CN118166209A - A continuous UHV vertical floating zone melting metal purification system - Google Patents
A continuous UHV vertical floating zone melting metal purification system Download PDFInfo
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- CN118166209A CN118166209A CN202410174220.XA CN202410174220A CN118166209A CN 118166209 A CN118166209 A CN 118166209A CN 202410174220 A CN202410174220 A CN 202410174220A CN 118166209 A CN118166209 A CN 118166209A
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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
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
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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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- 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
- Y02P10/25—Process efficiency
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Abstract
A continuous UHV vertical floating zone molten metal purification system can realize continuous preparation of ultra-pure metal, can be applied to industrial production, and particularly can further remove impurities with higher saturated vapor pressure than a matrix by utilizing the saturated vapor pressure difference of the matrix and the impurities by providing an ultra-high vacuum environment for zone melting.
Description
Technical Field
The invention relates to the technical field of metal purification, in particular to a continuous UHV vertical floating zone-melting metal purification system.
Background
Zone melting is a method of preparing high purity materials, which was invented by John Desmond Bernal and further developed by William g.pfann in bell laboratories. Prior to zone melting, it is generally necessary to prepare the feedstock into a rod-like material of a certain size and vertically secure the feedstock rod within the furnace chamber using two chucks. The high-frequency coil is used for induction heating and melting of a part of the raw material rod, so that a melting zone slowly passes through the whole raw material rod from one end to the other end to finish purification. Throughout the zone melting process, the molten zone melts the impure solid at its leading edge, and the impurities are concentrated in the melt and moved to one end of the feed rod, causing the molten zone to solidify after passing through the feed rod, leaving a purer material. The melt zone is supported by surface tension and is therefore also commonly referred to as the "suspension zone melting process". The method does not need a crucible, avoids the contact between the raw material and the crucible, and the purity of the purified material is high. On the other hand, in the process of zone melting, the main chamber is pumped to an ultrahigh vacuum state or some gas atmosphere is introduced according to the properties of the purified material, so that the zone melting effect can be further improved. In recent years, with the development of technology, the requirements of some devices on the purity of metal materials are more and more severe, and especially in the field of semiconductor industry, the improvement of the purity of raw materials of metal materials often leads to an exponential improvement of the performance of devices. However, the existing zone melting apparatus has the following disadvantages: the lack of a high-precision real-time temperature feedback system can not monitor the temperature and the length of a melting zone of a purified metal sample in a main chamber in real time and dynamically adjust the heating power, which may cause unstable melting zone and affect the purification efficiency of the metal; the lack of an ultra-high vacuum system can not enable the air pressure in the main cavity to reach an ultra-high vacuum state, and impurities with higher saturated vapor pressure than the matrix can be further removed by utilizing the saturated vapor pressure difference of the matrix and the impurities; the lack of a residual gas analyzer can not accurately measure the gas components in the main chamber, and the inability to accurately control the smelting atmosphere during zone smelting and purification can lead to unsatisfactory purification effect. Therefore, the invention provides a continuous UHV vertical floating zone-melting metal purification system (UHV, ultra-high vacuum), realizes continuous preparation of ultra-pure metal, and can be applied to industrial production.
Disclosure of Invention
Aiming at the defects or shortcomings in the prior art, the invention provides a continuous UHV vertical floating zone melting metal purification system, which can realize continuous preparation of ultra-pure metal, can be applied to industrial production, and can further remove impurities with higher saturated vapor pressure than the matrix by utilizing the saturated vapor pressure difference of the matrix and the impurities by providing an ultra-high vacuum environment for zone melting.
The technical scheme of the invention is as follows:
the utility model provides a continuous UHV vertical float zone molten metal purification system, its characterized in that, including the main cavity room that is used for carrying out the ultrahigh vacuum zone melting technology, the top of main cavity room is provided with three-dimensional moving platform, the multiaxis platform adjustment seat of three-dimensional moving platform lower extreme connects zone molten metal rod upper end clamping assembly, zone molten metal rod upper end clamping assembly passes the main cavity lid and gets into in the main cavity room, the right flank of main cavity room passes through transmission port flange joint pretreatment chamber, the magnetic force sample feed pole is connected on the right side of pretreatment chamber, the district of magnetic force sample feed pole melts pretreatment metal rod jack catch and is located in the pretreatment chamber, the low temperature pump is connected through the push-pull valve to the left surface of main cavity room, induction heating system is connected to the trailing flank of main cavity room, induction heating system heats zone molten metal rod through the induction coil that is located the main cavity in the waist in order to form vertical float zone.
Control buttons and a control panel are arranged on the front side face of the induction heating system, and a cooling port is arranged on the top face of the induction heating system.
The low-temperature pump is provided with a low-temperature pump heating wire, and is connected with a low-temperature pump transformer.
The right side face of the main chamber is provided with a micro-leakage valve and a residual gas analyzer interface, and the residual gas analyzer interface is connected with a residual gas analyzer.
The main chamber and the pretreatment chamber are respectively connected with a vacuum system, the vacuum system comprises a combination of a mechanical pump and a molecular pump, the vacuum system provides vacuum of 9X 10 -5 Pa for the pretreatment chamber, the vacuum system provides vacuum of 9X 10 -8 Pa for the main chamber, the vacuum system comprises a vacuum pump control panel and a molecular pump control panel, the vacuum pump control panel and the molecular pump control panel are both positioned below a table top for bearing the pretreatment chamber, and a central controller is arranged on the table top.
And the side edge of the main cavity cover is connected with a main cavity cover lifting device.
An annular groove formed by supporting a spring piece is arranged between the upper and lower combined structures of the upper end clamping assembly of the zone melting sample piece, so that thermal expansion caused by the zone melting sample piece is released.
The clamping jaw structure of the clamping assembly at the upper end of the zone melting sample piece comprises a spring piece device so as to eliminate the stress acting on the zone melting sample piece in the process of clamping the zone melting sample piece up and down.
The multi-axis platform adjusting seat is respectively connected with an X-axis driving motor, a Z-axis driving motor, a Y-axis driving motor and a rotary driving motor.
The pretreatment chamber is internally provided with a high-voltage arc discharge device to carry out plasma cleaning on the surface of the metal bar to be vacuum zone-melted.
The invention has the following technical effects: the continuous UHV vertical floating zone molten metal purification system can realize continuous preparation of ultrapure metal through the combination of the ultrahigh vacuum main chamber, the high vacuum pretreatment chamber, the three-dimensional moving platform, the clamping component, the induction heating system and the low-temperature pump, can be applied to industrial production, and can further remove impurities with higher saturated vapor pressure than the matrix by utilizing the saturated vapor pressure difference of the matrix and the impurities by providing an ultrahigh vacuum environment for zone melting.
Drawings
FIG. 1 is a schematic diagram of a continuous UHV vertical float zone molten metal purification system embodying the present invention.
Fig. 2 is a schematic view of the three-dimensional moving platform in fig. 1.
FIG. 3 is a schematic view of the magnetic force sample feeding rod in FIG. 1.
Fig. 4 is a schematic view of the main chamber structure of fig. 1.
Fig. 5 is a schematic view of the upper end clamp assembly of the zone-melted metal bar of fig. 2.
FIG. 6 is a schematic view of the induction heating system of FIG. 1 in a vertical float zone condition formed by heating a zone melting bar with an induction coil positioned at the waist in the main chamber.
The reference numerals are explained as follows: 1-a central controller (display screen); 2-a magnetic sample feeding rod; 3-a table top; 4-baffle plates; 5-a first metal panel; 6-a vacuum pump control panel; 7-a second metal panel; 8-a third metal panel; 9-a film thickness control panel; 10-molecular pump control panel; 11-a fourth metal panel; 12-a fifth metal panel; 13-a sixth metal panel; 14-cover plate; 15-a cryopump transformer; 16-an induction heating system; 17-a first control button; 18-a second control button; 19-a third control button; 20-fourth control button; 21-a first control panel; 22-a second control panel; 23-a first cooling port; 24-a second cooling port; 25-cryopump; 26-a low-temperature pump heating wire; 27-gate valve; 28-a main cavity cover lifting device; 29-a support plate; 30-a three-dimensional mobile platform; 31-a main chamber (i.e., an ultra-high vacuum zone melting process chamber or a UHV zone melting process chamber, UHV, ultra-high vacuum); 32-reversing lever; 33-micro leakage valve; 34-a pretreatment chamber; 35-a rotary drive motor; 36-Z axis driving motor; a 37-X axis driving motor; 38-Y axis driving motor; 39-gearing; 40-clamping the upper end of the zone-melting metal bar; 41-zone-melting pretreatment of metal bar clamping jaws; 42-residual gas analyzer interface; 43-jaw structure; 44-an annular groove; 45-multiaxial platform adjustment seat.
Detailed Description
The present invention will be described below with reference to examples and drawings (fig. 1 to 6).
FIG. 1 is a schematic diagram of a continuous UHV vertical float zone molten metal purification system embodying the present invention. Fig. 2 is a schematic view of the three-dimensional moving platform in fig. 1. FIG. 3 is a schematic view of the magnetic force sample feeding rod in FIG. 1. Fig. 4 is a schematic view of the main chamber structure of fig. 1. Fig. 5 is a schematic view of the upper end clamp assembly of the zone-melted metal bar of fig. 2. FIG. 6 is a schematic view of the induction heating system of FIG. 1 in a vertical float zone condition formed by heating a zone melting bar with an induction coil positioned at the waist in the main chamber. Referring to fig. 1 to 6, a continuous UHV vertical float zone molten metal purifying system includes a main chamber 31 for performing an ultra-high vacuum float zone process, a three-dimensional moving platform 30 is disposed above the main chamber 31, a multi-axis platform adjusting seat 45 at the lower end of the three-dimensional moving platform 30 is connected with a clamp assembly 40 at the upper end of a float zone metal bar, the clamp assembly 40 at the upper end of the float zone metal bar penetrates through the main chamber cover to enter the main chamber 31, the right side surface of the main chamber 31 is connected with a pretreatment chamber 34 through a transmission port flange, the right side of the pretreatment chamber 34 is connected with a magnetic sample feeding rod 2, a float zone pre-treated metal bar claw 41 of the magnetic sample feeding rod 2 is disposed in the pretreatment chamber 34, the left side surface of the main chamber 31 is connected with a cryopump 25 through a gate valve 27, the rear side surface of the main chamber 31 is connected with an induction heating system 16, and the induction heating system 16 heats the float zone metal bar through an induction coil disposed at the middle waist in the main chamber 31 to form a vertical float zone.
The induction heating system 16 is provided with control buttons and control panels (including a first control button 17, a second control button 18, a third control button 19, a fourth control button 20, a first control panel 21, a second control panel 22, etc.) on the front side, and the induction heating system 16 is provided with cooling ports (including a first cooling port 23, a second cooling port 24, etc.) on the top surface. The cryopump 25 is provided with a cryopump heating wire 26, and the cryopump 25 is connected with the cryopump transformer 15. A micro-leak valve 33 and a residual gas analyzer interface 42 are provided on the right side of the main chamber 31, the residual gas analyzer interface 42 being connected to a residual gas analyzer.
The main chamber 31 and the pretreatment chamber 34 are respectively connected with a vacuum system, the vacuum system comprises a combination of a mechanical pump and a molecular pump, the vacuum system provides vacuum of up to 9×10 -5 Pa for the pretreatment chamber 34, the vacuum system provides vacuum of up to 9×10 -8 Pa for the main chamber 31, the vacuum system comprises a vacuum pump control panel 6 and a molecular pump control panel 10, the vacuum pump control panel 6 and the molecular pump control panel 10 are both positioned below a table top 3 for bearing the pretreatment chamber 34, and a central controller 1 is arranged on the table top. The side of the main cavity cover is connected with a main cavity cover lifting device 28. An annular groove 44 formed by supporting a spring piece is arranged between the upper and lower combined structures of the upper end clamping assembly 40 of the zone melting sample piece, so as to release the thermal expansion caused by the zone melting sample piece. The jaw structure of the upper clamping assembly 40 of the zone-melting sample piece comprises a spring piece device so as to eliminate the stress on the zone-melting sample piece in the process of clamping the zone-melting sample piece up and down. The multi-axis platform adjusting seat 45 is respectively connected with the X-axis driving motor 37, the Z-axis driving motor 36, the Y-axis driving motor 38 and the rotary driving motor 35. A high-voltage arc discharge device is arranged in the pretreatment chamber 34 to perform plasma cleaning on the surface of the metal bar to be vacuum zone-melted.
A continuous UHV vertical float zone molten metal purification system. The system comprises: the clamping assembly is used for clamping the raw material rod in the main cavity; a sample delivery assembly for delivering the rod-like material from the pre-evacuation high vacuum chamber to a designated location in the ultra-high vacuum process chamber; the induction heating system comprises an induction heating power supply and an induction heating coil, and circulating cooling water is communicated inside the induction heating coil; the ultrahigh vacuum system consists of a low-temperature pump, a molecular pump and a mechanical pump; the residual gas analyzer is arranged in the main cavity; and the central control system is electrically connected with the clamping assembly, the induction heating system, the ultrahigh vacuum system and the residual gas detector. The ultra-high purity metal prepared by the system has the characteristics of high purity, controllable process, simple steps and continuous work, and can be applied to industrial production.
The continuous UHV vertical floating zone-melting metal purification system comprises a chassis, wherein the chassis internally comprises a vacuum process chamber, a pre-vacuumizing chamber, a vacuum system, a three-dimensional motion platform, a fixed rod, a magnetic sample feeding rod, an induction heating system and a central controller, and the vacuum process chamber internally comprises a clamping assembly, a temperature detection system and a residual gas analyzer. The three-dimensional motion platform is used for lifting the fixing rod, and the clamping assembly is used for clamping the rod-shaped material.
The vacuum system is a combination of a mechanical pump and a low-temperature pump, and can enable the highest vacuum degree in the vacuum process chamber to reach 9 multiplied by 10 -8 Pa.
The vacuum system in the pre-vacuumizing chamber is a combination of a mechanical pump and a low-temperature pump, the highest vacuum degree of the vacuum system can reach 9X 10 -5 Pa, and the pre-vacuumizing chamber can perform plasma cleaning on rod-shaped materials.
The clamping assembly comprises spring plate means which relieve the stress of the upper and lower clamping means on the rod-shaped material during clamping of the rod-shaped material.
The fixing rod is positioned in the chassis, and two ends of the fixing rod are fixedly connected with the three-dimensional motion platform and the clamping assembly.
The magnetic sample conveying rod is respectively positioned in the pre-vacuumizing chamber and the vacuum process chamber, and the magnetic sample conveying rod in the pre-vacuumizing chamber can convey rod-shaped materials into the vacuum process chamber; the magnetic force sample feeding rod in the vacuum process chamber can adjust the rod-shaped material from a horizontal state to a vertical state so as to be clamped.
The temperature detection system mainly comprises a film thickness instrument, the crystal oscillator probe is connected with the film thickness instrument and is positioned in the vacuum process chamber, the deposition rate of the rod-shaped material during melting is measured by the crystal oscillator probe, and the purpose of detecting the temperature can be achieved after the deposition rate during melting is determined through multiple experiments.
The induction heating system comprises a water cooling circulation system, the water cooling circulation system is connected with the central controller, cooling water is circulated into the heating coil, the cooling water temperature is controlled and set by the central controller, and the stability of the output power of the induction heating coil is guaranteed.
The three-dimensional motion platform comprises a sliding block, a motor, a corrugated pipe and a bearing; the bellows is arranged in the chassis along the vertical direction, the motor is arranged in the chassis, and the bearing is fixed on the inner side wall of the vacuum process chamber; the motor is used for driving power to be connected with one end of a corrugated pipe through an output shaft, and the other end of the corrugated pipe is connected with a bearing; the corrugated pipe is sleeved with a nut, the nut is fixedly connected with a nut seat, the sliding block is fixedly connected with the nut seat, and the fixed rod is fixedly connected with the sliding block.
The outside of machine case still is provided with all kinds of gas pitchers, and the gas pitcher passes through the trachea with vacuum process room intercommunication can be through the nature of bar-shaped material can be through the different gases of well accuse ware input parameter selection lets in order to improve purification effect.
The mechanical pump and the low-temperature pump of the vacuum system are arranged outside the chassis and are communicated with the vacuum process chamber through the vacuumizing tube; and the inner wall of the vacuum process chamber is provided with a vent, and the vent is controlled to be opened and closed by a gate valve.
An observation window is arranged above the vacuum process chamber.
The induction heating system consists of an induction coil and an induction heating host power supply.
The induction coil extends into the vacuum process chamber for heating rod-shaped materials.
The induction heating host power supply is used for controlling induction heating current and power.
A residual gas analyzer, said residual gas analyzer means being capable of detecting a gas composition within said vacuum process chamber.
The central controller is arranged in the case and is electrically connected with the three-dimensional motion platform, the temperature detection system, the vacuum system, the clamping assembly, the induction heating system, the current detection system and the residual gas analyzer.
The residual gas analyzer is electrically connected with the computer.
And after the residual gas analyzer detects the gas components in the vacuum process chamber, feeding back data to a computer.
As a further improvement of the continuous UHV vertical floating zone molten metal purification system, the three-dimensional motion platform is divided into an upper part and a lower part, and can be respectively displaced in the three-dimensional direction so as to be rapidly positioned and accurately displaced.
Compared with the prior art, the system has the following beneficial effects:
(1) The film thickness gauge probe arranged in the main chamber of the vertical zone melting furnace can feed back the real-time deposition rate of the rod-shaped material, judge the temperature of the melting zone according to the rate, adjust the power of the induction coil, and provide conditions for realizing the stability of the melting zone in the zone melting process.
(2) The ultra-high vacuum system of the vertical zone melting furnace enables the air pressure in the main chamber to reach an ultra-high vacuum state (9 multiplied by 10 -8 Pa) in the zone melting heating process, and further removes impurities with higher saturated vapor pressure than the matrix by utilizing the saturated vapor pressure difference of the matrix and the impurities under the condition of extremely low loss of the substrate, thereby improving the purification effect.
(3) The residual gas analyzer of the vertical zone melting furnace can accurately measure the gas components in the main chamber, accurately control the atmosphere during metal rod purification through the fed-back data, achieve the purpose of removing specific impurities by utilizing the specific gas atmosphere, and further improve the purification effect.
(4) The various systems in the vertical zone melting furnace can adjust parameters to achieve the best purification effect and the highest purification efficiency, and the vertical zone melting furnace has the advantages of wide application range, strong flexibility, high working efficiency, simple method and easy industrialization.
(5) The purification device can realize vertical zone melting purification of refractory metal and greatly improve the purity of refractory metal samples.
As shown in fig. 1, a central controller 1 (display screen): the air valve, mechanical pump, vacuum pump can be controlled. Magnetic force sample feeding rod 2: for transporting the sample between the pretreatment chamber and the main chamber. Table top 3: a pretreatment chamber is placed. Baffle 4: decorative effect. The first metal panel 5: decorative effect. Vacuum pump control panel 6: parameters of the vacuum pump are controlled. Second metal panel 7: decorative effect. Third metal panel 8: decorative effect. Film thickness control panel 9: for controlling the film thickness monitoring. Molecular pump control panel 10: for controlling parameters of the molecular pump. Fourth metal panel 11: decorative effect. Fifth metal panel 12: decorative effect. Sixth metal panel 13: decorative effect. Cover plate 14: decorative effect. Cryopump transformer 15: and controlling the power supply of the cryopump. Induction heating system 16: for controlling the current and frequency of the coil. The first control button 17, the second control button 8, the third control button 19, the fourth control button 20, the first control panel 21 and the second control panel 22 are all used for control. The first cooling port 23 and the second cooling port 24 are each used for cooling the sample holder. Cryogenic pump 25: for drawing the main chamber gas. Cryopump heater wire 26: for restoring pump activity. Gate valve 27: and controlling the switching of the cryopump and the main chamber. Main cover lifting device 28: for controlling the lifting of the main cavity cover. The support plate 29: and a corrugated pipe is arranged in the inner part. Three-dimensional mobile platform 30: the movement of the sample in the main chamber is controlled. A main chamber 31 (i.e., an ultra-high vacuum zone melting process chamber or a UHV zone melting process chamber, UHV, ultra-high vacuum): the method is used for zone melting treatment of a sample melting machine. Reversing lever 32 (located on the front side of main chamber 31): for exchanging the molten sample with the sample rod in the pretreatment chamber. Micro-leakage valve 33: the gas may be controlled to enter the main chamber. 34-pretreatment chamber: the pretreatment method is used for pretreatment of the molten sample.
The invention relates to a continuous UHV vertical floating zone-melting metal purification system, which is applied to 4N-level iron rod purification, and comprises the steps of opening a pretreatment chamber 34 (i.e. a pre-vacuumizing chamber) and placing 4N-level iron rods into the pretreatment chamber 34. And (3) turning on a bias power supply, and cleaning the surface of the 4N-level iron rod through a high-voltage arc. The vacuum system is opened through the central controller 1, the gate valve 27 is opened, the vacuum degree of the pretreatment chamber 34 reaches 10 -5 Pa, the sample conveying component conveys the 4N-level iron rod to the appointed position of the main chamber 31, and the vacuum degree of the main chamber 31 is 10 -5 Pa. The sample feeding assembly in the main chamber 31 clamps the 4N-level iron rod to perform steering transposition. The 4N-level iron rod is fixed through the clamping assembly, the gate valve is closed, the vacuum system is opened, and the vacuum degree of the main chamber 31 is waited to reach 9X 10 -8 Pa. The induction heating system 16 is set to have a current range of 40-140A and a vertical movement speed of 0.1-200 mm/min and a rotation speed of 1-25r/min. The input parameters operate the three-dimensional motion platform 30 to move the 4N-level iron rod from the initial position to the set position, the process is repeated according to the set parameters, N-pass vertical zone melting purification is sequentially performed according to different process parameters, and N is a positive integer, for example, n=7. After the steps of n times are repeated, the induction heating system 30 is powered off, after the iron rod subjected to zone melting purification is cooled to room temperature, the iron rod is taken out to the pretreatment chamber 34 by utilizing the sample feeding component, a gate valve is closed, protective atmosphere is introduced, and after the internal pressure and the external pressure are consistent, the rod-shaped material is taken out, and a new rod-shaped material can be filled for continuous production. And cutting out preset parts (5% -15%) of the upper end and the lower end of the purified iron rod, wherein the middle rest part is the purified product, namely the 5N (the iron element content is 99.995-99.9994 wt%) or higher N iron rod.
What is not described in detail in this specification is prior art known to those skilled in the art. It is noted that the above description is helpful for a person skilled in the art to understand the present invention, but does not limit the scope of the present invention. Any and all such equivalent substitutions, modifications and/or deletions as may be made without departing from the spirit and scope of the invention.
Claims (10)
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|---|---|
| CN118166209B (en) | 2025-04-11 |
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Denomination of invention: A continuous UHV vertical floating zone metal purification system Granted publication date: 20250411 Pledgee: Wu'an Rural Credit Union Co.,Ltd. Pledgor: Hebei Longfengshan Chenxin New Materials Technology Co.,Ltd. Registration number: Y2025130000013 |
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