CN113493904B - High-temperature high-vacuum annealing furnace - Google Patents
High-temperature high-vacuum annealing furnace Download PDFInfo
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- CN113493904B CN113493904B CN202010194318.3A CN202010194318A CN113493904B CN 113493904 B CN113493904 B CN 113493904B CN 202010194318 A CN202010194318 A CN 202010194318A CN 113493904 B CN113493904 B CN 113493904B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
- C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/54—Apparatus specially adapted for continuous coating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
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- 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 relates to vacuum coating experimental equipment, in particular to a high-temperature high-vacuum annealing furnace, which comprises an ion pump, an annealing chamber cavity, a sample feeding chamber cavity and a molecular pump which are sequentially connected, wherein the molecular pump is connected with a mechanical pump through a pipeline; the annealing chamber cavity is internally provided with a fixed upper heater and a lower heater capable of ascending and descending, the sampling chamber cavity is internally provided with a multi-layer sample library capable of ascending and descending, and one side of the sampling chamber cavity is provided with a manual transmission rod manipulator. The invention can rapidly complete sample exchange with the annealing chamber under the vacuum condition, and ensure that the annealing chamber is always in a high vacuum state. The high-temperature high-vacuum annealing furnace has an annealing chamber with a cold state ultimate vacuum degree of 10‑8Pa ultrahigh vacuum, and the thermal state vacuum degree can reach 10 when the vacuum is heated to 1600 DEG C‑ 6Pa, and can realize long-time heat preservation annealing of the sample at the temperature of not higher than 1600 ℃.
Description
Technical Field
The invention relates to vacuum coating experimental equipment, in particular to a high-temperature high-vacuum annealing furnace.
Background
Annealing is a common process for heat treatment of vacuum coating experimental equipment. The technical problems of the current vacuum annealing furnace are as follows:
1. the vacuum degree of the existing vacuum annealing furnace is low, and a very clean process environment cannot be provided.
2. The temperature of the existing vacuum annealing furnace is not high, so that the high-temperature and long-time heat preservation is difficult to realize.
3. The temperature uniformity of annealing of the sample was not good.
Disclosure of Invention
In view of the above problems of the conventional vacuum annealing furnace, the present invention aims to provide a high temperature high vacuum annealing furnace. The annealing chamber cold state electrode of the high-temperature high-vacuum annealing furnaceThe vacuum limiting degree can reach 10-8Pa ultrahigh vacuum, and the thermal state vacuum degree can reach 10 when the vacuum is heated to 1600 DEG C-6Pa, and can realize long-time heat preservation annealing of the sample at the temperature of not higher than 1600 ℃.
The purpose of the invention is realized by the following technical scheme:
the device comprises a sampling chamber assembly, an annealing chamber assembly and a vacuumizing assembly, wherein the vacuumizing assembly comprises an ion pump, a molecular pump and a mechanical pump, the sampling chamber assembly comprises a sampling chamber cavity, a sample library and a manual transmission rod manipulator, the annealing chamber assembly comprises an annealing chamber cavity, an upper heater and a lower heater, the ion pump, the annealing chamber cavity, the sampling chamber cavity and the molecular pump are sequentially connected, the molecular pump is connected with the mechanical pump through a pipeline, and gate valves are arranged between the ion pump and the annealing chamber cavity, between the annealing chamber cavity and the sampling chamber cavity and between the sampling chamber cavity and the molecular pump; the annealing chamber is characterized in that a fixed upper heater and a lower heater capable of ascending and descending are arranged in the annealing chamber cavity, a multi-layer sample library capable of ascending and descending is arranged in the sample introduction chamber cavity, and a manual transmission rod manipulator used for moving an annealing sample between the sample introduction chamber cavity and the annealing chamber cavity is arranged on one side of the sample introduction chamber cavity.
Wherein: the upper heater comprises an upper shell, a heat shielding layer and a graphite heating sheet, the upper shell is connected to an upper flange of the annealing chamber arranged at the top of the cavity of the annealing chamber, the heat shielding layer is arranged in the upper shell, and the graphite heating sheet is arranged in the heat shielding layer; the upper shell outside the heat shielding layer is divided into a heat preservation shell layer and a water cooling shell layer which are mutually independent from inside to outside, the heat preservation shell layer is communicated with an air discharging pipe, and the water cooling shell layer is respectively communicated with a water inlet pipe and a water outlet pipe.
The lower heater is driven to lift up and down by a first welding corrugated pipe lifting mechanism and comprises a lower shell, a heat shielding layer and graphite heating sheets, the lower shell is connected with the first welding corrugated pipe lifting mechanism, the heat shielding layer is arranged in the lower shell, and the graphite heating sheets are arranged inside the heat shielding layer; the external lower shell of heat shield is divided into mutually independent heat preservation shell and water-cooling shell from inside to outside, and this heat preservation shell intercommunication has the gas release pipe, the water-cooling shell communicates respectively has inlet tube and outlet pipe.
The lower heater also comprises an all-metal vent angle valve, the all-metal vent angle valve is arranged on a lower flange of the annealing chamber connected with the bottom of the cavity of the annealing chamber, one end of the all-metal vent angle valve is communicated with the inside of the cavity of the annealing chamber, the other end of the all-metal vent angle valve is communicated with an external gas cylinder or a gas source, and process gas or cooling gas is introduced into the cavity of the annealing chamber.
The heat shield layer is made of tantalum sheets, the heat preservation shell layer is formed by welding stainless steel, the heat preservation graphite felt is filled in the heat preservation shell layer, the water cooling shell layer is formed by welding the stainless steel, and the water cooling shell layer is internally filled with circulating cooling water through a water inlet pipe and a water outlet pipe.
The annealing chamber cavity is provided with a baffle observation window and a vacuum gauge for measuring vacuum degree, and the sample injection chamber cavity is provided with a vacuum gauge for measuring vacuum degree.
The lower heater is driven to lift up and down by a first welding corrugated pipe lifting mechanism, the first welding corrugated pipe lifting mechanism comprises a lifting motor, a support, a lead screw, a nut, a corrugated pipe and a connecting pipe, a knife edge flange at the lower end of the corrugated pipe is fixed on a foundation, the lifting motor is installed on the knife edge flange at the lower end of the corrugated pipe through the support, the output end of the lifting motor is connected with the lead screw, the nut is in threaded connection with the lead screw, and the nut is connected with the knife edge flange at the upper end of the corrugated pipe; one end of the connecting pipe is connected with a knife edge flange at the upper end of the corrugated pipe, and the other end of the connecting pipe penetrates into the cavity of the annealing chamber and is connected with the lower heater.
The sample library is driven to ascend and descend up and down by a second welding corrugated pipe lifting mechanism, the second welding corrugated pipe lifting mechanism comprises a lifting motor, a support, a screw rod, a nut, a corrugated pipe and a connecting pipe, a knife edge flange at the upper end of the corrugated pipe is fixed on a foundation, the lifting motor is installed on the knife edge flange at the upper end of the corrugated pipe through the support, the output end of the lifting motor is connected with the screw rod, the nut is in threaded connection with the screw rod, and the nut is connected with the knife edge flange at the lower end of the corrugated pipe; one end of the connecting pipe is connected with a knife edge flange at the lower end of the corrugated pipe, and the other end of the connecting pipe penetrates into the cavity of the sample chamber and is connected with the sample warehouse.
The vacuumizing assembly also comprises an angle valve and an electromagnetic isolating valve, and the angle valve is arranged on the cavity of the sample injection chamber and is connected with the mechanical pump through a pipeline; one end of the electromagnetic isolating valve is installed on the molecular pump, and the other end of the electromagnetic isolating valve is connected with the mechanical pump through a pipeline.
And a molybdenum sample support is arranged on each layer of the sample library.
The invention has the advantages and positive effects that:
1. the cold state ultimate vacuum degree of the annealing chamber component can reach 10-8Pa ultrahigh vacuum, and the thermal state ultimate vacuum degree can reach 10 when the vacuum is heated to 1600 DEG C-6Pa; the ultimate vacuum degree of the sample introduction chamber assembly can reach 10-6Pa, the sample transfer with the annealing chamber can be realized under the high vacuum condition, and the annealing chamber is further ensured to be always in an ultrahigh vacuum state.
2. The heating temperature of the annealing chamber is 1600 ℃, and the annealing chamber can be kept warm for a long time at high temperature; the heat-insulating shell of the annealing chamber can well prevent heat loss, improve the heat utilization rate and reduce energy consumption; the water-cooling shell of the annealing chamber can quickly take away useless heat loss, and peripheral parts of the heater are not affected by heat.
3. The annealing chamber has good sample heating uniformity, and the deviation between the center temperature and the edge temperature of a 4-inch round sample is less than 2%.
4. The upper heater and the lower heater of the annealing chamber component can be rapidly cooled when being opened, and the inside of the heater is provided with the vent pipeline, so that on one hand, process gas can be introduced during annealing to enable a sample to be in the process gas atmosphere; on the other hand, cooling gas can be introduced during cooling, so that the sample is cooled rapidly.
Drawings
FIG. 1 is a front view of the structure of the present invention;
FIG. 2 is a top view of the structure of the present invention;
FIG. 3 is a cross-sectional view of the construction of an annealing chamber assembly according to the invention;
FIG. 4 is a sectional view of a sample introduction chamber assembly according to the present invention;
wherein: 1 is a sample feeding chamber component, 2 is an annealing chamber component, 3 is an ion pump, 4 is a first gate valve, 5 is a second gate valve, 6 is a third gate valve, 7 is a molecular pump, 8 is a mechanical pump, 9 is a first high vacuum ionization gauge, 10 is a first low vacuum resistance gauge, 11 is an angle valve, 12 is a second high vacuum ionization gauge, 13 is an electromagnetic isolating valve, 14 is a second low vacuum resistance gauge, 15 is an annealing chamber cavity, 16 is an upper heater, 17 is a water-cooling shell, 18 is a heat-insulating shell, 19 is a heat-shielding layer, 20 is a graphite heating plate, 21 is a lower heater, 22 is an all-metal vent angle valve, 23 is a first welding bellows elevating mechanism, 24 is a baffle observation window, 25 is a sample feeding chamber cavity, 26 is a second welding bellows elevating mechanism, 27 is a sample holder, 28 is a molybdenum sample holder, 29 is a manual transfer lever manipulator, 30 is an upper flange of the annealing chamber, and 31 is a lower flange of the annealing chamber, 32 is a gas release pipe, 33 is a water inlet pipe, and 34 is a water outlet pipe.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
As shown in fig. 1 to 4, the invention comprises a sample introduction chamber assembly 1, an annealing chamber assembly 2 and a vacuum pumping assembly, wherein the vacuum pumping assembly comprises an ion pump 3, a molecular pump 7 and a mechanical pump 8, the sample introduction chamber assembly 1 comprises a sample introduction chamber cavity 25, a sample library 27 and a manual transmission rod manipulator 29, the annealing chamber assembly 2 comprises an annealing chamber cavity 15, an upper heater 16 and a lower heater 21, the ion pump 3, the annealing chamber cavity 15, the sample introduction chamber cavity 25 and the molecular pump 7 are sequentially connected, the molecular pump 7 is connected with the mechanical pump 8 through a pipeline, and gate valves are respectively arranged between the ion pump 3 and the annealing chamber cavity 15, between the annealing chamber cavity 15 and the sample introduction chamber cavity 25 and between the sample introduction chamber cavity 25 and the molecular pump 7; namely, a first gate valve 4 is arranged between the annealing chamber cavity 15 and the ion pump 3, a second gate valve 5 is arranged between the annealing chamber cavity 15 and the sample injection chamber cavity 25, and a third gate valve 6 is arranged between the sample injection chamber cavity 25 and the molecular pump 7. A fixed upper heater 16 and a lower heater 21 capable of ascending and descending are arranged in the annealing chamber cavity 15, a multi-layer sample warehouse 27 capable of ascending and descending is arranged in the sample inlet chamber cavity 25, and a manual transmission rod manipulator 29 for moving an annealing sample between the sample inlet chamber cavity 25 and the annealing chamber cavity 15 is arranged on one side of the sample inlet chamber cavity 25.
The top and the bottom of the cavity 15 of the annealing chamber of this embodiment are respectively and fixedly connected with an upper flange 30 and a lower flange 31 of the annealing chamber, the upper heater 16 and the lower heater 21 are both located in the cavity 15 of the annealing chamber, and the upper heater 16 is fixedly installed right above the lower heater 21. The upper heater 16 of the present embodiment comprises an upper shell, a heat shield layer 19 and a graphite heating plate 20, wherein the upper shell is connected to an upper flange 30 of the annealing chamber, the heat shield layer 19 is arranged in the upper shell, and the graphite heating plate 20 is installed in the heat shield layer 19. The upper shell outside the heat shield layer 19 is divided into a heat-insulating shell layer 18 and a water-cooling shell layer 17 which are mutually independent from inside to outside, the heat-insulating shell layer 18 is communicated with an air discharge pipe 32, and the water-cooling shell layer 17 is respectively communicated with an inlet pipe 33 and an outlet pipe 34.
The lower heater 21 of the present embodiment includes a lower housing, a heat shield layer 19, and a graphite heating plate 20, the lower housing is connected to the first welding bellows lifting mechanism 23, the heat shield layer 19 is provided in the lower housing, and the graphite heating plate 20 is installed inside the heat shield layer 19. The lower shell outside the heat shield layer 19 is divided into a heat-insulating shell layer 18 and a water-cooling shell layer 17 which are mutually independent from inside to outside, the heat-insulating shell layer 18 is communicated with an air discharge pipe 32, and the water-cooling shell layer 17 is respectively communicated with an inlet pipe 33 and an outlet pipe 34. The lower heater 21 of the embodiment further comprises an all-metal vent angle valve 22, the all-metal vent angle valve 22 is mounted on the lower flange 31 of the annealing chamber, one end of the all-metal vent angle valve is communicated with the inside of the cavity 15 of the annealing chamber, the other end of the all-metal vent angle valve is communicated with an external gas cylinder or a gas source, and process gas or cooling gas is introduced into the cavity 15 of the annealing chamber; the process gas or cooling gas of this embodiment may be argon in an inert gas.
The heat shield layer 19 in the upper heater 16 and the lower heater 21 in the present embodiment is made of tantalum sheet; the heat preservation shell layer 18 is formed by welding stainless steel, and heat preservation graphite felt is filled in the heat preservation shell layer 18; the water-cooling shell layer 17 is formed by welding stainless steel, circulating cooling water is introduced into the water-cooling shell layer 17 through the water inlet pipe 33 and the water outlet pipe 34, useless dissipated heat can be taken away in time by the water-cooling shell layer 17, and peripheral parts of the upper heater 16 and the lower heater 21 are guaranteed not to be affected by heat.
The cavity 15 of the annealing chamber in this embodiment is respectively provided with a baffle observation window 24, and a first ionization high vacuum gauge 9 and a first resistance low vacuum gauge 10 for measuring the vacuum degree. The sample chamber cavity 25 of this embodiment is mounted with a second ionization high vacuum gauge 12 and a second resistance low vacuum gauge 14 for measuring vacuum degree. The ionization high vacuum gauge and the resistance low vacuum gauge of this embodiment are both commercially available products, and are purchased from Chengdui Rui Bao electronic technology Co., Ltd, and the model of the ionization high vacuum gauge is ZJ-12 ionization vacuum gauge, and the model of the resistance low vacuum gauge is ZJ-52T resistance vacuum gauge.
The lower heater 21 of the present embodiment is driven to move up and down by the first welding bellows elevating mechanism 23, and thus the engagement and opening of the upper heater 16 and the lower heater 21 can be realized. The first welding bellows lifting mechanism 23 includes a lifting motor, a bracket, a lead screw, a nut, a bellows and a connecting pipe, wherein a knife edge flange at the lower end of the bellows is fixed on a foundation (such as a workbench), the lifting motor is fixedly mounted on the knife edge flange at the lower end of the bellows through the bracket, the output end of the lifting motor is connected with the lead screw, the nut is in threaded connection with the lead screw, and the nut is connected with the knife edge flange at the upper end of the bellows. One end of the connecting pipe is connected with the knife edge flange at the upper end of the corrugated pipe, and the other end of the connecting pipe penetrates into the cavity 15 of the annealing chamber through the lower flange 31 of the annealing chamber and is connected with the lower shell of the lower heater 21. The lifting motor works, the knife edge flange at the upper end of the corrugated pipe is lifted through a screw pair formed by the lead screw and the nut, and then the whole lower heater 21 is driven by the connecting pipe to lift in the cavity 15 of the annealing chamber. The corrugated pipe has the function of dynamic sealing, can realize movement lifting, can seal vacuum and is airtight. Therefore, the design of the bellows can realize the ultrahigh vacuum dynamic seal that the whole lower heater 21 ascends and descends in the annealing chamber cavity 15.
The sample library 27 of the embodiment is four layers, and each layer of the sample library 27 is provided with a molybdenum sample holder 28; the molybdenum sample holder 28 of this embodiment can hold a 4 inch round sample at the maximum. The sample storage 27 is driven to move up and down by a second welding bellows lifting mechanism 26, and the second welding bellows lifting mechanism 26 and a manual transmission rod manipulator 29 cooperate to realize the taking and the transmission of the molybdenum sample support 28 on the sample storage 27. The lifting mechanism 26 for the two-welding corrugated pipe in this embodiment includes a lifting motor, a bracket, a lead screw, a nut, a corrugated pipe and a connecting pipe, wherein a knife edge flange at the upper end of the corrugated pipe is fixed on a foundation (such as a workbench), the lifting motor is installed on the knife edge flange at the upper end of the corrugated pipe through the bracket, the output end of the lifting motor is connected with the lead screw, the nut is in threaded connection with the lead screw, and the nut is connected with the knife edge flange at the lower end of the corrugated pipe. One end of the connecting pipe is connected with a knife edge flange at the lower end of the corrugated pipe, and the other end of the connecting pipe penetrates into the sample chamber cavity 25 and is connected with the sample storage 27. The lifting motor works, the knife edge flange at the lower end of the corrugated pipe is lifted through a screw pair formed by the lead screw and the nut, and then the sample storage 27 is driven by the connecting pipe to lift in the sample chamber cavity 25. The manual transfer bar robot 29 of the present embodiment is a commercially available product, available from Kurt J. Lesker Company, USA, and is model number EPP 35-609-H.
The vacuum pumping assembly of the embodiment further comprises an angle valve 11 and an electromagnetic isolating valve 13, wherein the angle valve 11 is mounted on the sampling chamber cavity 25 and is connected with the mechanical pump 8 through a pipeline; one end of the electromagnetic isolating valve 13 is arranged on the molecular pump 7, and the other end is connected with the mechanical pump 8 through a pipeline.
The piping mentioned in this embodiment may be a suction hydraulic bellows as in the prior art.
In this embodiment, the first and second welding bellows lifting mechanisms 23 and 26 are driven by lifting motors, and other driving methods can also achieve this function. Further, the four-layer sample storage 27 may be formed in more layers.
In this embodiment, the upper and lower heaters 16 and 21 preferably use graphite heating plates as heating media, and other heating media such as tantalum plates, tantalum wires, molybdenum plates, tungsten plates, etc. may also be used.
In this embodiment, the heat-insulating shell 18 of the upper and lower heaters 16 and 21 is made of a heat-insulating soft graphite felt as an internal filling heat-insulating medium, and other soft high-temperature-resistant materials can be used without limitation.
In this embodiment, the annealing chamber assembly 2 is configured to achieve high-temperature heating and heat preservation by using a combination of the upper and lower heaters 16 and 21, and other structural forms such as front and rear, left and right or a combination of a plurality of blocks are replaced within the protection scope of the present invention.
The working principle of the invention is as follows:
in this embodiment, the annealed sample is a 4-inch round sample, and various shaped samples having a size of less than 4 inches may be placed on the molybdenum sample holder 28 without limitation.
1. The annealed sample is placed on the molybdenum sample holder 28 of the sample reservoir 27 in the sample introduction chamber cavity 25, then the movable door on the sample introduction chamber cavity 25 is closed, and the vacuum pumping system is started.
2. The annealing chamber cavity 15 is pumped by the ion pump 3 and kept at 10-8Pa ultrahigh vacuum state, the vacuum degree in the cavity 25 of the sample chamber reaches 10-5And when Pa is needed, the second gate valve 5 between the annealing chamber cavity 15 and the sample feeding chamber cavity 25 is opened, and the annealing sample is taken and placed into the annealing chamber cavity 15 through the manual transfer rod manipulator 29. After the sample to be annealed is placed in the lower heater 21 in the annealing chamber cavity 15, the manual transfer bar robot 29 is retracted. The second gate valve 5 between the annealing chamber cavity 15 and the sample introduction chamber cavity 25 is closed.
3. The first welding bellows lifting mechanism 23 drives the lower heater 21 to ascend, after the upper heater 16 and the lower heater 21 in the cavity 15 of the annealing chamber are buckled, the cavity 15 of the annealing chamber starts to heat, and the heat preservation shell 18 can well prevent heat loss.
4. After the sample is annealed, the upper heater 16 and the lower heater 21 in the cavity 15 of the annealing chamber can be in an open state, so that the sample can be rapidly cooled.
5. After the sample is annealed and cooled, the second gate valve 5 between the sample feeding chamber cavity 25 and the annealing chamber cavity 15 is opened, and the sample is taken back into the sample feeding chamber cavity 25 through the manual transfer rod manipulator 29. The next sample is then fed into the annealing chamber cavity 15 to begin annealing.
6. And so on until the annealing of all samples on the four-layer sample library 27 in the sample chamber cavity 25 is completed.
Claims (8)
1. A high-temperature high-vacuum annealing furnace is characterized in that: comprises a sample introduction chamber component (1), an annealing chamber component (2) and a vacuum pumping component, wherein the vacuum pumping component comprises an ion pump (3), a molecular pump (7) and a mechanical pump (8), the sample introduction chamber component (1) comprises a sample introduction chamber cavity (25), a sample library (27) and a manual transfer rod manipulator (29), the annealing chamber component (2) comprises an annealing chamber cavity (15), an upper heater (16) and a lower heater (21), the ion pump (3), the annealing chamber cavity (15), the sample injection chamber cavity (25) and the molecular pump (7) are connected in sequence, the molecular pump (7) is connected with the mechanical pump (8) through a pipeline, and gate valves are arranged between the ion pump (3) and the annealing chamber cavity (15), between the annealing chamber cavity (15) and the sample injection chamber cavity (25) and between the sample injection chamber cavity (25) and the molecular pump (7); a fixed upper heater (16) and a lower heater (21) capable of ascending and descending are arranged in the annealing chamber cavity (15), a multi-layer sample library (27) capable of ascending and descending is arranged in the sampling chamber cavity (25), and a manual transmission rod manipulator (29) for moving an annealed sample between the sampling chamber cavity (25) and the annealing chamber cavity (15) is arranged on one side of the sampling chamber cavity (25);
the upper heater (16) comprises an upper shell, a heat shielding layer (19) and a graphite heating sheet (20), the upper shell is connected to an upper flange (30) of the annealing chamber arranged at the top of the annealing chamber cavity (15), the heat shielding layer (19) is arranged in the upper shell, and the graphite heating sheet (20) is arranged in the heat shielding layer (19); the upper shell outside the heat shield layer (19) is divided into a heat-insulating shell layer (18) and a water-cooling shell layer (17) which are mutually independent from inside to outside, the heat-insulating shell layer (18) is communicated with an air discharge pipe (32), and the water-cooling shell layer (17) is respectively communicated with a water inlet pipe (33) and a water outlet pipe (34);
the lower heater (21) is driven to lift up and down through a first welding corrugated pipe lifting mechanism (23), the lower heater (21) comprises a lower shell, a heat shielding layer (19) and graphite heating sheets (20), the lower shell is connected with the first welding corrugated pipe lifting mechanism (23), the heat shielding layer (19) is arranged in the lower shell, and the graphite heating sheets (20) are installed in the heat shielding layer (19); the external lower shell of heat shield (19) is divided into mutually independent heat preservation shell (18) and water-cooling shell (17) from inside to outside, and this heat preservation shell (18) intercommunication has gas release pipe (32), water-cooling shell (17) communicate respectively has inlet tube (33) and outlet pipe (34).
2. The high-temperature high-vacuum annealing furnace according to claim 1, characterized in that: the lower heater (21) further comprises an all-metal vent angle valve (22), the all-metal vent angle valve (22) is mounted on a lower annealing chamber flange (31) connected with the bottom of the annealing chamber cavity (15), one end of the all-metal vent angle valve is communicated with the inside of the annealing chamber cavity (15), the other end of the all-metal vent angle valve is communicated with an external gas cylinder or a gas source, and process gas or cooling gas is introduced into the annealing chamber cavity (15).
3. The high-temperature high-vacuum annealing furnace according to claim 1, characterized in that: the heat shield (19) adopts the tantalum piece to make, heat preservation shell (18) adopt the stainless steel welding to form, and this heat preservation shell (18) inside packing has the heat preservation graphite felt, water-cooling shell (17) adopt the stainless steel welding to form, and this water-cooling shell (17) is inside through inlet tube (33) and outlet pipe (34) through going into recirculated cooling water.
4. The high temperature high vacuum annealing furnace according to claim 1, wherein: the annealing chamber cavity (15) is provided with a baffle plate observation window (24) and a vacuum gauge for measuring vacuum degree, and the sampling chamber cavity (25) is provided with the vacuum gauge for measuring vacuum degree.
5. The high-temperature high-vacuum annealing furnace according to claim 1, characterized in that: the lower heater (21) is driven to lift up and down through a first welding corrugated pipe lifting mechanism (23), the first welding corrugated pipe lifting mechanism (23) comprises a lifting motor, a support, a screw rod, a nut, a corrugated pipe and a connecting pipe, a knife edge flange at the lower end of the corrugated pipe is fixed on a foundation, the lifting motor is installed on the knife edge flange at the lower end of the corrugated pipe through the support, the output end of the lifting motor is connected with the screw rod, the nut is in threaded connection with the screw rod, and the nut is connected with the knife edge flange at the upper end of the corrugated pipe; one end of the connecting pipe is connected with a knife edge flange at the upper end of the corrugated pipe, and the other end of the connecting pipe penetrates into the annealing chamber cavity (15) and is connected with the lower heater (21).
6. The high-temperature high-vacuum annealing furnace according to claim 1, characterized in that: the sample library (27) is driven to lift up and down through a second welding corrugated pipe lifting mechanism (26), the second welding corrugated pipe lifting mechanism (26) comprises a lifting motor, a support, a screw rod, a nut, a corrugated pipe and a connecting pipe, a knife edge flange at the upper end of the corrugated pipe is fixed on a base, the lifting motor is installed on the knife edge flange at the upper end of the corrugated pipe through the support, the output end of the lifting motor is connected with the screw rod, the nut is in threaded connection with the screw rod, and the nut is connected with the knife edge flange at the lower end of the corrugated pipe; one end of the connecting pipe is connected with a knife edge flange at the lower end of the corrugated pipe, and the other end of the connecting pipe penetrates into the sample introduction chamber cavity (25) and is connected with the sample library (27).
7. The high-temperature high-vacuum annealing furnace according to claim 1, characterized in that: the vacuumizing assembly further comprises an angle valve (11) and an electromagnetic isolating valve (13), wherein the angle valve (11) is installed on the sampling chamber cavity (25) and is connected with the mechanical pump (8) through a pipeline; one end of the electromagnetic isolating valve (13) is installed on the molecular pump (7), and the other end of the electromagnetic isolating valve is connected with the mechanical pump (8) through a pipeline.
8. The high-temperature high-vacuum annealing furnace according to claim 1, characterized in that: and a molybdenum sample support (28) is arranged on each layer of the sample library (27).
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| CN202010194318.3A CN113493904B (en) | 2020-03-19 | 2020-03-19 | High-temperature high-vacuum annealing furnace |
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| CN113493904B true CN113493904B (en) | 2022-06-07 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4308756A (en) * | 1979-10-04 | 1982-01-05 | Ultra High Vacuum Instruments Ltd. | Vacuum sample introduction unit |
| JPS5893230A (en) * | 1981-11-30 | 1983-06-02 | Toshiba Corp | Ultra high vacuum processing apparatus |
| JPS6088433A (en) * | 1983-10-21 | 1985-05-18 | Seiko Epson Corp | Semiconductor manufacturing device |
| JPS627124A (en) * | 1985-07-02 | 1987-01-14 | Sharp Corp | Annealing device for semiconductor substrate |
| JPS6247116A (en) * | 1985-08-26 | 1987-02-28 | Semiconductor Energy Lab Co Ltd | Semiconductor device manufacturing equipment |
| US4721836A (en) * | 1986-05-14 | 1988-01-26 | The United States Of America As Represented By The Secretary Of The Navy | Apparatus for transient annealing of semiconductor samples in a controlled ambient |
| US6276072B1 (en) * | 1997-07-10 | 2001-08-21 | Applied Materials, Inc. | Method and apparatus for heating and cooling substrates |
| US7723649B2 (en) * | 2002-08-05 | 2010-05-25 | Steed Technology, Inc. | Vacuum thermal annealer |
| CN201212046Y (en) * | 2008-06-27 | 2009-03-25 | 中国科学院沈阳科学仪器研制中心有限公司 | Vacuum annealing furnace |
| US20140273533A1 (en) * | 2013-03-15 | 2014-09-18 | Taiwan Semiconductor Manufacturing Company, Ltd. | Semiconductor Annealing Method Utilizing a Vacuum Environment |
| CN106222753B (en) * | 2016-08-22 | 2018-07-06 | 中国科学技术大学 | A kind of miniature rapid temperature rise and drop annealing furnace |
| CN107099781A (en) * | 2017-04-20 | 2017-08-29 | 邵海平 | A kind of filming equipment and film plating process |
| CN208432627U (en) * | 2018-07-17 | 2019-01-25 | 苏州华杨赛斯真空设备有限公司 | Portable ultrahigh vacuum sample transfer device |
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