CN115386960B - Mercury source furnace and method for supplementing mercury liquid - Google Patents
Mercury source furnace and method for supplementing mercury liquid Download PDFInfo
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- CN115386960B CN115386960B CN202211137323.6A CN202211137323A CN115386960B CN 115386960 B CN115386960 B CN 115386960B CN 202211137323 A CN202211137323 A CN 202211137323A CN 115386960 B CN115386960 B CN 115386960B
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- valve
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- charging bucket
- vacuum
- source furnace
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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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a mercury source furnace which comprises a charging bucket, a valve control assembly, a conveying pipeline and a jet pipe, wherein the charging bucket, the conveying pipeline and the jet pipe are positioned outside a vacuum chamber, the charging bucket, the conveying pipeline and the jet pipe are sequentially communicated, a vacuum valve, a liquid injection valve and a liquid discharge valve are arranged on the charging bucket, the valve control assembly is arranged on the conveying pipeline, the valve control assembly comprises a stop valve and a metering valve which are connected in parallel, and the conductance of the stop valve is larger than that of the metering valve. The invention uses the metering valve with smaller conductance to control the mercury flow, reduces the influence of the valve switch on the mercury vapor pressure in the charging bucket, has good beam stability, high control precision and quick response speed; the high-vacuum state is obtained by using the large-conductance stop valve and the pump set of the vacuum chamber, and an additional mercury liquid supplementing device is not required to be configured, so that the structure is simple and effective, and the rapid mercury liquid supplementing can be realized under the condition that the vacuum environment of the growth chamber is not damaged.
Description
Technical Field
The invention relates to a semiconductor device and a using method thereof, in particular to a mercury source furnace and a method for supplementing mercury liquid.
Background
Tellurium-cadmium-mercury materials are always in the mainstream position in the technical field of infrared detectors, and detectors prepared from the tellurium-cadmium-mercury materials can cover the whole infrared band, and the detectors in all the bands show excellent performance from short waves to very long waves. The mainstream molecular beam epitaxy technology of the mercury cadmium telluride material has been successfully converted from 3 inches to 4 inches growth, so as to meet the various index requirements of engineering application on the mercury cadmium telluride material.
The design of a mercury source furnace in a mercury cadmium telluride molecular beam epitaxy device is extremely critical, which is determined by the specificity of mercury: mercury is in a liquid state at normal temperature, the mercury vapor pressure is extremely sensitive to temperature change and is far higher than that of other solid source materials, the adhesion coefficient of mercury is only one percent to one thousandth of that of tellurium and cadmium, the consumption of mercury is large in the epitaxial growth process of tellurium-cadmium mercury materials, and the loading capacity of mercury often restricts the number of pieces of materials capable of continuously growing, so that the mercury source furnace is required to realize rapid mercury liquid replenishment under the condition of not damaging the vacuum environment of a growth chamber.
The gas flows through the narrow pores, when the pressure difference between the upstream and the downstream is large enough, the blocking flow phenomenon can be generated, the gas flow mainly depends on the air pressure of the upstream high-pressure side, and the downstream flow Q down And upstream pressure P up In a linear relationship Q down ＝C(T,γ,M,r)·P up Where C is conductance at the orifice, and is related to the temperature T of the gas, the heat capacity ratio gamma, the molecular weight M and the pore radius r. When the mercury source furnace works at the process temperature, the pressure in the upstream charging tank is in the order of magnitude of several Torr, and the pressure in the downstream vacuum chamber is 10 -7 ～10 -6 The Torr level, the valve is equivalent to an orifice, the pressure difference between two sides is extremely large, and the condition of generating the blocking flow is met.
The existing mercury source furnace is provided with only one valve between a charging tank and a vacuum chamber for flow control, and is provided with an additional mercury liquid supplementing device, wherein the mercury liquid supplementing device comprises a supplementing charging tank, an isolating valve, an injection/drainage pipeline, an inflation valve, an extraction valve, a liquid level monitoring device and the like. When loading and unloading, firstly, closing the isolating valve between the mercury source furnace charging tank and the supplementary charging tank, completing the mercury liquid filling operation of the supplementary charging tank, then opening the isolating valve, and hydraulically feeding the mercury in the supplementary charging tank into the mercury source furnace charging tank through the nitrogen filling operation of the supplementary charging tank, or evacuating the mercury liquid in the mercury source furnace charging tank into the supplementary charging tank through the vacuumizing operation of the supplementary charging tank, thereby having more complex operation.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and providing the mercury source furnace which has a simple structure and is convenient to operate and can realize rapid mercury liquid replenishment under the condition of not damaging the vacuum environment of a growth chamber.
The invention further provides a method for supplementing mercury liquid for the mercury liquid furnace.
In order to solve the technical problems, the invention adopts the following technical scheme:
the utility model provides a mercury source stove, includes that is located the outside material jar of vacuum chamber, valve accuse subassembly, pipeline and is located the inside injection pipe of vacuum chamber, the material jar pipeline with the injection pipe communicates in proper order, be equipped with vacuum valve, notes liquid valve and flowing back valve on the material jar, valve accuse subassembly is located on the pipeline, valve accuse subassembly includes parallelly connected stop valve and metering valve, the conductance of stop valve is greater than the conductance of metering valve.
As a further improvement of the above technical scheme: the temperature of the charging bucket, the valve control assembly, the conveying pipeline and the injection pipe is gradually increased along the conveying direction of mercury vapor.
As a further improvement of the above technical scheme: the temperature of the charging bucket is 180-190 ℃, the temperature of the valve control assembly is 190-200 ℃, the temperature of the conveying pipeline is 200-210 ℃, and the temperature of the injection pipe is 350-400 ℃.
As a further improvement of the above technical scheme: the material tank is provided with a material tank heater, the valve control assembly is provided with a valve heater or a heater shared by the valve control assembly and the material tank, and the injection pipe is provided with an injection pipe heater.
As a further improvement of the above technical scheme: and a liquid level sensor is also arranged on the charging bucket.
As a further improvement of the above technical scheme: the stop valve is an all-metal angle valve.
As a further improvement of the above technical scheme: the metering valve is a needle valve.
As a further improvement of the above technical scheme: the delivery pipeline is close to the one end of injection pipe is the bellows to dispose the bellows heating mantle.
As a further improvement of the above technical scheme: the valve control assembly is arranged at one end of the conveying pipeline, which is close to the charging bucket.
The method for supplementing mercury liquid for the mercury source furnace comprises the following steps:
s1, closing the stop valve and the metering valve, and opening the vacuum valve to be externally connected with a nitrogen pipeline for inflation operation;
s2, after the charging bucket is restored to a normal pressure state, opening the liquid injection valve to complete mercury liquid supplementing operation, and then closing the liquid injection valve;
s3, performing pre-vacuumizing operation through the external rough pump of the vacuum valve, closing the vacuum valve after the charging bucket reaches the designed vacuum degree, opening the stop valve, pumping the charging bucket to a high vacuum state through the pump group in the vacuum chamber, and closing the stop valve.
Compared with the prior art, the invention has the advantages that: the mercury source furnace disclosed by the invention has the advantages that the mercury flow is controlled by the metering valve with smaller conductance, the influence of a valve switch on the mercury vapor pressure in the charging bucket is reduced, the beam stability is good, the control precision is high, and the response speed is high; the high-vacuum state is obtained by using the large-conductance stop valve and the pump set of the vacuum chamber, and an additional mercury liquid supplementing device is not required to be configured, so that the structure is simple and effective, and the rapid mercury liquid supplementing can be realized under the condition that the vacuum environment of the growth chamber is not damaged.
The method for supplementing the mercury liquid in the mercury source furnace disclosed by the invention is simple to operate, and can realize rapid mercury liquid supplementation without damaging the vacuum environment of the growth chamber.
Drawings
Fig. 1 is a schematic view of the structure of a mercury source furnace of the present invention.
In the drawings, each reference numeral represents 1, furnace body: 11. a charging bucket; 12. a tank heater; 13. a vacuum valve; 14. a liquid injection valve; 15. a liquid discharge valve; 2. a valve control assembly; 21. a stop valve; 22. a metering valve; 23. a valve heater; 3. a delivery conduit; 4. a jet pipe; 41. a mounting flange; 42. a jet pipe heater; 5. a vacuum chamber.
Detailed Description
The invention is described in further detail below with reference to the drawings and specific examples of the specification.
Fig. 1 shows an embodiment of the mercury source furnace of the present invention, which comprises a furnace body 1 located outside a vacuum chamber 5, a valve control assembly 2, a transport pipe 3 and a lance 4 mounted inside the vacuum chamber 5.
The furnace body 1 includes a tank 11 for holding mercury liquid, a tank heater 12 for heating mercury liquid, a vacuum valve 13 for preliminary evacuation and inflation operation, a liquid filling valve 14 for filling mercury liquid, a liquid discharge valve 15 for discharging mercury liquid, and a liquid level sensor (not shown in the figure) for monitoring the position of mercury liquid. Preferably, the material of the material tank 11 is 316L stainless steel with a capacity of 500cc, 1000cc or more. The charging bucket heater 12 is a resistance heater or a PBN/PG/PBN heater, adopts an upper and a lower dual temperature areas or a plurality of temperature areas for heating, corresponds to dual thermocouple or multi thermocouple temperature measurement, and carries out PID accurate temperature control through an European table. The vacuum valve 13 can be externally connected with a rough pump or a nitrogen pipeline respectively. The liquid filling valve 14 and the liquid discharging valve 15 are respectively positioned on the upper side and the lower side of the charging bucket 11, and the liquid level sensor can realize multi-liquid level monitoring.
The valve control assembly 2 comprises a shut-off valve 21, a metering valve 22 and a valve heater 23 for valve heating, preferably arranged at the end of the delivery conduit 3 near the feed tank 11. The shut-off valve 21 and the metering valve 22 are connected in parallel via the feed line 3 to the feed tank 11 and the injection line 4, respectively. The shut-off valve 21 has a high conductance for rapidly reaching a high vacuum state, so that no additional mercury-liquid replenishing means need be provided. The metering valve 22 has a low conductance for precisely regulating the flow of mercury vapor and minimizing the effect of the valve switch on the mercury vapor pressure in the tank. Preferably, the shut-off valve 21 is an all-metal angle valve. The metering valve 22 is a needle valve, is resistant to 230 ℃ high temperature, is driven by a servo motor or a stepping motor, and can realize accurate adjustment of mercury vapor flow. The valve heater 23 is a resistance heater or a heating sleeve, has a temperature measurement and control function, and the valve control assembly 2 can also share the heater above the charging bucket 11.
The conveying pipeline 3 is used for connecting the charging bucket 11, the valve control assembly 2 and the injection pipe 4, and is preferably made of 316L stainless steel, the part of the conveying pipeline 3 between the valve control assembly 2 and the injection pipe 4 is a corrugated pipe (not shown in the figure), and further the corrugated pipe is provided with a corrugated pipe heating sleeve.
The ejector tube 4 is located inside the vacuum chamber 5, is mounted on a mounting flange 41 connected to the vacuum chamber 5, and is provided with an ejector tube heater 42. Preferably, the part of the injection tube 4 in direct contact with mercury vapor is made of high-purity tantalum. The jet pipe heater 42 is a PBN/PG/PBN heater or a tantalum wire heater, and is used for measuring temperature through a thermocouple and performing PID accurate temperature control through an European table.
The inside of the feed tank 11, the valve control assembly 2, the delivery pipe 3 and the injection pipe 4 maintain a gradually increasing temperature gradient in the direction of mercury vapor transport to prevent mercury vapor condensation at the pipe or valve. For example, the temperature of the tank 11 is controlled to 180 ℃ to 190 ℃, the temperature of the valve control assembly 2 is controlled to 190 ℃ to 200 ℃, the temperature of the bellows part of the conveying pipeline 3 is controlled to 200 ℃ to 210 ℃, and the temperature of the injection pipe 4 is controlled to 350 ℃ to 400 ℃ by reasonably setting the set temperatures and output powers of the tank heater 12, the valve heater 23, the injection pipe heater 42 and the bellows heating jacket.
The parts of the tank 11, the valve control assembly 2, the conveying pipeline 3 and the injection pipe 4, which are in direct contact with mercury vapor, such as a tank body, the inner wall of a pipeline, a valve core and the like, are made of 316L stainless steel or other materials which do not react with mercury vapor.
When the mercury liquid is needed to be replenished, the stop valve 21 and the metering valve 22 are closed firstly, the vacuum valve 13 is opened to be externally connected with a nitrogen pipeline for inflation operation, after the charging tank 11 is restored to the normal pressure state, the liquid injection valve 14 is opened to complete the mercury liquid replenishing operation, the liquid injection valve 14 is closed, the preliminary vacuumizing operation is carried out through the vacuum valve 13 which is externally connected with a rough vacuumizing pump, after the charging tank 11 reaches a certain vacuum degree, the vacuum valve 13 is closed, the stop valve 21 is opened again, finally, the charging tank 11 is pumped to the high vacuum state through a pump group (such as a cryopump, an ion pump and the like) in the vacuum chamber 5, and the stop valve 21 is closed.
While the invention has been described with reference to preferred embodiments, it is not intended to be limiting. Many possible variations and modifications of the disclosed technology can be made by anyone skilled in the art, or equivalent embodiments with equivalent variations can be made, without departing from the scope of the invention. Therefore, any simple modification, equivalent variation and modification of the above embodiments according to the technical substance of the present invention shall fall within the scope of the technical solution of the present invention.
Claims (10)
1. A mercury source furnace, characterized in that: including being located outside material jar (11), valve accuse subassembly (2), pipeline (3) and being located inside injection pipe (4) of vacuum chamber (5), material jar (11) pipeline (3) with injection pipe (4) communicate in proper order, be equipped with vacuum valve (13), notes liquid valve (14) and flowing back valve (15) on material jar (11), valve accuse subassembly (2) are located on pipeline (3), valve accuse subassembly (2) include parallelly connected stop valve (21) and metering valve (22), the conductance of stop valve (21) is greater than the conductance of metering valve (22).
2. The mercury source furnace of claim 1, wherein: the temperature of the charging bucket (11), the valve control assembly (2), the conveying pipeline (3) and the injection pipe (4) is gradually increased along the conveying direction of mercury vapor.
3. The mercury source furnace of claim 2, wherein: the temperature of the charging bucket (11) is 180-190 ℃, the temperature of the valve control assembly (2) is 190-200 ℃, the temperature of the conveying pipeline (3) is 200-210 ℃, and the temperature of the injection pipe (4) is 350-400 ℃.
4. A mercury source furnace according to claim 3, characterized in that: the material tank (11) is provided with a material tank heater (12), the valve control assembly (2) is provided with a valve heater (23) or a heater shared by the valve control assembly and the material tank (11), and the injection pipe (4) is provided with an injection pipe heater (42).
5. The mercury source furnace of claim 1, wherein: and a liquid level sensor is also arranged on the charging bucket (11).
6. The mercury source furnace of any one of claims 1 to 5, wherein: the stop valve (21) is an all-metal angle valve.
7. The mercury source furnace of any one of claims 1 to 5, wherein: the metering valve (22) is a needle valve.
8. The mercury source furnace of any one of claims 1 to 5, wherein: one end of the conveying pipeline (3) close to the injection pipe (4) is a corrugated pipe and is provided with a corrugated pipe heating sleeve.
9. The mercury source furnace of any one of claims 1 to 5, wherein: the valve control assembly (2) is arranged at one end of the conveying pipeline (3) close to the charging bucket (11).
10. A method of replenishing mercury in a mercury source furnace as claimed in any one of claims 1 to 9, wherein: the method comprises the following steps:
s1, closing the stop valve (21) and the metering valve (22), and opening the vacuum valve (13) to be externally connected with a nitrogen pipeline for inflation operation;
s2, after the charging bucket (11) is restored to a normal pressure state, opening the liquid injection valve (14) to finish mercury liquid supplementing operation, and then closing the liquid injection valve (14);
s3, performing pre-vacuumizing operation through the external rough pump of the vacuum valve (13), closing the vacuum valve (13) after the charging bucket (11) reaches the designed vacuum degree, opening the stop valve (21), pumping the charging bucket (11) to a high vacuum state through the pump group in the vacuum chamber (5), and closing the stop valve (21).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211137323.6A CN115386960B (en) | 2022-09-19 | 2022-09-19 | Mercury source furnace and method for supplementing mercury liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211137323.6A CN115386960B (en) | 2022-09-19 | 2022-09-19 | Mercury source furnace and method for supplementing mercury liquid |
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| CN115386960A CN115386960A (en) | 2022-11-25 |
| CN115386960B true CN115386960B (en) | 2023-09-05 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4901670A (en) * | 1988-08-22 | 1990-02-20 | Santa Barbara Research Center | Elemental mercury source for metal-organic chemical vapor deposition |
| CN106525554A (en) * | 2016-12-16 | 2017-03-22 | 上海华川环保科技有限公司 | High-concentration gaseous mercury generator |
| CN206281702U (en) * | 2016-12-16 | 2017-06-27 | 上海华川环保科技有限公司 | A kind of high concentration gaseous mercury generator |
| CN111735916A (en) * | 2020-07-21 | 2020-10-02 | 华能国际电力股份有限公司 | Elemental mercury and bivalent mercury standard gas generation system and working method thereof |
| CN215953514U (en) * | 2021-03-09 | 2022-03-04 | 上海华川环保科技有限公司 | Mercury permeation source releasing device, mercury analysis equipment and equipment |
-
2022
- 2022-09-19 CN CN202211137323.6A patent/CN115386960B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4901670A (en) * | 1988-08-22 | 1990-02-20 | Santa Barbara Research Center | Elemental mercury source for metal-organic chemical vapor deposition |
| CN106525554A (en) * | 2016-12-16 | 2017-03-22 | 上海华川环保科技有限公司 | High-concentration gaseous mercury generator |
| CN206281702U (en) * | 2016-12-16 | 2017-06-27 | 上海华川环保科技有限公司 | A kind of high concentration gaseous mercury generator |
| CN111735916A (en) * | 2020-07-21 | 2020-10-02 | 华能国际电力股份有限公司 | Elemental mercury and bivalent mercury standard gas generation system and working method thereof |
| CN215953514U (en) * | 2021-03-09 | 2022-03-04 | 上海华川环保科技有限公司 | Mercury permeation source releasing device, mercury analysis equipment and equipment |
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| CN115386960A (en) | 2022-11-25 |
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