CN212404223U - Ultra-pure beryllium ultra-vacuum molecular distillation system - Google Patents
Ultra-pure beryllium ultra-vacuum molecular distillation system Download PDFInfo
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- CN212404223U CN212404223U CN202021829340.2U CN202021829340U CN212404223U CN 212404223 U CN212404223 U CN 212404223U CN 202021829340 U CN202021829340 U CN 202021829340U CN 212404223 U CN212404223 U CN 212404223U
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Abstract
The utility model relates to the technical field of a color metal ultra-vacuum melting device, in particular to an ultra-pure beryllium ultra-vacuum molecular distillation system, which comprises an ultra-vacuum air exhaust and vacuum control unit, a beryllium oxide ceramic crucible distillation unit, a heating device and a temperature control unit, wherein the beryllium oxide ceramic crucible distillation unit, the heating device and the temperature control unit are arranged at the bottom of the ultra-vacuum air exhaust and vacuum control unit; the ultra-vacuum pumping unit comprises a raw material storage tank, a vacuum feeding module, a finished product receiving module and a full-range composite vacuum gauge A1 for controlling vacuum; the beryllium oxide ceramic crucible distillation unit comprises a beryllium oxide crucible and a crucible supporting seat; the heating device and the temperature control unit comprise a low-temperature super-vacuum pump, light-phase vacuum pipelines and heavy-phase vacuum pipelines which are arranged on two sides of the low-temperature super-vacuum pump, and a full-range composite vacuum gauge A2 for controlling vacuum. The utility model discloses process flow is short, and production method is simple, and preparation cycle is short, and the beryllium metal purity of producing is high, ensures that the product of production reaches 5N purity.
Description
Technical Field
The utility model relates to a non ferrous metal ultra-vacuum melting equipment technical field, in particular to ultrapure beryllium ultra-vacuum molecular distillation system.
Background
Because of the characteristics of high melting point, small thermal expansion coefficient, good physical and chemical stability and the like of beryllium metal and beryllium oxide, the material is the most ideal material for aerospace, nuclear energy, war industry, chip packaging, infrared optics and the like. Beryllium metal is active in chemical property and is very easy to have replacement reaction with other ceramic containers and metal containers at high temperature in the smelting process. Thereby introducing harmful impurities such as metal, nonmetal, gas and the like, and reducing the purity of the metal beryllium ingot. At present, the domestic common production methods comprise an electric arc melting method, a zone melting method and an induction melting method. The disadvantages of the above method are: the process flow is long, the production method is complex, the production period is long, and the problems of safety and environmental protection are difficult to solve. The prepared metal beryllium has huge quality difference with foreign products.
SUMMERY OF THE UTILITY MODEL
Aiming at the defects in the prior art, the utility model provides an ultra-pure beryllium ultra-vacuum molecular distillation system, the production method is simple, the preparation period is short, and the purity of the produced beryllium metal is high.
An ultra-pure beryllium ultra-vacuum molecular distillation system comprises an ultra-vacuum air exhaust and vacuum control unit, a beryllium oxide ceramic crucible distillation unit, a heating device and a temperature control unit, wherein the beryllium oxide ceramic crucible distillation unit, the heating device and the temperature control unit are arranged at the bottom of the ultra-vacuum air exhaust and vacuum control unit;
the ultra-vacuum pumping unit comprises a raw material storage tank, a vacuum feeding module, a finished product receiving module and a full-range composite vacuum gauge A1 for controlling vacuum, wherein a feeding port is formed in the top of the raw material storage tank, a viewing mirror is arranged on the side surface of the raw material storage tank, the vacuum feeding module and the full-range composite vacuum gauge A1 are respectively arranged at the bottom of the raw material storage tank, a coarse bowl inlet is formed between the vacuum feeding module and the full-range composite vacuum gauge A1, a raw material quantitative push rod is arranged on the coarse bowl inlet, and the finished product receiving module comprises an oxidized ceramic crucible metal beryllium receiving vessel and a receiving module temperature transmitter;
the beryllium oxide ceramic crucible distillation unit comprises a beryllium oxide crucible and a crucible supporting seat, the top of the beryllium oxide crucible is connected with the inlet of the coarse pot, the two sides of the beryllium oxide crucible are respectively provided with a low-boiling point metal distillation outlet and a high-boiling point metal distillation outlet, a distillation cavity is arranged inside the beryllium oxide crucible, the outer wall of the distillation cavity is provided with a connected heating rod inserting opening and a heating temperature control element, the bottom of the beryllium oxide crucible is provided with a temperature transmitter, the bottom of the temperature transmitter is provided with a finished product outlet, the crucible supporting seat is arranged at the bottom of the beryllium oxide crucible, and an overhaul opening is arranged below the crucible supporting seat;
the heating device and the temperature control unit comprise a low-temperature super-vacuum pump, light-phase vacuum pipelines and heavy-phase vacuum pipelines which are arranged on two sides of the low-temperature super-vacuum pump, and a full-range composite vacuum gauge A2 for controlling vacuum, the low-temperature super-vacuum pump is arranged at the bottom of the finished product outlet, the light-phase vacuum pipelines are connected to the low-boiling-point metal distillation outlet through a light-phase receiver, and the heavy-phase vacuum pipelines are connected to the high-boiling-point metal distillation outlet through a heavy-phase receiver.
Preferably, the bottom of the vacuum feeding module is provided with a feeding module supporting device.
Preferably, the integrated heating rod insertion opening is provided with a nickel alloy heating rod, and the beryllium oxide crucible and the nickel alloy heating rod are formed at one time.
Preferably, the light phase receiver and the heavy phase receiver are both provided with receiver mirrors.
Preferably, the beryllium oxide crucible is prepared by high-temperature oxidation of high-purity metal beryllium.
The utility model has the advantages that:
1) the utility model discloses utilize general thick beryllium in market (the purity generally is: 99.5%) was subjected to ultra-vacuum molecular distillation to produce ultrapure beryllium. The working pressure of the ultra-vacuum pumping unit is high, and the operation is stable; the beryllium oxide crucible is resistant to high-temperature corrosion, soft melting does not occur when the crucible is used for smelting metal beryllium, the crucible material does not pollute the metal, the slag resistance is good, and the crucible is not corroded by slag. The thermal shock resistance stability is good; the crucible has good dimensional stability at high temperature and does not deform.
2) The utility model discloses process flow is short, and production method is simple, and preparation cycle is short, and the beryllium metal purity of producing is high, ensures that the product of production reaches 5N purity.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention, and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a schematic sectional structure of the present invention;
FIG. 2 is a top view of the structure of the present invention;
FIG. 3 is a schematic structural view of a beryllium oxide crucible;
1-feeding port, 2-raw material storage tank, 3-viewing mirror, 4-vacuum feeding module, 5-full range composite vacuum gauge A1, 6-coarse bowl inlet, 7-feeding module supporting device, 8-temperature transmitter, 9-crucible supporting seat, 10-beryllium oxide crucible, 11-integrated heating rod insertion port, 12-inspection port, 13-finished product outlet, 14-low-temperature ultra-vacuum pump, 15-finished product receiving system, 16-ceramic oxide crucible metal beryllium receiving vessel, 17-light phase vacuum pipeline, 18-light phase receiver, 19-receiver viewing mirror, 20-heavy phase receiver, 21-vacuum furnace shell, 22-heavy phase vacuum pipeline, 23-full range composite vacuum gauge A2, 24-receiving module temperature transmitter, 25-low boiling point metal distillation outlet, 26-high boiling point metal distillation outlet and 27-distillation cavity.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention easier to be clearly understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. The components of embodiments of the present invention, as generally described and illustrated in the figures herein, may be arranged and designed in a wide variety of different configurations.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only used for convenience of description and simplification of description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
As shown in the attached drawing, the ultra-pure beryllium ultra-vacuum molecular distillation system comprises an ultra-vacuum air pumping and vacuum control unit, a beryllium oxide ceramic crucible distillation unit, a heating device and a temperature control unit, wherein the beryllium oxide ceramic crucible distillation unit, the heating device and the temperature control unit are arranged at the bottom of the ultra-vacuum air pumping and vacuum control unit;
the ultra-vacuum pumping unit comprises a raw material storage tank 2, a vacuum feeding module 4, a finished product receiving module 15 and a full-range composite vacuum gauge A1 for controlling vacuum, wherein a feeding port 1 is formed in the top of the raw material storage tank 2, a viewing mirror 3 is arranged on the side face of the raw material storage tank 2, the vacuum feeding module 4 and the full-range composite vacuum gauge A1 are respectively arranged at the bottom of the raw material storage tank 2, a coarse bowl inlet 6 is formed between the vacuum feeding module 4 and the full-range composite vacuum gauge A1, a raw material quantitative push rod is arranged on the coarse bowl inlet 6, the finished product receiving module 15 comprises an oxidized ceramic crucible metal beryllium receiving vessel 16 and a receiving module temperature transmitter 24, and a feeding module supporting device 7 is arranged at the bottom of;
the beryllium oxide ceramic crucible distillation unit comprises a beryllium oxide crucible 10 and a crucible support seat 9, the top of the beryllium oxide crucible 10 is connected with a coarse pot inlet 6, two sides of the beryllium oxide crucible 10 are respectively provided with a low-boiling point metal distillation outlet 25 and a high-boiling point metal distillation outlet 26, a distillation cavity 27 is arranged in the beryllium oxide crucible 10, the outer wall of the distillation cavity 27 is provided with a connected heating rod insertion opening 11 and a heating temperature control element, a nickel alloy heating rod is arranged in the connected heating rod insertion opening 11, the beryllium oxide crucible 10 and the nickel alloy heating rod are formed in one step, the bottom of the beryllium oxide crucible 10 is provided with a temperature transmitter 8, the bottom of the temperature transmitter 8 is provided with a finished product outlet 13, the crucible support seat 9 is arranged at the bottom of the beryllium oxide crucible 10, an inspection opening 12 is arranged below the crucible support seat 9, and the outer part of;
the heating device and the temperature control unit comprise a low-temperature super-vacuum pump 14, light-phase vacuum pipelines 17, heavy-phase vacuum pipelines 22 and a full-range composite vacuum gauge A2 for controlling vacuum, the light-phase vacuum pipelines 17 and the heavy-phase vacuum pipeline 22 are arranged on two sides of the low-temperature super-vacuum pump 14, the low-temperature super-vacuum pump 14 is arranged at the bottom of a finished product outlet 13, the light-phase vacuum pipelines 17 are connected to a low-boiling-point metal distillation outlet 25 through a light-phase receiver 18, the heavy-phase vacuum pipelines 22 are connected to a high-boiling-point metal distillation outlet 26 through a heavy-phase receiver 20, and receiver sight.
In this embodiment, the beryllium oxide crucible 11 is prepared by high-temperature oxidation of high-purity beryllium (99.999%) (a ceramic crucible is prepared by high-temperature oxidation of self-produced ultrapure beryllium metal and high-purity beryllium oxide). The preparation method comprises the following steps: briquetting and sintering at 1300 ℃. The sintering material is crushed, screened and mixed, and then the inorganic binder and a proper amount of water are added in proportion. The mixture was placed in a mold and cold isostatic pressed at 50 Mpa. And taking out after maintaining the pressure for 10/min, removing the outer die, and putting into a high-temperature furnace for secondary sintering. The temperature rise speed is 10 ℃/min, the sintering temperature is 1550 ℃, the time is 3h, and the temperature is kept for 2h and then the material is taken out.
Methods and principles of use:
1) opening commercially available crude beryllium in an air-isolated device, adding an oxidant, uniformly mixing, then putting into a raw material storage tank 2, and quantitatively feeding the mixed raw materials into a beryllium oxide crucible 10 from a crude bowl inlet 6 through a vacuum feeding module 4;
2) starting the low-temperature ultra-vacuum pump 14, and vacuumizing to 1.33 multiplied by 10-5pa, detecting the leak rate by using a helium mass spectrometer, wherein the leak rate is controlled to be 5 x 10-11pa；
3) And opening a high-temperature pipeline valve of the light phase receiver 18, opening a power supply of the heating device and the temperature control unit, controlling the heating speed to be 15 ℃/min, and keeping the temperature for 4h when the temperature is raised to 850 ℃. Preferentially distilling the low boiling point metal, and recovering the low boiling point metal through a condenser;
4) and (3) closing a high-temperature pipeline valve of the light phase receiver 18, opening a metal beryllium molecular distillation valve, and continuously heating to 1250 ℃ to perform molecular distillation on the main metal beryllium. The molecular distillation time is 8 h. And closing the metal beryllium receiver tube valve after the distillation is finished.
5) The high boiling point metal distillation outlet 26 is opened and pressurized to 0.2mpa with argon to allow the high boiling point metal to pass smoothly into the heavy phase receiver 20. The purity of the prepared metal beryllium is detected for many times as follows: 99.998 percent, belonging to ultra-pure grade.
The utility model discloses process flow is short, and production method is simple, and preparation cycle is short, and the beryllium metal purity of producing is high, ensures that the product of production reaches 5N purity.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not intended to limit the present invention, and all modifications, equivalents, improvements and the like that are made within the spirit and principles of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. An ultra-pure beryllium ultra-vacuum molecular distillation system is characterized by comprising an ultra-vacuum air pumping and vacuum control unit, a beryllium oxide ceramic crucible distillation unit arranged at the bottom of the ultra-vacuum air pumping and vacuum control unit, a heating device and a temperature control unit;
the ultra-vacuum pumping unit comprises a raw material storage tank (2), a vacuum feeding module (4), a finished product receiving module (15) and a full-range composite vacuum gauge A1(5) for controlling vacuum, wherein a feeding port (1) is formed in the top of the raw material storage tank (2), a viewing mirror (3) is arranged on the side face of the raw material storage tank (2), the vacuum feeding module (4) and the full-range composite vacuum gauge A1(5) are respectively arranged at the bottom of the raw material storage tank (2), a coarse bowl inlet (6) is formed between the vacuum feeding module (4) and the full-range composite vacuum gauge A1(5), a raw material quantitative push rod is arranged on the coarse bowl inlet (6), and the finished product receiving module (15) comprises an oxidized ceramic crucible metal beryllium receiving vessel (16) and a receiving module temperature transmitter (24);
the beryllium oxide ceramic crucible distillation unit comprises a beryllium oxide crucible (10) and a crucible supporting seat (9), the top of the beryllium oxide crucible (10) is connected to the coarse pot inlet (6), two sides of the beryllium oxide crucible (10) are respectively provided with a low-boiling-point metal distillation outlet (25) and a high-boiling-point metal distillation outlet (26), a distillation cavity (27) is arranged inside the beryllium oxide crucible (10), the outer wall of the distillation cavity (27) is provided with a connected heating rod insertion hole (11) and a heating temperature control element, the bottom of the beryllium oxide crucible (10) is provided with a temperature transmitter (8), the bottom of the temperature transmitter (8) is provided with a finished product outlet (13), the crucible supporting seat (9) is arranged at the bottom of the beryllium oxide crucible (10), and a maintenance hole (12) is arranged below the crucible supporting seat (9);
the heating device and the temperature control unit comprise a low-temperature super-vacuum pump (14), a light-phase vacuum pipeline (17) and a heavy-phase vacuum pipeline (22) which are arranged on two sides of the low-temperature super-vacuum pump (14) and a full-range composite vacuum gauge A2(23) for controlling vacuum, the low-temperature super-vacuum pump (14) is arranged at the bottom of the finished product outlet (13), the light-phase vacuum pipeline (17) is connected to the low-boiling-point metal distillation outlet (25) through a light-phase receiver (18), and the heavy-phase vacuum pipeline (22) is connected to the high-boiling-point metal distillation outlet (26) through a heavy-phase receiver (20).
2. The ultra-pure beryllium ultra-vacuum molecular distillation system of claim 1, wherein: and a feeding module supporting device (7) is arranged at the bottom of the vacuum feeding module (4).
3. The ultra-pure beryllium ultra-vacuum molecular distillation system of claim 1, wherein: the integrated heating rod insertion opening (11) is internally provided with a nickel alloy heating rod, and the beryllium oxide crucible (10) and the nickel alloy heating rod are formed in one step.
4. The ultra-pure beryllium ultra-vacuum molecular distillation system of claim 1, wherein: and receiver sight glasses (19) are arranged on the light phase receiver (18) and the heavy phase receiver (20).
5. The ultra-pure beryllium ultra-vacuum molecular distillation system of claim 1, wherein: the beryllium oxide crucible (10) is prepared by high-temperature oxidation of high-purity metal beryllium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021829340.2U CN212404223U (en) | 2020-08-28 | 2020-08-28 | Ultra-pure beryllium ultra-vacuum molecular distillation system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021829340.2U CN212404223U (en) | 2020-08-28 | 2020-08-28 | Ultra-pure beryllium ultra-vacuum molecular distillation system |
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| CN212404223U true CN212404223U (en) | 2021-01-26 |
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| CN202021829340.2U Active CN212404223U (en) | 2020-08-28 | 2020-08-28 | Ultra-pure beryllium ultra-vacuum molecular distillation system |
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