CN101445876A - Withdrawing device of high-purity mercury in a mercury purifying device and method - Google Patents
Withdrawing device of high-purity mercury in a mercury purifying device and method Download PDFInfo
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- CN101445876A CN101445876A CNA2008102045641A CN200810204564A CN101445876A CN 101445876 A CN101445876 A CN 101445876A CN A2008102045641 A CNA2008102045641 A CN A2008102045641A CN 200810204564 A CN200810204564 A CN 200810204564A CN 101445876 A CN101445876 A CN 101445876A
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Abstract
The invention discloses a withdrawing device of high-purity mercury in a mercury purifying device and a method; the method is characterized in that: the purified mercury is sucked into a mercury withdrawing vessel under the action of negative pressure by an adapter which is not in contact with a third party. The withdrawing device of the high-purity mercury has the advantages that: in the whole process, the purified mercury is only in contact with a high-purity quartz pipe and the vessel, and a purifying device and the vessel for withdrawing the mercury are in a nitrogen-protecting state, thus preventing a purifying system and the purified mercury from being polluted in the process, and the operation is very convenient and safe.
Description
Technical field
The present invention relates to the material purification techniques among the semiconductor material preparation technology, the withdrawing device and the method that specifically refer to high-purity mercury in a kind of mercury purifying plant, it is mainly used in the preparation of II-VI tellurium cadmium mercury epitaxial material, and then is used for the manufacturing of high-performance infrared focal plane device and the application of infrared detection technique.
Technical background
The history in 50 years has been experienced in the development of tellurium-cadmium-mercury infrared material and device, the research and the production of unit and polynary photocon and monochromatic infrared focal plane device two generations infrared eye have successively been finished, after entering 2000, Hg-Cd-Te material and device stride into again with polychrome, very long wave and single photon detection are the third generation infrared focus plane technology New Times of feature, along with improving constantly of device performance level, device is also more and more higher to the purity requirement of material, especially the avalanche-type device of very long wave HgCdTe device and single photon, in order to improve the knot impedance, increase breakdown reverse voltage, requirement to material purity is higher, and raw-material on-the-spot the purification progressively is included into the common process of Hg-Cd-Te material preparation.In three kinds of starting material of Te-Cd-Hg, mercury at room temperature is fluent material, and be than the material that is easier to oxidation and is stained, the oxidation of introducing in packing, transportation and the storage process and staining, mercury needed to carry out primary purification before being used for Hg-Cd-Te material, and avoided introducing in the process as far as possible and stain.In the prior art, the quartz apparatus of placing purification mercury is that the heat shrink by Meltability polytetrafluorethyletubular (PFA) plastics tubing (see figure 1) is connected with equipment for purifying, coupling device is that pipe two is enclosed within connected silica tube outer wall respectively, heat with naked light, cooling back plastics tubing shrinks the back and realizes sealing with silica tube, must plastics tubing be cut off with cutter when taking off once more.There are two shortcomings in such mode, the one, the reliability of sealing is not high, heat factor such as inhomogeneous and can cause the stopping property variation, the 2nd, add hot tie-in and cutting and disconnect all very complicated, heating will consider evenly, and grasps suitable Heating temperature, considers quartz member during disconnection, should cut off and can not overexert, whether also be X factor in the plastics tubing heating if having volatile matter to discharge in addition.The existence of this problem has caused certain difficulty to mercury purification common process.
Summary of the invention
Based on the problem that exists on the mercury purification techniques, the present invention proposes a kind of improved apparatus and method.
Fig. 2 is high-purity mercury withdrawing device high pressure protective gas pressure-controlling schematic diagram of the present invention; the ultimate principle of this device is to utilize the pressure reduction mercury of back in high-purity mercury collection vessel 1 of will purifying to be transported to and to get in the mercury vessel 4, whole device relate to inhale mercury pipeline 7, pollution-free docking adapter 3, communicating vessels switch 2, get mercury vessel 4, mercury draws silica tube 13, negative pressure switch 6 and the PFA integral parts such as pipeline 12 that are tightly connected.
Stainless steel sealing docking adapter 3 is to get mercury vessel 4 and purification system to realize the part that is connected gradually, after getting mercury vessel 4 and taking off, and in the sealing that available silica tube is silently unstowed docking adapter 3, the state when this also is mercury purification system works better.The sealing of O type circle is all adopted in the sealing of docking adapter 3 two and silica tube, sealing principle is, the inner screw sheath of trim ring 10 is on the outside screw of stainless steel pipe connecting 11, by rotation trim ring 10, can push pressure ring 9, pressure ring 9 acts on the O type circle 8, and extruding makes O type circle lateral expansion, thereby the slit between silica tube and the stainless steel pipe connecting is blocked, realize sealing.
The suction mercury pipeline 7 that is made in high-purity mercury collection vessel 1 is to be the designed passage of the taking-up of mercury, when communicating vessels switch 2 is in closing condition, negative pressure is incorporated into inhales mercury pipeline 7 through getting mercury vessel 4, docking adapter 3 by vacuum pump, utilize the pressure reduction of inhaling between the mercury pipeline 7 inside and outside equal height mercury faces that mercury is extruded from inhale mercury pipeline 7, in this system, pressure reduction is about 1atm, the height that can extrude is about 13.5cm, promptly inhale mercury pipeline 7 height and can not surpass 13.5cm, otherwise the mercury of collection vessel 1 bottom can't be sucked into and get mercury vessel 4.
The effect of communicating vessels switch 2 is when getting the mercury operation, by closing communicating vessels, to provide pressure reduction inside and outside inhaling mercury pipeline 7.When the quantity of taking out mercury reaches requirement, can suction mercury pipeline 7 inside and outside differential pressures be rapidly disappeared by opening communicating vessels switch 2, the output of mercury stops immediately.The existence of communicating vessels switch 2 also provides passage for protective gas flow to docking adapter 3, and after getting mercury vessel 4 and docking adapter 3 separates, protective gas constantly flows out from docking adapter 3, reduces the air admission purifying plant in the environment.
Adopt such get the mercury apparatus and method after, mercury is purified gets the improvement of mercury technology aspect following three:
A) security is improved.After utilizing the docking adapter of O type circle sealing, getting taking off of mercury vessel only needs to rotate trim ring 10 and can finish, and having avoided may be to quartz apparatus and pipeline destroyed when lancinating plastics tubing;
B) Mi Feng reliability is improved.As adopt the plastics tubing collapsed seal, as heat inhomogeneous or temperature appropriately all can cause poor sealing, though, seal bad can the detection, but caused technology to do over again, simultaneously through regular meeting by the total system suction, gas in the environment can be drawn into purification system, influences the purity of system;
C) getting the amount of mercury can be controlled.In former technology, use the mercury of purification, need all mercury of purifying are taken off from purifying plant, remaining mercury can only be purified again again.And after using this device, can control the quantity of taking out mercury, realize what what get with.
Description of drawings
Fig. 1: Meltability polytetrafluorethyletubular (PFA) plastics tubing.
Fig. 2: high-purity mercury withdrawing device high pressure protective gas pressure-controlling schematic diagram;
Wherein:
1---high-purity mercury collection vessel;
2---the communicating vessels switch;
3---docking adapter;
4---get the mercury vessel;
5---quartzy rectifier unit;
6---negative pressure connects switch;
7---inhale the mercury pipeline;
8---the O RunddichtringO;
9---pressure ring;
10---trim ring;
11---the stainless steel pipe connecting;
12---the PFA pipeline that is tightly connected;
13---mercury is drawn silica tube.
Embodiment:
(1) described high-purity mercury collector (1) and inhale mercury pipeline (7), mercury and draw the fairlead of silica tube (13) and communicating vessels switch (2) and be quartz member, by high temperature sintering they are linked together, before using, quartz member and polyfluortetraethylene pipe all need to remove surface dirt and grease through standard cleaning technology;
(2) because the purifying plant of mercury is complete quartzy rectifier unit, high-purity mercury withdrawing device also mostly is a quartz member, be difficult for adopting the such hard connecting mode of quartzy butt joint between the two, the hard connecting mode theory says it is best mode, but just in case cause the infringement of quartz member in the operation, reparation is with extremely difficult, therefore, in the device that the present invention proposes, being connected between collection vessel 1 and the quartzy rectifier unit 5 adopted tetrafluoroethylene 12 (PFA) (see figure 1), and the outflow that guarantees high-purity mercury in the design of butt joint silica tube can not contact with polyfluortetraethylene pipe, because the existence of polyfluortetraethylene pipe, no longer be that rigidity connects between high-purity mercury withdrawing device and the purifying plant, certain displacement or distortion can take place between the two, security increases greatly;
(3) communicating vessels switch 2 must adopt two cutting ferrule mode of connection valve switch of semiconductor material special use, equally, this mode of connection can't directly be connected with silica tube, between need to use the tetrafluoroethylene tube transitions, because connecting pipe does not directly contact with high-purity mercury, can not pollute high-purity mercury;
(4) between the external diameter of its internal diameter of processing request of stainless steel sealing docking adapter 3 (in the O type circle) and silica tube and the clearance control of outer its internal diameter of O type circle and O type circle external diameter at about 20% of O type circle thickness, the smooth finish of O type circle sealing place stainless steel inwall is better than 1 micron;
(5) 2 points are accomplished in the design requirements of getting mercury vessel 4 of band negative pressure, one provide negative pressure take out mouthful will get the mercury device above, taking out mouthful place's processing quartz baffle prevents that the mercury that may splash from entering and takes out a mouthful place, the 2nd, for providing the vacuum pump of negative pressure, it need adopt oil-less pump, to avoid the vacuum pump volatilization gas to getting the contamination of mercury system and purification system;
(6) communicating vessels switch 2 and stainless steel sealing docking adapter 3 need be provided with fixed mechanism, with convenient corresponding operation, avoids operating and causes moving of quartz member.
Claims (8)
1. the withdrawing device of high-purity mercury in the mercury purifying plant, it by communicating vessels switch (2), inhale that mercury pipeline (7), mercury are drawn silica tube (13), docking adapter (3), got mercury vessel (4), negative pressure switch (6) and the PFA pipeline (12) that is tightly connected forms, it is characterized in that: described suction mercury pipeline (7) is inserted in high-purity mercury solution of the high-purity mercury collection vessel (1) in the quartzy rectifier unit (5), and its rear end is drawn silica tube (13) with mercury and is communicated with; Described mercury is drawn silica tube (13) three Link Ports in two ends and middle part up and down, the middle part Link Port is communicated with described suction mercury pipeline (7), the upper end Link Port is communicated with described communicating vessels switch (2) afterwards by the PFA pipeline (12) that is tightly connected and is communicated with high-purity mercury collection vessel (1), the lower end Link Port with access mercury vessel (4) after docking adapter (3) is communicated with; Negative pressure line through negative pressure switch (6) with get mercury vessel (4) and be communicated with.
2. the withdrawing device of high-purity mercury in a kind of mercury purifying plant according to claim 1, it is characterized in that: the length of described suction mercury pipeline (7) is less than 13.5cm.
3. the withdrawing device of high-purity mercury in a kind of mercury purifying plant according to claim 1, it is characterized in that: described docking adapter (3) is made up of stainless steel pipe connecting (11), stainless steel pressure ring (9), stainless steel trim ring (10) and O RunddichtringO (8), screwed stainless steel trim ring (10) is tightened on and compresses stainless steel pressure ring (9) when stainless steel pipe connecting (11) is gone up, and realizes drawing silica tube (13) and getting being tightly connected of mercury vessel (4) with mercury by stainless steel pressure ring (9) extruding O RunddichtringO (8).
4. the withdrawing device of high-purity mercury in a kind of mercury purifying plant according to claim 1, it is characterized in that: the gap between the internal diameter at the stainless steel pipe connecting (11) of described docking adapter (3) and O type circle (8) sealing position and the external diameter of O type circle (8) is 20% of O type circle (a 8) thickness, and the smooth finish of inner wall surface is better than 1 micron.
5. the withdrawing device of high-purity mercury in a kind of mercury purifying plant according to claim 1 is characterized in that: described mercury draw silica tube (13) the gap between the internal diameter of the middle O RunddichtringO (8) of external diameter and junctor (3) is 20% of O type circle (a 8) thickness.
6. the withdrawing device of high-purity mercury in a kind of mercury purifying plant according to claim 1 is characterized in that: described communicating vessels switch (2) adopts two cutting ferrule mode of connection valve switch of semiconductor material special use.
7. the withdrawing device of high-purity mercury in a kind of mercury purifying plant according to claim 1, it is characterized in that: the fairlead that described high-purity mercury collector (1) and suction mercury pipeline (7), mercury are drawn silica tube (13) and communicating vessels switch (2) is quartz member, by high temperature sintering they is linked together.
8. high-purity mercury extracting method based on the described device of claim 1 is characterized in that it may further comprise the steps:
A. when communicating vessels switch (2) when being in closing condition, open negative pressure switch (6), from the negative pressure of vacuum pump through get mercury vessel (4), docking adapter (3) is incorporated into and inhales mercury pipeline (7), utilize the pressure reduction of inhaling between the inside and outside equal height mercury face of mercury pipeline (7) that mercury is extruded from inhale mercury pipeline (7), high-purity mercury flows into through the mercury introduction pipe and gets mercury vessel (4);
B. when high-purity mercury quantity of taking out reaches requirement, can suction mercury pipeline (7) inside and outside differential pressure be rapidly disappeared by opening communicating vessels switch (2), the output of mercury stops immediately;
C. close negative pressure switch (6), open communicating vessels switch (2), unscrew the last sealing of junctor (3) and get the trim ring of mercury vessel (4), take off mercury vessel (4);
D. a sealing of silently docking adapter (3) being unstowed with silica tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102045641A CN101445876B (en) | 2008-12-15 | 2008-12-15 | Withdrawing device of high-purity mercury in a mercury purifying device and method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102045641A CN101445876B (en) | 2008-12-15 | 2008-12-15 | Withdrawing device of high-purity mercury in a mercury purifying device and method |
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| CN101445876A true CN101445876A (en) | 2009-06-03 |
| CN101445876B CN101445876B (en) | 2011-04-27 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102363843A (en) * | 2011-11-19 | 2012-02-29 | 元亮科技有限公司 | Device and method for purifying mercury |
| CN105586492A (en) * | 2016-03-17 | 2016-05-18 | 江苏三联安全评价咨询有限公司 | Waste mercury recovery and purification device and use method thereof |
| CN112014028A (en) * | 2020-08-27 | 2020-12-01 | 北京智创芯源科技有限公司 | Quartz tube assembly and vacuum inspection method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102836575A (en) * | 2012-09-04 | 2012-12-26 | 济南美医林电子仪器有限公司 | Device suitable for collecting mercury waste liquid of mercury electrodes |
-
2008
- 2008-12-15 CN CN2008102045641A patent/CN101445876B/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102363843A (en) * | 2011-11-19 | 2012-02-29 | 元亮科技有限公司 | Device and method for purifying mercury |
| CN102363843B (en) * | 2011-11-19 | 2013-08-28 | 元亮科技有限公司 | Device and method for purifying mercury |
| CN105586492A (en) * | 2016-03-17 | 2016-05-18 | 江苏三联安全评价咨询有限公司 | Waste mercury recovery and purification device and use method thereof |
| CN105586492B (en) * | 2016-03-17 | 2017-07-18 | 江苏三联安全评价咨询有限公司 | A kind of useless mercury reclaims purifying plant |
| CN112014028A (en) * | 2020-08-27 | 2020-12-01 | 北京智创芯源科技有限公司 | Quartz tube assembly and vacuum inspection method thereof |
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| Publication number | Publication date |
|---|---|
| CN101445876B (en) | 2011-04-27 |
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