is extremely low, and a manual vacuum isolation valve is adopted.
The working principle of this embodiment is as follows:
s1, keeping a first isolation element 2, a second isolation element 3 and a third isolation element 5 in an open state, wherein an MBE system cavity 1, a phosphorus recovery module 4 and a vacuum pump 6 are communicated with each other, and liquid nitrogen is introduced into a cold trap 8; it should be noted that, in this step, the volume of the cold trap 8 into which the liquid nitrogen is introduced only needs to ensure that the temperature in the cold trap 8 approaches the temperature of the liquid nitrogen during the baking in step S2 of the MBE system cavity 1.
S2, driving the phosphorus in the MBE system cavity 1 into a phosphorus recovery module 4 through baking; in the step, the baking temperature is more than or equal to 200 ℃, so that residual impurity materials in each vacuum chamber of the MBE system are removed as much as possible. The principle of phosphorus entering the phosphorus recovery module 4 in this step is as follows: because the saturated vapor pressure of phosphorus is very high, phosphorus condensed in the MBE system cavity 1 is easily evaporated or sublimated to form gas, the gas flows to the phosphorus recovery module 4, liquid nitrogen is introduced into the phosphorus recovery module 4, the temperature is about-190 ℃, and gas molecules reaching the position can be condensed to realize interception. The phosphorus recovery module 4 does not participate in baking of the MBE system.
S3, closing the first isolation element 2, the second isolation element 3 and the third isolation element 5 to enable the MBE system cavity 1, the phosphorus recovery module 4 and the vacuum pump 6 to be separated, and stopping introducing liquid nitrogen into the cold trap 8;
and S4, before the cold trap 8 is warmed to a preset temperature, opening a vacuum water mist spraying module 9 to enable the surface of phosphorus on the cold trap 8 to condense an ice layer. Further, the preset temperature is more than or equal to minus 30 ℃.
It should be noted that the vacuum water mist spray module 9 must be started with both the second and third isolation elements 3, 5 closed, otherwise there is a risk of water contaminating the MBE system cavity 1 or damaging the vacuum pump 6. The specific principle is as follows: the constant pressure deionized water source is used for supplying water, and the deionized water faucet which is directly installed in a purifying room is generally used. When in use, the third control element 17 is opened first, so that water enters the atomizer; thereafter the second control element 16 is opened, whereupon the mist of water produced by the atomizer is flushed into the phosphorus recovery module 4, and rapidly condenses on the cold trap 8, whereupon the temperature of the cold trap 8 remains around-190 ℃.
The reason for using the vacuum mist spray module 9 instead of directly feeding water here is as follows: the water flow pressure is generally larger and the coverage area is smaller, so that the whole cold trap 8 is difficult to uniformly cover; the vacuum water mist spraying module 9 solves the problems well, and can well control the water inflow while spraying water in a large range, so that the controllability of the whole spraying process is greatly improved. If the atomizer is not used, it is easy for the part of the cold trap 8 facing the water inlet to be already covered with a thicker layer of ice, while the part far from the water inlet is not covered with the layer of ice.
S5, after the ice layer is condensed, the phosphorus recovery module 4 is disassembled and transferred to a waste treatment tank for innocent treatment. It should be noted that, in the process of disassembly and transfer, the first isolation element 2, the second isolation element 3 and the third isolation element 5 need to be kept in a closed state, and the second isolation element 3 and the third isolation element 5 need to be opened quickly, so that the ice layer is not melted before the second isolation element 3 and the third isolation element 5 are opened for innocent treatment.
Example 2:
as shown in fig. 3, the cleaning system for phosphorus material in a molecular beam epitaxy chamber further comprises a coolant supply module 12 based on embodiment 1, the coolant supply module 12 comprising a gas phase separator provided with a coolant circulation outlet 10, a coolant circulation inlet 11, a coolant replenishment inlet 13 and an exhaust port 14, the coolant circulation outlet 10 and the coolant circulation inlet 11 being connected to the cold trap 8.
Wherein, the coolant can be liquid nitrogen. Typically, the coolant make-up port 13 is connected to a storage tank that feeds liquid nitrogen into the vapor phase separator. The arrow indication direction in fig. 3 is the entering direction of external liquid nitrogen source, the flowing direction of gas-liquid mixed medium discharged from the coolant circulation inlet 11 of the cold trap 8, the flowing direction of liquid nitrogen from the gas phase separator into the coolant circulation outlet 10 of the cold trap 8 and the discharging direction of gas, respectively from left to right.
Further, the coolant supplementing port 13 is provided with a first control element 15, and the first control element 15 can adopt an electric control valve capable of automatically regulating and controlling the liquid level, and the method for automatically regulating and controlling the liquid level is to detect the liquid level by using an electric, pneumatic or hydraulic control system and the like through a sensor, so that the automatic control of the liquid level is realized, the production efficiency can be greatly improved, the manual intervention is reduced, and higher cost is required to be input.
It should be noted that it is only necessary to ensure that the temperature in the cold trap approaches the liquid nitrogen temperature during baking, so the simplest way is to manually add liquid nitrogen to the liquid nitrogen inlet of the cold trap 8 via a stainless steel funnel. Of course, liquid nitrogen gas-liquid separators commonly found in MBE plants can also be used, but are correspondingly costly, selected and adjusted as needed by those skilled in the art.
Example 3:
a phosphorus recovery system for use in a molecular beam epitaxy chamber, comprising:
the MBE system cavity 1,
and a phosphorus recovery unit for use in a molecular beam epitaxy chamber as provided in example 2.
The working principle of this embodiment is as follows:
s1, connecting a first channel of a phosphorus recovery unit with an outlet of an MBE system cavity 1, wherein a third isolation element 5 is arranged on the outlet of the MBE system cavity 1;
s2, starting a vacuum pump 6 to enable the pressure in the phosphorus recovery cavity 7 to be lower than the atmospheric pressure; introducing a coolant into a cold trap 8 in the phosphorus recovery cavity 7, and starting the first isolation element 2 and the third isolation element 5 to drive phosphorus in the MBE system cavity 1 into the phosphorus recovery cavity 7 through baking;
s3, closing the first isolation element 2 and the third isolation element 5, stopping introducing the coolant into the cold trap 8, and spraying water mist to the phosphorus recovery cavity 7 by the water mist spraying module to enable the phosphorus on the cold trap 8 to have an ice layer condensed on the surface;
s4, disconnecting the first channel of the phosphorus recovery unit from the molecular beam epitaxy cavity, and treating phosphorus in the phosphorus recovery unit.
In the description of the embodiments of the present invention, it should also be noted that, unless explicitly specified and limited otherwise, the terms "disposed," "connected," and "connected" should be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations and modifications of the present invention will be apparent to those of ordinary skill in the art in light of the foregoing description. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (10)
1. A phosphorus recovery unit for use in a molecular beam epitaxy chamber, comprising:
the device comprises a phosphorus recovery module (4), wherein a phosphorus recovery cavity (7) is formed in the phosphorus recovery module (4), the phosphorus recovery cavity (7) is connected with a first channel, the first channel is used for being connected with an MBE system cavity (1), and a first isolation element (2) is arranged on the first channel; a cold trap (8) and a vacuum water mist spraying module (9) are arranged in the phosphorus recovery cavity (7);
a vacuum pump (6) connected to the phosphorus recovery chamber (7) through a second channel.
2. The phosphorus recovery unit for use in a molecular beam epitaxy chamber according to claim 1, characterized in that the cold trap (8) comprises a cold trap tube on which a coolant inlet and a coolant outlet are provided, which extend outside the phosphorus recovery module (4).
3. The phosphorus recovery unit for use in a molecular beam epitaxy chamber according to claim 2, further comprising a coolant supply module (12), the coolant supply module (12) comprising a gas-liquid separator, the gas-liquid separator having a gas-containing space and a liquid-containing space formed therein, the gas-liquid separator having a coolant circulation outlet (10), a coolant circulation inlet (11), a coolant replenishment inlet (13) and an exhaust outlet (14), respectively, the coolant circulation outlet (10), the coolant circulation inlet (11) being connected to a coolant inlet and a coolant outlet of the cold trap (8), respectively; the coolant circulation outlet (10) communicates with the space containing the liquid in the gas-liquid separator, and the exhaust port communicates with the space containing the gas in the gas-liquid separator.
4. A phosphorus recovery unit for use in a molecular beam epitaxy chamber according to claim 3, wherein said coolant is liquid nitrogen.
5. A phosphorus recovery unit for use in a molecular beam epitaxy chamber according to claim 3, characterized in that the coolant replenishment port (13) is provided with a first control element (15).
6. Phosphorus recovery unit for use in a molecular beam epitaxy chamber according to claim 1, characterized in that the vacuum mist spray module (9) comprises an atomizer and a water source (18) connected by a pipe, the pipe being provided with a second control element (16) and a third control element (17), the second control element (16) controlling the water mist entering the phosphorus recovery chamber (7), the third control element (17) controlling the water intake of the water source (18).
7. Phosphorus recovery unit for use in a molecular beam epitaxy chamber according to claim 1, characterized in that the second channel is provided with a second isolation element (3).
8. The phosphorus recovery unit for use in a molecular beam epitaxy chamber according to claim 1, characterized in that a third isolation element (5) is provided between the vacuum pump (6) and the phosphorus recovery module (4).
9. A method for a phosphorus recovery unit in a molecular beam epitaxy chamber based on any one of claims 1 to 8, comprising the steps of:
s1, connecting a first channel of the phosphorus recovery unit with an outlet of an MBE system cavity (1), wherein a third isolation element (5) is arranged on the outlet of the MBE system cavity (1);
s2, starting a vacuum pump (6) to enable the pressure in the phosphorus recovery cavity (7) to be lower than the atmospheric pressure; introducing a coolant into a cold trap (8) in the phosphorus recovery cavity (7), and starting a first isolation element (2) and a third isolation element (5) to drive phosphorus in the MBE system cavity (1) into the phosphorus recovery cavity (7) through baking;
s3, closing the first isolation element (2) and the third isolation element (5), stopping introducing the coolant into the cold trap (8), and spraying water mist to the phosphorus recovery cavity (7) by the water mist spraying module to enable the phosphorus on the cold trap (8) to be condensed into an ice layer on the surface;
s4, disconnecting the first channel of the phosphorus recovery unit from the molecular beam epitaxy cavity, and processing phosphorus in the phosphorus recovery unit.
10. A phosphorus recovery system for use in a molecular beam epitaxy chamber, comprising:
MBE system cavity (1),
and a phosphorus recovery unit for use in a molecular beam epitaxy chamber according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310880689.0A CN116588907B (en) | 2023-07-18 | 2023-07-18 | Phosphorus recovery unit, system and recovery method for molecular beam epitaxy cavity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310880689.0A CN116588907B (en) | 2023-07-18 | 2023-07-18 | Phosphorus recovery unit, system and recovery method for molecular beam epitaxy cavity |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116588907A true CN116588907A (en) | 2023-08-15 |
| CN116588907B CN116588907B (en) | 2023-10-27 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2050796A (en) * | 1932-10-25 | 1936-08-11 | Kerschbaum Friedrich Paul | Recovery of phosphorus |
| US6408860B1 (en) * | 2000-09-21 | 2002-06-25 | Trw Inc. | Method for cleaning phosphorus from an MBE chamber |
| DE102007054851A1 (en) * | 2007-11-16 | 2009-05-20 | Createc Fischer & Co. Gmbh | MBE facility and method of operation |
| CN112408344A (en) * | 2020-09-30 | 2021-02-26 | 无锡中科德芯光电感知技术研究院有限公司 | Method for converting white phosphorus |
| CN214612846U (en) * | 2021-05-12 | 2021-11-05 | 新磊半导体科技（苏州）有限公司 | Phosphorus source furnace with temperature control for molecular beam epitaxy equipment |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2050796A (en) * | 1932-10-25 | 1936-08-11 | Kerschbaum Friedrich Paul | Recovery of phosphorus |
| US6408860B1 (en) * | 2000-09-21 | 2002-06-25 | Trw Inc. | Method for cleaning phosphorus from an MBE chamber |
| DE102007054851A1 (en) * | 2007-11-16 | 2009-05-20 | Createc Fischer & Co. Gmbh | MBE facility and method of operation |
| CN112408344A (en) * | 2020-09-30 | 2021-02-26 | 无锡中科德芯光电感知技术研究院有限公司 | Method for converting white phosphorus |
| CN214612846U (en) * | 2021-05-12 | 2021-11-05 | 新磊半导体科技（苏州）有限公司 | Phosphorus source furnace with temperature control for molecular beam epitaxy equipment |
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