CN103505980B - One realizes and maintains pressure≤15 × 10 -13torr vacuum pumping method - Google Patents
One realizes and maintains pressure≤15 × 10 -13torr vacuum pumping method Download PDFInfo
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- CN103505980B CN103505980B CN201210204296.XA CN201210204296A CN103505980B CN 103505980 B CN103505980 B CN 103505980B CN 201210204296 A CN201210204296 A CN 201210204296A CN 103505980 B CN103505980 B CN 103505980B
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Abstract
The present invention relates to a kind of realization and maintenance pressure≤15 × 10
-13torr vacuum pumping method, adopts following methods: by vacuum tank outside for vaccum-pumping equipment access, bled by vavuum pump, leak detection is without leak source; Utilize the mode of external heat to toast vaccum-pumping equipment and outside vacuum tank, reach ultrahigh vacuum requirement, inject liquid nitrogen to liquid nitrogen Thin-wall Barrel successively, until liquid nitrogen thin wall cylinder and oxygen-free copper sleeving temperature constant after (~-180 DEG C); Use titanium sublimation pump 90 seconds, stable about half an hour, vacuum chamber vacuum≤15 × 10 can be realized
-13torr.Advantage of the present invention is easy and simple to handle, and cost is low, and efficiency is high.
Description
Technical field
The present invention relates to a kind of realization and maintenance pressure≤1.5 × 10
-12torr vacuum pumping method, can realize experimental study explorer portion has better vacuum environment in ultrahigh vacuum equipment.
Background technology
In the research field of ultrahigh vacuum experiment, gas component remaining inside vacuum, the mass spectrometry detection of the corresponding product of small-signal can be affected, especially at Surface Science, the material of adsorption is relatively less, and effects on surface reaction or desorption material out will accomplish the detection of zero background, improve the degree of accuracy of signal analysis, and can maintain this experiment condition in experimentation, be that peoples dream is thought all the time.
Realize vacuum up to now and be better than 1.5 × 10
-12torr, and the vacuum pumping method that can maintain more than 24 hours, have two kinds.
First method, as shown in Figure 1, has reached (<8 × 10 under the condition of ultrahigh vacuum in ultravacuum chamber vacuum
-11torr), directly use helium cold head 20, cooling oxygen-free copper block 30, reaches and is better than 1.5 × 10
-12the vacuum of torr.
Second method, as shown in Figure 2, has reached (<8 × 10 under the condition of ultrahigh vacuum in ultravacuum chamber vacuum
-11torr), inject liquid nitrogen in liquid nitrogen thin wall cylinder 8, then use helium cold head, cooling oxygen-free copper block, reaches and is better than 1.5 × 10
-12the vacuum of torr.【Linetal，Rev.Sci.Instrum.69,1642(1998)】
But their shortcoming is:
(1) this kind of vacuum is generally used for the weak-signal measurement of scientific research field, aspires for stability, and vibration can be introduced for complete equipment in the use procedure of helium cold head, the detection accuracy of signal can be had influence on;
(2) helium cold head uses more complicated, consuming time long, for the realization of ultrahigh vacuum, conventional means all will through overbaking, and in this process, the core component of helium cold head is needed to take apart, after baking, installed back by these core components, this process is complicated again, and easily damage parts, complex operation;
(3) helium cold head cost is too high, needs often to safeguard;
Summary of the invention
The object of the invention is providing one can realize and maintain pressure≤1.5 × 10
-12torr, raises the efficiency, and reduces costs, method easy and simple to handle.
For realizing above object, technical scheme of the present invention is to provide one and is realizing and maintaining pressure being better than 1.5 × 10
-12torr vacuum pumping method, is characterized in that, the titanium film adsorbed gas that the inwall utilizing two liquid nitrogen thin wall cylinder extremely cold and titanium sublimation pump evaporate, and realizes vacuum and is better than 1.5 × 10
-12torr vacuum pumping method, its method is:
Vavuum pump is accessed vacuum pump interface and the second vacuum pump interface by step 1. respectively, vacuumizes, and baking vaccum-pumping equipment and vacuum tank make its temperature be in 150-200 DEG C, and baking limit, limit vacuumizes, pressure≤3 × 10 in vaccum-pumping equipment and vacuum tank
-8during torr, toast complete, room temperature is down to by vaccum-pumping equipment and vacuum tank, pressure≤8 × 10 now in vaccum-pumping equipment and vacuum tank
-11torr, reaches ultrahigh vacuum;
Step 2. imported and exported by liquid nitrogen and gateway respectively to continuing injection liquid nitrogen in the interlayer of cooled with liquid nitrogen interlayer and liquid nitrogen thin wall cylinder, waiting for that titanium sublimation pump and oxygen-free copper sleeving temperature are down to constant, bleeds with adsorption form in cooled with liquid nitrogen interlayer inner surface, liquid nitrogen thin wall cylinder surface, anaerobic copper sheathing inner surface;
Step 3. uses titanium sublimation pump, and be evaporated to by titanium on liquid nitrogen thin wall cylinder inner surface and anaerobic copper sheathing inwall and form cold titanium film, cold titanium film is bled by absorption, makes pressure≤1.5 × 10 in vaccum-pumping equipment
-12torr.
Advantage of the present invention is:
(1) realize easily, simple to operate, efficiency is higher;
(2) cost is realized lower
Due to 1 in the present invention) adopt the mode of pole cold surface absorption to vacuumize, do not introduce vibration, for it provides guarantee at the stability in use of ultrahigh vacuum research equipment; 2) realize pole cold surface to be lowered the temperature by cooled with liquid nitrogen, the injection of liquid nitrogen, based on automatically, decreases artificial restraint, adds cooling stability, and operator, only it should be noted that the change of several instrument numerical value, just can know vacuum condition; 3) adopt cooled with liquid nitrogen cooling, thin wall cylinder directly contacts with liquid nitrogen, effectively raises rate of temperature fall; 4) cavity only needs once mounting, just can normally use later, does not need the repeatedly dismounting of picture helium cold head in bake process and installation.
Accompanying drawing explanation
Fig. 1. former method 1 realizes and maintains pressure≤1.5 × 10
-12torr vacuum pumping method schematic diagram;
Fig. 2. former method 2 realizes and maintains pressure≤1.5 × 10
-12torr vacuum pumping method schematic diagram;
Fig. 3. be better than 1.5 × 10 for realizing vacuum in a kind of ultrahigh vacuum cavity of the present invention
-12torr vacuum pumping method schematic diagram.
Specific implementation method
Below in conjunction with accompanying drawing 3. and embodiment, the present invention will be further described.
Embodiment
As shown in fig. 3, the present invention's one obtains parital vacuum and is better than 1.5 × 10 in vacuum tank
-12torr method schematic diagram, its specific implementation method is as follows:
(1) equipment is accessed ultra high vacuum container by access port 6.The preposition ionization device of mass spectrometry detector is arranged on anaerobic copper sheathing 7, and preposition ionization device is arranged on the aperture axis of anaerobic copper sheathing 7 front and back end, coordinates preposition ionization device and the small-signal of reaction zone in ultrahigh vacuum equipment collected by supporting simple detector with ionization device.
(2) this vacuum equipment and outside vacuum tank are by difference vacuum pump evacuation
(3) when vacuum equipment and outside vacuum tank all reach ~ 10
-7during torr, carry out helium leak check, as without leaking, then can toast vacuum equipment and outside vacuum tank at the temperature of 150 ± 10 DEG C, if there is leakage, stop vacuumizing, process leak source, until without leakage.
(4) when pressure≤3 × 10 in vaccum-pumping equipment and vacuum tank
-8during torr, toast complete, room temperature is down to by vaccum-pumping equipment and vacuum tank, pressure≤8 × 10 now in vaccum-pumping equipment and vacuum tank
-11torr, reaches ultrahigh vacuum; As do not reached, repeat step (3).
(5) by liquid nitrogen import and export 2 and gateway 9 inject liquid nitrogen respectively to continuing in the interlayer of cooled with liquid nitrogen interlayer 3 and liquid nitrogen thin wall cylinder 8, waiting for that titanium sublimation pump 5 and anaerobic copper sheathing 7 temperature are down to constant, bleeds with adsorption form in cooled with liquid nitrogen interlayer 3 inner surface, liquid nitrogen thin wall cylinder 8 surface, anaerobic copper sheathing 7 inner surface;
(6) use titanium sublimation pump 90 seconds, be evaporated to by titanium on liquid nitrogen thin wall cylinder 8 inner surface and anaerobic copper sheathing 7 inwall and form cold titanium film, cold titanium film is bled by absorption, makes pressure≤1.5 × 10 in vaccum-pumping equipment
-12torr.
Claims (4)
1. one kind realizes and maintains pressure≤15 × 10
-13torr vacuum pumping method, is characterized in that: under the prerequisite not introducing vibration, utilizes the mode that cold surface adsorbs, and realizes and maintain vacuum being better than 15 × 10
-13torr, its method is:
The vaccum-pumping equipment adopted is the enclosed cavity that a lower end is provided with through hole, vaccum-pumping equipment is provided with vacuum pump interface (1), the tubular cooled with liquid nitrogen interlayer (3) of the both ends open up and down of hollow is provided with in the internal face of vaccum-pumping equipment, cooled with liquid nitrogen interlayer (3) is provided with liquid nitrogen and imports and exports (2), and cooled with liquid nitrogen interlayer (3) bottom is provided with the tubular anaerobic copper sheathing (7) of upper end open, lower end closed; In vaccum-pumping equipment, be provided with liquid nitrogen thin wall cylinder (8), liquid nitrogen thin wall cylinder (8) be upper and lower both ends open, cylindrical shell that sidewall is hollow sandwich structure, liquid nitrogen thin wall cylinder (8) is provided with liquid nitrogen gateway (9); Titanium sublimation pump (5) is had in the suspension of liquid nitrogen thin wall cylinder (8) inside;
Described vaccum-pumping equipment outer wall is provided with ring-type access port (6), vaccum-pumping equipment is connected with outside vacuum tank by ring-type access port (6), vaccum-pumping equipment is connected with vacuum tank by through hole (4), and vacuum tank is provided with the second vacuum pump interface;
Vavuum pump is accessed vacuum pump interface (1) and the second vacuum pump interface by step 1. respectively, vacuumize, baking vaccum-pumping equipment and vacuum tank make its temperature be in 150-200 DEG C, and baking limit, limit vacuumizes, pressure≤3 × 10 in vaccum-pumping equipment and vacuum tank
-8during torr, toast complete, room temperature is down to by vaccum-pumping equipment and vacuum tank, pressure≤8 × 10 now in vaccum-pumping equipment and vacuum tank
-11torr, reaches ultrahigh vacuum;
Step 2. is imported and exported (2) and gateway (9) by liquid nitrogen and is injected liquid nitrogen respectively to interior the continuing of interlayer of cooled with liquid nitrogen interlayer (3) and liquid nitrogen thin wall cylinder (8), waiting for that titanium sublimation pump (5) and anaerobic copper sheathing (7) temperature are down to constant, bleeds with adsorption form in cooled with liquid nitrogen interlayer (3) inner surface, liquid nitrogen thin wall cylinder (8) surface, anaerobic copper sheathing (7) inner surface;
Step 3. uses titanium sublimation pump (5), and be evaporated to by titanium on liquid nitrogen thin wall cylinder (8) inner surface and anaerobic copper sheathing (7) inwall and form cold titanium film, cold titanium film is bled by absorption, makes pressure≤15 × 10 in vaccum-pumping equipment
-13torr.
2. vacuum pumping method according to claim 1, is characterized in that:
Thin wall cylinder (8) is connected with the mode of anaerobic copper sheathing (7) by welding, realizes sealing;
Whole vaccum-pumping equipment can be connected on other vacuum tanks by connector (6), if access vacuum tank, anaerobic copper sheathing (7) and thin wall cylinder (8) are by weld or the mode of screw tightening is connected, anaerobic copper sheathing (7) can be processed through hole (4), realize detector is installed, wiring function.
3. vacuum pumping method according to claim 1, is characterized in that:
The diameter of described through hole is≤5mm and >=0.01mm.
4. vacuum pumping method according to claim 1, is characterized in that:
The cavity volume of described vaccum-pumping equipment is≤15L and >=0.5L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210204296.XA CN103505980B (en) | 2012-06-20 | 2012-06-20 | One realizes and maintains pressure≤15 × 10 -13torr vacuum pumping method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210204296.XA CN103505980B (en) | 2012-06-20 | 2012-06-20 | One realizes and maintains pressure≤15 × 10 -13torr vacuum pumping method |
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| Publication Number | Publication Date |
|---|---|
| CN103505980A CN103505980A (en) | 2014-01-15 |
| CN103505980B true CN103505980B (en) | 2016-04-27 |
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|---|---|---|---|
| CN201210204296.XA Expired - Fee Related CN103505980B (en) | 2012-06-20 | 2012-06-20 | One realizes and maintains pressure≤15 × 10 -13torr vacuum pumping method |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106930923B (en) * | 2015-12-30 | 2018-11-30 | 核工业西南物理研究院 | A kind of large size straight-plate-type titanium sublimation pump structure |
| CN113237943B (en) * | 2021-05-12 | 2023-10-20 | 中国科学技术大学 | Reduce mass spectrum detection H 2 And H 2 Ultrahigh vacuum device for O background noise |
| CN114878841A (en) * | 2022-04-26 | 2022-08-09 | 中国工程物理研究院材料研究所 | Interconnecting switching vacuum device and ultrahigh vacuum equipment |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB902161A (en) * | 1960-02-25 | 1962-07-25 | New York Air Brake Co | Improvements in ultra high vacuum chambers |
| CN101692368A (en) * | 2009-09-30 | 2010-04-07 | 中国科学院等离子体物理研究所 | High-temperature superconductive magnet system for magnetically confined plasma propeller |
-
2012
- 2012-06-20 CN CN201210204296.XA patent/CN103505980B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB902161A (en) * | 1960-02-25 | 1962-07-25 | New York Air Brake Co | Improvements in ultra high vacuum chambers |
| CN101692368A (en) * | 2009-09-30 | 2010-04-07 | 中国科学院等离子体物理研究所 | High-temperature superconductive magnet system for magnetically confined plasma propeller |
Non-Patent Citations (2)
| Title |
|---|
| Low-temperature ultra-high-vacuum scanning tunneling microscope;R. Gaisch et al.;《Ultramicroscopy》;19921231;1621-1626 * |
| 超高真空中使用的高纯过渡金属蒸发源;陆华 等;《真空科学与技术》;20000531(第3期);210-213 * |
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|---|---|
| CN103505980A (en) | 2014-01-15 |
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