CN111690833A - High-temperature efficient alloy reaction purification furnace and alloy reaction process - Google Patents
High-temperature efficient alloy reaction purification furnace and alloy reaction process Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 75
- 239000000956 alloy Substances 0.000 title claims abstract description 75
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 71
- 238000000746 purification Methods 0.000 title claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 58
- 238000001816 cooling Methods 0.000 claims abstract description 55
- 230000005540 biological transmission Effects 0.000 claims abstract description 48
- 229910052751 metal Inorganic materials 0.000 claims abstract description 33
- 239000002184 metal Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000007789 gas Substances 0.000 claims description 51
- 238000003756 stirring Methods 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 24
- 238000007599 discharging Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000155 melt Substances 0.000 claims description 14
- 239000011261 inert gas Substances 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 238000006073 displacement reaction Methods 0.000 claims 1
- 239000004065 semiconductor Substances 0.000 abstract description 11
- 230000015572 biosynthetic process Effects 0.000 abstract description 8
- 238000003786 synthesis reaction Methods 0.000 abstract description 8
- 150000002739 metals Chemical class 0.000 abstract description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 4
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000011777 magnesium Substances 0.000 abstract description 4
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 abstract description 4
- 229910000925 Cd alloy Inorganic materials 0.000 abstract description 3
- 229910000807 Ga alloy Inorganic materials 0.000 abstract description 3
- 229910000861 Mg alloy Inorganic materials 0.000 abstract description 3
- 229910001215 Te alloy Inorganic materials 0.000 abstract description 3
- 229910002065 alloy metal Inorganic materials 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
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- 229910002601 GaN Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910001092 metal group alloy Inorganic materials 0.000 description 2
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- 229910000980 Aluminium gallium arsenide Inorganic materials 0.000 description 1
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- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- MDPILPRLPQYEEN-UHFFFAOYSA-N aluminium arsenide Chemical compound [As]#[Al] MDPILPRLPQYEEN-UHFFFAOYSA-N 0.000 description 1
- RNQKDQAVIXDKAG-UHFFFAOYSA-N aluminum gallium Chemical compound [Al].[Ga] RNQKDQAVIXDKAG-UHFFFAOYSA-N 0.000 description 1
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- 238000011031 large-scale manufacturing process Methods 0.000 description 1
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- 230000015654 memory Effects 0.000 description 1
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- 229910052714 tellurium Inorganic materials 0.000 description 1
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- 239000002699 waste material Substances 0.000 description 1
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/006—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with use of an inert protective material including the use of an inert gas
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
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Abstract
The invention discloses a high-temperature high-efficiency alloy reaction purification furnace, which comprises a furnace body, wherein the interior of the furnace body is hollow and is provided with a reaction cavity, a crucible is arranged in the reaction cavity, the crucible is connected with a transmission system, the transmission system comprises a lifting device which can stretch into the crucible and a transmission device which is connected outside the crucible, the reaction cavity is connected with a vacuum system, so that a heating system is arranged in the reaction cavity, the furnace body is connected with a cooling system, the high-temperature high-efficiency alloy reaction purification furnace also comprises a control cabinet and a power supply system, and the transmission system, the heating system, the cooling system and the vacuum system are respectively connected with the; also discloses an alloy reaction process; the device can replace a small test metal synthesis device and can be produced in a large scale; the method has strong universality, adopts combination of a plurality of functional systems, and is suitable for various semiconductor alloy metals, not limited to alloys of gallium, magnesium, cadmium, tellurium and other metals.
Description
Technical Field
The invention relates to the field of high-temperature heating furnaces and new materials, in particular to a high-temperature efficient alloy reaction purification furnace and an alloy reaction process.
Background
With the rise of new LED materials, new generation solar cells (including gallium arsenide solar cells and amorphous silicon thin film solar cells), phase change memories, semiconductor lasers, radio frequency integrated circuit chips and other fields, the industrial development demand is urgent due to the excellent characteristics of high electron mobility, large forbidden band width, good photoelectric characteristics and the like of compounds (such as gallium nitride GaN, aluminum gallium indium phosphide InGaAlP, gallium aluminum arsenide AlGaAs and the like) generated by elements in groups iii-v and ii-vi in the periodic table of elements.
As a high-purity metal organic source (MO) and a high-purity synthetic metal for preparing a compound semiconductor material, are key supporting raw materials of the compound semiconductor material.
The metal alloy has a series of excellent performances of high hardness, wear resistance, strength, toughness, heat resistance, corrosion resistance and the like, particularly high hardness and wear resistance, and basically keeps unchanged even at the temperature of 500 ℃. Therefore, the preparation of high purity alloy generally carries out the synthesis of simple substances in high temperature vacuum, and simultaneously needs heating, smelting, solid solution, heat preservation and purification to form a metal alloy ingot with processing characteristics.
At present, the production process for preparing high-purity alloy generally adopts an experimental device, and mainly adopts the steps of mixing two kinds of high-purity metal powder, placing the mixture into a graphite or quartz boat, placing the graphite or quartz boat into a quartz tube of a synthesis furnace, exhausting air, and heating for synthesis. The small-scale preparation process is influenced by graphite and quartz tube devices and cannot be used for large-scale continuous production. Particularly, because tellurium, magnesium, gallium, cadmium and the like used for semiconductors are relatively active metals, the reaction is violent, even splashing can be caused, waste is caused, and the product yield is low. Meanwhile, active metals are easily oxidized at high temperature, and the traditional vacuum synthesis method is easily oxidized and easily volatilized due to the limitation of vacuum degree, so that the proportion of various metal components in an alloy product is changed, and the yield of the product is low.
Disclosure of Invention
In order to solve the problems of large-scale production, product yield and product yield of the traditional alloy synthesis reactor and synthesis process, the invention provides a high-temperature high-efficiency alloy reaction purification furnace.
In order to achieve the above purpose, the embodiment of the invention adopts the following technical scheme:
the utility model provides a high-temperature high-efficient alloy reaction purification stove, high-temperature high-efficient alloy reaction purification stove includes that inside cavity is established to the furnace body of reaction cavity, be equipped with the crucible in the reaction cavity, the crucible is connected with transmission system, transmission system is including the device of pulling up in can stretching into the crucible and the transmission of connection outside the crucible, reaction cavity is connected with vacuum system, so be equipped with heating system in the reaction cavity, furnace body connection has cooling system, still includes switch board and electrical power generating system, transmission system, heating system, cooling system and vacuum system link to each other with switch board and electrical power generating system respectively.
According to one aspect of the invention, the upper end and/or the lower end of the furnace body is provided with an openable and closable detachable furnace cover, the upper furnace cover of the crucible is opened to carry out charging or discharging from the upper end, or the crucible is separated from the furnace body from the lower end through a transmission device to carry out charging or discharging when the lower furnace cover is opened.
According to one aspect of the invention, the furnace body wall is provided with an openable and closable furnace door, and the crucible leaves the furnace body from the furnace door opening through a transmission device for charging or discharging when the furnace door is opened.
According to one aspect of the invention, the lifting device comprises a lifting shaft and a stirring device, wherein the stirring device is driven by the lifting shaft to sink into the crucible to rotate and stir or driven by the lifting shaft to lift away from the crucible.
According to one aspect of the invention, the stirring device and the lifting shaft are provided with material metal cooling seed crystals.
According to one aspect of the invention, the furnace body is arranged on a furnace frame.
According to one aspect of the invention, the cooling system comprises furnace jacket water cooling, furnace chassis water cooling and heating electrode water cooling.
According to one aspect of the invention, the vacuum system comprises a vacuum pump, a filter and a specific gas inlet device, the vacuum pump is connected with the furnace body through a pipeline after passing through the filter through the pipeline, and the specific gas inlet device is connected to a connecting pipeline of the filter and the furnace body.
According to one aspect of the invention, the control cabinet controls the heating temperature of the furnace body, the vacuum degree of the furnace chamber, the rotating speed of the material, the pulling speed and the vacuum degree and performs air inlet control of specific gas through PLC control software.
According to one aspect of the invention, the specific gas is a reducing gas.
An alloy reaction process, comprising the steps of:
feeding: adding a certain proportion of crushed high-purity alloy powder into a crucible in a furnace body;
pressure maintaining replacement: the vacuum pump vacuumizes the furnace body through a gas filter, then inert gas is filled into the furnace for replacement protection, pressure maintaining replacement is carried out for 3 times, then a specific reduction body is introduced from a specific gas inlet device for replacement, and the final pressure is determined;
heating and melting: setting the heating temperature and the heating time according to the process requirements until the solid is completely molten and no steam exists;
rotating and stirring: after the metal is molten, descending the lifting shaft to drive the rotating device to be immersed into the melt, rotating at a certain speed, stopping rotating after the process required time is reached, lifting the lifting shaft to enable the rotating device to be separated from the melt, and stopping heating;
cooling, demoulding and discharging, and taking out the alloy.
According to one aspect of the invention, in the pressure maintaining and replacing step, the vacuum pump vacuumizes the furnace body through the gas filter, the inflation pressure is less than 0.1MPa, and the pressure surface is unchanged within 10 minutes when the ultimate vacuum degree of the cooling furnace is less than or equal to 3P.
The implementation of the invention has the advantages that: the high-temperature high-efficiency alloy reaction purification furnace comprises a furnace body, wherein the interior of the furnace body is hollow and is provided with a reaction cavity, a crucible is arranged in the reaction cavity, the crucible is connected with a transmission system, the transmission system comprises a lifting device capable of stretching into the crucible and a transmission device connected outside the crucible, and the reaction cavity is connected with a vacuum system, so that a heating system is arranged in the reaction cavity, the furnace body is connected with a cooling system, the high-temperature high-efficiency alloy reaction purification furnace also comprises a control cabinet and a power supply system, and the transmission system, the heating system, the cooling system and the vacuum system are respectively connected with the control cabinet and the; the device can replace a small test metal synthesis device and can be produced in a large scale; the universality is strong, several functional systems are combined, and the method is suitable for various semiconductor alloy metals, and is not limited to alloys of gallium, magnesium, cadmium, tellurium and other metals; the controllable heating system is arranged, the material is placed in the closed crucible, and the crucible can be lifted up and down and rotated by the crucible through the transmission system, so that the material is heated uniformly; the vacuum system is arranged, so that inert gas is filled into the cavity of the furnace body under the effective control of the gas inlet instrument valve in a vacuum environment, and the vacuum system is matched for multiple times of alternate operation, so that impurity gas is fully replaced, and the purity of the internal environment of the system is ensured; before production, introducing inert gas or other specific reducing gas into the system to keep the interior of the system in a positive pressure inert atmosphere in the production process; furthermore, the specific gas is generally reducing gas, so that the metal can not volatilize even at high temperature in the reducing gas environment, the oxidation phenomenon is avoided, the obtained product alloy components meet the process requirements, and the product yield is greatly improved.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a high-temperature high-efficiency alloy reaction purification furnace according to a first embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a high-temperature high-efficiency alloy reaction purification furnace according to a second embodiment of the present invention;
fig. 3 is a schematic structural diagram of a high-temperature high-efficiency alloy reaction purification furnace according to a third embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
As shown in fig. 1, the high-temperature high-efficiency alloy reaction purification furnace comprises a furnace body 1 with a hollow interior as a reaction cavity, a crucible 2 is arranged in the reaction cavity, the crucible is connected with a transmission system 3, the transmission system comprises a lifting device 31 capable of extending into the crucible and a transmission device 32 connected outside the crucible, the reaction cavity is connected with a vacuum system 4, so that a heating system is arranged in the reaction cavity, the furnace body is connected with a cooling system 5, the high-temperature high-efficiency alloy reaction purification furnace also comprises a control cabinet 6 and a power supply system 7, and the transmission system, the heating system, the cooling system and the vacuum system are respectively connected with the control cabinet and the power supply system; the upper end of the furnace body is provided with an upper furnace cover 11 which can be opened, closed and disassembled, and when the upper furnace cover is opened, feeding or discharging is carried out from the upper end.
In practical application, the lifting device comprises a lifting shaft 33 and a stirring device 34, and the stirring device is driven by the lifting shaft to sink into the crucible to rotate and stir or driven by the lifting shaft to rise and leave the crucible.
In practical application, the stirring device and the lifting shaft are provided with material metal cooling seed crystals, and the self metal cooling seed crystals are adopted for the rotary stirring of the alloy, so that the quality is ensured.
In practical application, the furnace body sets up on furnace frame 8, and the operation platform of steel construction is used for fixed furnace body, provides physics for each part and supports to for operating personnel provides operation platform.
In practical application, the cooling system comprises furnace body jacket water cooling, furnace body chassis water cooling and heating electrode water cooling.
In practical application, the vacuum system comprises a vacuum pump 41, a filter 42 and a specific gas inlet device 43, the vacuum pump is connected with the furnace body through a pipeline after passing through the filter through the pipeline, and the specific gas inlet device is connected on the connecting pipeline of the filter and the furnace body.
In practical application, the control cabinet controls the heating temperature of the furnace body, the vacuum degree of the furnace chamber, the rotating speed of materials, the pulling speed and the vacuum degree through PLC control software and performs air inlet control of specific gas.
In practical applications, the specific gas is a reducing gas.
The workflow of this embodiment includes:
1. top feeding: the upper furnace cover is opened, the crucible is lifted, and the raw materials are put into the crucible in proportion, so that the crucible is suitable for the working condition with light material quantity;
2. raw materials: generally, because the melting point of metal used for semiconductor alloy raw materials is lower, when the alloy is melted, firstly, high-purity alloy powder which is crushed in a certain proportion is added into a crucible in a furnace body;
3. pressure maintaining replacement: the alloy preparation is carried out under vacuum, the vacuum pump vacuumizes the furnace body through a gas filter, the general inflation pressure is less than 0.1MPa, the pressure surface is unchanged within 10 minutes under the condition of low vacuum (the ultimate vacuum degree of a cold furnace) being less than or equal to 3P, then inert gas is filled into the furnace for replacement protection, pressure maintaining replacement is carried out for 3 times, then a specific reduction body is introduced from a specific gas inlet device for replacement, and the final pressure is determined;
4. heating and melting: setting heating temperature and heating time according to process requirements, and rotating and stirring until the solid is completely molten and no steam exists;
5. rotating and stirring: after the metal is molten, descending the lifting shaft to drive the rotating device to be immersed into the melt, rotating at a certain speed, stopping rotating after the process required time is reached, lifting the lifting shaft to enable the rotating device to be separated from the melt, and stopping heating;
6. cooling, demolding and discharging, and discharging from the top: and opening the upper furnace cover and taking out the alloy.
Example two
As shown in fig. 2, the high-temperature high-efficiency alloy reaction purification furnace comprises a furnace body 1 with a hollow interior as a reaction cavity, a crucible 2 is arranged in the reaction cavity, the crucible is connected with a transmission system 3, the transmission system comprises a lifting device 31 capable of extending into the crucible and a transmission device 32 connected outside the crucible, the reaction cavity is connected with a vacuum system 4, so that a heating system is arranged in the reaction cavity, the furnace body is connected with a cooling system 5, the high-temperature high-efficiency alloy reaction purification furnace also comprises a control cabinet 6 and a power supply system 7, and the transmission system, the heating system, the cooling system and the vacuum system are respectively connected with the control cabinet and the power supply system; the lower end of the furnace body is provided with a lower furnace cover 12 which can be opened, closed and disassembled, and the crucible leaves the furnace body from the lower end through a transmission device when the lower furnace cover is opened so as to carry out charging or discharging.
In practical application, the lifting device comprises a lifting shaft 33 and a stirring device 34, and the stirring device is driven by the lifting shaft to sink into the crucible to rotate and stir or driven by the lifting shaft to rise and leave the crucible.
In practical application, the stirring device and the lifting shaft are provided with material metal cooling seed crystals, and the self metal cooling seed crystals are adopted for the rotary stirring of the alloy, so that the quality is ensured.
In practical application, the furnace body sets up on furnace frame 8, and the operation platform of steel construction is used for fixed furnace body, provides physics for each part and supports to for operating personnel provides operation platform.
In practical application, the cooling system comprises furnace body jacket water cooling, furnace body chassis water cooling and heating electrode water cooling.
In practical application, the vacuum system comprises a vacuum pump 41, a filter 42 and a specific gas inlet device 43, the vacuum pump is connected with the furnace body through a pipeline after passing through the filter through the pipeline, and the specific gas inlet device is connected on the connecting pipeline of the filter and the furnace body.
In practical application, the control cabinet controls the heating temperature of the furnace body, the vacuum degree of the furnace chamber, the rotating speed of materials, the pulling speed and the vacuum degree through PLC control software and performs air inlet control of specific gas.
In practical applications, the specific gas is a reducing gas.
The workflow of this embodiment includes:
1. bottom feeding: lowering the furnace cover, taking out the crucible through a transmission device, adding materials into the crucible in proportion, raising the crucible, and closing the lower furnace cover;
2. raw materials: generally, because the melting point of metal used for semiconductor alloy raw materials is lower, when the alloy is melted, firstly, high-purity alloy powder which is crushed in a certain proportion is added into a crucible in a furnace body;
3. pressure maintaining replacement: the alloy preparation is carried out under vacuum, the vacuum pump vacuumizes the furnace body through a gas filter, the general inflation pressure is less than 0.1MPa, the pressure surface is unchanged within 10 minutes under the condition of low vacuum (the ultimate vacuum degree of a cold furnace) being less than or equal to 3P, then inert gas is filled into the furnace for replacement protection, pressure maintaining replacement is carried out for 3 times, then a specific reduction body is introduced from a specific gas inlet device for replacement, and the final pressure is determined;
4. heating and melting: setting heating temperature and heating time according to process requirements, and rotating and stirring until the solid is completely molten and no steam exists;
5. rotating and stirring: after the metal is molten, descending the lifting shaft to drive the rotating device to be immersed into the melt, rotating at a certain speed, stopping rotating after the process required time is reached, lifting the lifting shaft to enable the rotating device to be separated from the melt, and stopping heating;
6. cooling, demolding and discharging, and discharging from the bottom: and opening the lower furnace cover, descending the crucible through a transmission device, and taking out the alloy.
EXAMPLE III
As shown in fig. 3, the high-temperature high-efficiency alloy reaction purification furnace comprises a furnace body 1 with a hollow interior as a reaction cavity, a crucible 2 is arranged in the reaction cavity, the crucible is connected with a transmission system 3, the transmission system comprises a lifting device 31 capable of extending into the crucible and a transmission device 32 connected outside the crucible, the reaction cavity is connected with a vacuum system 4, so that a heating system is arranged in the reaction cavity, the furnace body is connected with a cooling system 5, the high-temperature high-efficiency alloy reaction purification furnace also comprises a control cabinet 6 and a power supply system 7, and the transmission system, the heating system, the cooling system and the vacuum system are respectively connected with the control cabinet and the power supply system; the wall of the furnace body is provided with a furnace door 13 which can be opened and closed and disassembled, and the crucible leaves the furnace body from a furnace door opening through a transmission device when the furnace door is opened so as to carry out charging or discharging.
In practical application, the lifting device comprises a lifting shaft 33 and a stirring device 34, and the stirring device is driven by the lifting shaft to sink into the crucible to rotate and stir or driven by the lifting shaft to rise and leave the crucible.
In practical application, the stirring device and the lifting shaft are provided with material metal cooling seed crystals, and the self metal cooling seed crystals are adopted for the rotary stirring of the alloy, so that the quality is ensured.
In practical application, the furnace body sets up on furnace frame 8, and the operation platform of steel construction is used for fixed furnace body, provides physics for each part and supports to for operating personnel provides operation platform.
In practical application, the cooling system comprises furnace body jacket water cooling, furnace body chassis water cooling and heating electrode water cooling.
In practical application, the vacuum system comprises a vacuum pump 41, a filter 42 and a specific gas inlet device 43, the vacuum pump is connected with the furnace body through a pipeline after passing through the filter through the pipeline, and the specific gas inlet device is connected on the connecting pipeline of the filter and the furnace body.
In practical application, the control cabinet controls the heating temperature of the furnace body, the vacuum degree of the furnace chamber, the rotating speed of materials, the pulling speed and the vacuum degree through PLC control software and performs air inlet control of specific gas.
In practical applications, the specific gas is a reducing gas.
The workflow of this embodiment includes:
1. feeding: opening a furnace door, taking out the crucible through a transmission device, adding materials into the crucible in proportion, withdrawing the crucible, and closing the furnace door;
2. raw materials: generally, because the melting point of metal used for semiconductor alloy raw materials is lower, when the alloy is melted, firstly, high-purity alloy powder which is crushed in a certain proportion is added into a crucible in a furnace body;
3. pressure maintaining replacement: the alloy preparation is carried out under vacuum, the vacuum pump vacuumizes the furnace body through a gas filter, the general inflation pressure is less than 0.1MPa, the pressure surface is unchanged within 10 minutes under the condition of low vacuum (the ultimate vacuum degree of a cold furnace) being less than or equal to 3P, then inert gas is filled into the furnace for replacement protection, pressure maintaining replacement is carried out for 3 times, then a specific reduction body is introduced from a specific gas inlet device for replacement, and the final pressure is determined;
4. heating and melting: setting heating temperature and heating time according to process requirements, and rotating and stirring until the solid is completely molten and no steam exists;
5. rotating and stirring: after the metal is molten, descending the lifting shaft to drive the rotating device to be immersed into the melt, rotating at a certain speed, stopping rotating after the process required time is reached, lifting the lifting shaft to enable the rotating device to be separated from the melt, and stopping heating;
6. cooling, demolding and discharging: and opening the furnace door, moving out the crucible through a transmission device, and taking out the alloy.
Example four
An alloy reaction process, comprising the steps of:
feeding: adding a certain proportion of crushed high-purity alloy powder into a crucible in a furnace body;
raw materials: generally, because the melting point of metal used for semiconductor alloy raw materials is low, high-purity alloy powder which is crushed in a certain proportion is firstly added into a crucible in a furnace body when the alloy is melted.
In practical application, the feeding process comprises the following steps:
top feeding: the upper furnace cover is opened, the crucible is lifted, and the raw materials are put into the crucible in proportion, so that the crucible is suitable for the working condition with light material quantity;
bottom feeding: lowering the furnace cover, taking out the crucible through a transmission device, adding materials into the crucible in proportion, raising the crucible, and closing the lower furnace cover;
side feeding: opening the furnace door, taking out the crucible through the transmission device, adding the materials into the crucible in proportion, withdrawing the crucible, and closing the furnace door.
And (II) pressure maintaining replacement: the vacuum pump vacuumizes the furnace body through a gas filter, then inert gas is filled into the furnace for replacement protection, pressure maintaining replacement is carried out for 3 times, then a specific reduction body is introduced from a specific gas inlet device for replacement, and the final pressure is determined;
the alloy preparation is carried out under vacuum, the vacuum pump vacuumizes the furnace body through a gas filter, the general inflation pressure is less than 0.1MPa, the pressure surface is unchanged within 10 minutes under the condition of low vacuum (the ultimate vacuum degree of a cooling furnace) being less than or equal to 3P, then inert gas is filled into the furnace for replacement protection, pressure maintaining replacement is carried out for 3 times, then a specific reduction body is introduced from a specific gas inlet device for replacement, and the final pressure is determined.
(III) heating and melting: setting the heating temperature and the heating time according to the process requirements until the solid is completely molten and no steam exists;
and setting the heating temperature and the heating time according to the process requirements, and rotating and stirring until the solid is completely molten and no steam exists.
(IV) rotating and stirring: after the metal is molten, descending the lifting shaft to drive the rotating device to be immersed into the melt, rotating at a certain speed, stopping rotating after the process required time is reached, lifting the lifting shaft to enable the rotating device to be separated from the melt, and stopping heating;
and after the metal is molten, descending the lifting shaft to drive the rotating device to be immersed into the melt, rotating at a certain speed, stopping rotating after the process required time is reached, lifting the lifting shaft to enable the rotating device to be separated from the melt, and stopping heating.
And (V) cooling, demoulding and discharging, and taking out the alloy.
In practical application, the discharging comprises the following steps:
cooling, demolding and discharging, and discharging from the top: and opening the upper furnace cover and taking out the alloy.
Cooling, demolding and discharging, and discharging from the bottom: and opening the lower furnace cover, descending the crucible through a transmission device, and taking out the alloy.
Cooling, demolding and discharging: and opening the furnace door, moving out the crucible through a transmission device, and taking out the alloy.
The implementation of the invention has the advantages that: the high-temperature high-efficiency alloy reaction purification furnace comprises a furnace body, wherein the interior of the furnace body is hollow and is provided with a reaction cavity, a crucible is arranged in the reaction cavity, the crucible is connected with a transmission system, the transmission system comprises a lifting device capable of stretching into the crucible and a transmission device connected outside the crucible, and the reaction cavity is connected with a vacuum system, so that a heating system is arranged in the reaction cavity, the furnace body is connected with a cooling system, the high-temperature high-efficiency alloy reaction purification furnace also comprises a control cabinet and a power supply system, and the transmission system, the heating system, the cooling system and the vacuum system are respectively connected with the control cabinet and the; the device can replace a small test metal synthesis device and can be produced in a large scale; the universality is strong, several functional systems are combined, and the method is suitable for various semiconductor alloy metals, and is not limited to alloys of gallium, magnesium, cadmium, tellurium and other metals; the controllable heating system is arranged, the material is placed in the closed crucible, and the crucible can be lifted up and down and rotated by the crucible through the transmission system, so that the material is heated uniformly; the vacuum system is arranged, so that inert gas is filled into the cavity of the furnace body under the effective control of the gas inlet instrument valve in a vacuum environment, and the vacuum system is matched for multiple times of alternate operation, so that impurity gas is fully replaced, and the purity of the internal environment of the system is ensured; before production, introducing inert gas or other specific reducing gas into the system to keep the interior of the system in a positive pressure inert atmosphere in the production process; furthermore, the specific gas is generally reducing gas, so that the metal can not volatilize even at high temperature in the reducing gas environment, the oxidation phenomenon is avoided, the obtained product alloy components meet the process requirements, and the product yield is greatly improved.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention disclosed herein are intended to be covered by the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. The utility model provides a high temperature high efficiency alloy reaction purification stove, its characterized in that, high temperature high efficiency alloy reaction purification stove includes that inside cavity is established to the furnace body of reaction cavity, be equipped with the crucible in the reaction cavity, the crucible is connected with transmission system, transmission system includes the device of carrying in the protractile crucible and connects the transmission outside the crucible, reaction cavity is connected with vacuum system, so be equipped with heating system in the reaction cavity, the furnace body is connected with cooling system, still includes switch board and electrical power generating system, transmission system, heating system, cooling system and vacuum system link to each other with switch board and electrical power generating system respectively.
2. The high-temperature high-efficiency alloy reaction and purification furnace as claimed in claim 1, wherein the upper end and/or the lower end of the furnace body is provided with a detachable furnace cover, the upper furnace cover of the crucible is opened to feed or discharge from the upper end, or the crucible is separated from the furnace body from the lower end through a transmission device to feed or discharge when the lower furnace cover is opened.
3. The high-temperature high-efficiency alloy reaction and purification furnace as claimed in claim 1, wherein the furnace body wall is provided with a furnace door which can be opened and closed and disassembled, and the crucible is separated from the furnace body from the furnace door opening through a transmission device for charging or discharging when the furnace door is opened.
4. The high-temperature high-efficiency alloy reaction and purification furnace as claimed in claim 1, wherein the lifting device comprises a lifting shaft and a stirring device, the stirring device is driven by the lifting shaft to sink into the crucible for rotating and stirring or driven by the lifting shaft to rise out of the crucible.
5. The high-temperature high-efficiency alloy reaction and purification furnace as claimed in claim 4, wherein the stirring device and the lifting shaft are provided with material metal cooling seed crystals, and the furnace body is arranged on the furnace frame.
6. The high-temperature high-efficiency alloy reaction and purification furnace as claimed in claim 1, wherein the cooling system comprises furnace body jacket water cooling, furnace body chassis water cooling and heating electrode water cooling.
7. The high-temperature high-efficiency alloy reaction and purification furnace as claimed in one of claims 1 to 6, wherein the vacuum system comprises a vacuum pump, a filter and a specific gas inlet device, the vacuum pump is connected with the furnace body through a pipeline after passing through the filter, and the specific gas inlet device is connected to a connecting pipeline of the filter and the furnace body.
8. The high-temperature high-efficiency alloy reaction and purification furnace as claimed in claim 7, wherein the control cabinet controls the heating temperature of the furnace body, the vacuum degree of the furnace chamber, the rotation speed of the material, the pulling speed, the vacuum degree and the air intake control of specific gas through PLC control software.
9. An alloy reaction process, characterized in that it comprises the following steps:
feeding: adding a certain proportion of crushed high-purity alloy powder into a crucible in a furnace body;
pressure maintaining replacement: the vacuum pump vacuumizes the furnace body through a gas filter, then inert gas is filled into the furnace for replacement protection, pressure maintaining replacement is carried out for 3 times, then a specific reduction body is introduced from a specific gas inlet device for replacement, and the final pressure is determined;
heating and melting: setting the heating temperature and the heating time according to the process requirements until the solid is completely molten and no steam exists;
rotating and stirring: after the metal is molten, descending the lifting shaft to drive the rotating device to be immersed into the melt, rotating at a certain speed, stopping rotating after the process required time is reached, lifting the lifting shaft to enable the rotating device to be separated from the melt, and stopping heating;
cooling, demoulding and discharging, and taking out the alloy.
10. The alloy reaction process according to claim 9, wherein in the pressure maintaining displacement step, the vacuum pump vacuumizes the furnace body through a gas filter, the inflation pressure is less than 0.1MPa, and the pressure surface is unchanged within 10 minutes when the cold furnace ultimate vacuum degree is less than or equal to 3P.
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