CN104030259A - Device for purifying high-purity argon gas - Google Patents
Device for purifying high-purity argon gas Download PDFInfo
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- CN104030259A CN104030259A CN201410247692.XA CN201410247692A CN104030259A CN 104030259 A CN104030259 A CN 104030259A CN 201410247692 A CN201410247692 A CN 201410247692A CN 104030259 A CN104030259 A CN 104030259A
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Abstract
The invention relates to a device for purifying a high-purity argon gas and belongs to the technical field of gas purification. The device comprises a resistance furnace, a quartz glass tube, joints and a water cooler, wherein the resistance furnace consists of a spiral type electric heating wire, a thermocouple, a temperature controller and a heat insulating material; the quartz glass tube is arranged in the resistance furnace and filled with sponge titanium; the joints are used for sealing and fixing two ends of the quartz glass tube; the water cooler is used for cooling the joints; a gas inlet outlet is connected with a high-purity argon-gas gas source, a gas outlet joint is connected with a flow rate meter capable of adjusting gas flow rate, and connected with gas consumption equipment; and after the resistance furnace is increased to a target temperature and kept for a certain time, a gas cylinder is opened to regulate the flow rate meter, so that high-purity argon gas flows through the heated sponge titanium along an arrowhead direction in the figure for being purified. The device disclosed by the invention is simple in structure, convenient to install, easy to operate, can effectively lower content of impurities in the high-purity argon gas to realize purifying the high-purity argon gas.
Description
Technical field
The invention belongs to gas purification technique field, specially refer to a kind of device that purifies high-purity argon gas.
Technical background
The character of argon gas is torpescence very, even the in the situation that of High Temperature High Pressure, also can not react with other material.Therefore; as protective atmosphere be widely used in produce and scientific research among, as the chemical vapor deposition in welding, stainless steel smelting, semiconductor fabrication process, crystal growth, thermooxidizing, extension, diffusion, polysilicon, tungsten, ion implantation, current-carrying, sintering and be used as the carrier gas etc. of the equipment such as gas chromatograph.Owing to mainly utilizing argon gas to be used as protective atmosphere, so require its purity high as far as possible, foreign matter content is low as far as possible, has reduced the effect of protection in order to avoid the impurity such as oxygen G&W wherein and material to be protected react.
According to national standard, the specification demands of argon gas divides straight argon (99.99%), high-purity argon (99.999%) and ultrapure argon (99.9999%), on market, to have purposes wide for straight argon and high-purity argon, low and the large feature of consumption of price, and though the ultrapure argon consumption of 6 N of purity is little, but be strategic materials indispensable in national defence and hard-core technology, be mainly used in electronics, metallurgical, in the branch of industry such as semi-conductor and instrumental analysis and scientific research, Si, the production of the monocrystalline such as GaAs and the necessary condition of direct-reading spectrometer work, also be protective atmosphere splendid in multiple Physical Chemical Experiment, compare the high-purity argon of 5 N, ultrapure argon can play more effectively protection to metal, significantly reduce the rate of loss of burning and nitrogenize etc. in pyroprocess.
Argon gas high purity purifies the general equipment of purifying in enormous quantities that adopts at present, after gas product packing, resupplying different production departments uses, but regrettably, even if factory can be purified to argon gas the degree of 6 N, but gas is filling, is storing, is transporting and using in link, pipeline and valve port etc. locate all to exist contaminated possibility, cause sneaking in gas impurity, and for production and the scientific research field of some electrician's materializations, even if be mixed with the impurity of trace in ultrapure argon, also may cause product rejection or the failure of an experiment.And the price of ultrapure argon is very high, several times even tens times of high-purity argon, therefore at the ultrapure argon of producing, costliness is not selected to buy in scientific research scene, but the lower high-purity argon of price is purified and makes it approach the purity that even surpasses 6 N, it is an effective selection, but the ultrapure argon refining plant of factory is very heavy, investment is very large, be difficult to carrying, cannot adapts to the on-the-spot needs of production and scientific research and purify in time the needs that obtain a small amount of ultrapure argon use.
Summary of the invention
For the deficiencies in the prior art part, the object of this invention is to provide a kind of device that purifies high-purity argon gas, and simple in structure, easy for installation, easy handling.
For achieving the above object, the present invention adopts following technical scheme: the present invention includes: the resistance furnace being comprised of volution nichrome wire, thermopair, temperature controller and thermal insulation material, be placed in resistance furnace and fill the quartz glass tube of titanium sponge, sealing the fixedly joint at quartz glass tube two ends, play the cooling-water machine of cooling joint effect etc.; Inlet suction port connects high-purity argon gas source of the gas, and air outlet adapter connects the under meter of adjustable gas flow velocity, then is connected to gas equipment; Resistance furnace rises to target temperature and keeps after for some time, makes the titanium sponge in quartz glass tube reach same temperature.Open gas cylinder adjust flux meter, make the high-purity argon gas of certain flow rate along the direction of arrow in figure, flow through the titanium sponge of heating, utilize the impurity such as titanium sponge and oxygen, nitrogen G&W react and high-purity argon is purified.
The water coolant of above-mentioned cooling-water machine preferably first arrives inlet suction port through water pipe, then arrives air outlet adapter through water pipe, finally by water pipe, flows back to cooling-water machine.
Above-mentioned thermopair is preferably fixed on resistance furnace inwall by high-temp glue, and the thermometric termination of thermopair is equal with the distance at resistance furnace two ends.
The working temperature of above-mentioned resistance furnace is preferably 700-900 ℃.
The length of above-mentioned quartz glass tube is preferably 30-100cm, and external diameter is preferably 5-20cm, and wall thickness is preferably 0.5-2.5cm.
Above-mentioned titanium sponge grade is preferably selected 0 grade, and particle diameter is preferably selected 0.1-10mm.
Above-mentioned thermal insulation material is preferably selected asbestos, and thickness is preferably 5-40cm.
The power of above-mentioned nichrome wire is preferably 1-5kw.
The refrigerating duty of above-mentioned cooling-water machine is preferably 0.3-1kw.
The material of above-mentioned inlet suction port and air outlet adapter is preferably selected stainless steel or brass.
Above-mentioned inlet suction port and air outlet adapter can take off from quartz glass tube easily, are convenient to the renewal of titanium sponge.
The flow rate control scope of above-mentioned under meter is preferably 0.1-10L/h.
The principle that the present invention purifies high-purity argon is that at the temperature based on more than 700 degree, the purification effect reaching compared with strong reaction occurs the impurity such as titanium sponge and oxygen in high-purity argon, nitrogen G&W.
The present invention has following beneficial effect:
1. the present invention can effectively reduce the oxygen in high-purity argon, the content of nitrogen G&W, can approach the purity that even surpasses 6 N, can meet a lot of scientific researches, production scene needs and purify in time the needs that obtain a small amount of ultrapure argon use, such as heating of metal is played to the effect of atmosphere protection, reduce oxidation and the nitrogenize of metal in pyroprocess;
2. the invention belongs to no-hydrogen deoxygen, avoided the potential safety hazard that may cause owing to adding hydrogen;
3. the present invention is without vacuumizing, and two joint easy accessibility can judge whether it needs to upgrade by titanium sponge variable color degree after unloading, and has simple in structurely, is convenient to install the features such as good purification.
Accompanying drawing explanation
Fig. 1 is a kind of apparatus structure schematic diagram that purifies high-purity argon gas.
In figure: 1. temperature controller, 2. joint, 3. cooling-water machine, 4. water pipe, 5. thermopair, 6. thermal insulation material, 7. volution nichrome wire, 8. quartz glass tube, 9. titanium sponge, 10. under meter.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
As shown in Figure 1, a kind of device that purifies high-purity argon gas, comprise: the resistance furnace being formed by volution nichrome wire 7, thermopair 5, temperature controller 1 and thermal insulation material 6, be placed in resistance furnace and fill the quartz glass tube 8 of titanium sponge 9, sealing the fixedly joint 2 at quartz glass tube 8 two ends, play the cooling-water machine 3 of cooling joint 2 effects etc.; Inlet suction port 2-1 connects high-purity argon gas source of the gas, and air outlet adapter 2-2 connects the under meter 10 of adjustable gas flow velocity, then is connected to gas equipment.
Utilize the present invention and special purpose device thereof, completed the experiment of doing for high-purity argon, its experiment situation and result are described below:
This covering device has been assembled and after sealing propertytest is qualified, controlling temperature controller makes quartz glass tube be warmed up to 900 ℃ and be incubated 30 minutes with the temperature rise rate of 10 ℃/min, guarantee that the titanium sponge in pipe also reaches this temperature, from inlet suction port, pass into high-purity argon gas, adjust flux meter makes argon gas through purifying flow into the speed of 10L/h the process furnace that another has been evacuated to vacuum, in process furnace, fill high-purity iron block (oxide skin on iron block surface is polished) of heavy 100mg, make to be full of in process furnace the high-purity argon through purifying, process furnace is raised to 1580 ℃ with the temperature rise rate of 20 ℃/min afterwards, and be incubated after ten minutes, with 15 ℃/min, drop to room temperature, open heating furnace cover, observe pure iron, find that its surface is comparatively smooth bright clean, (in this kind of situation, Pure Iron Surface is pitch-dark far below the situation of direct use high-purity argon for degree of oxidation, oxidation is serious).
Claims (10)
1. a device that purifies high-purity argon gas, mainly comprise: the resistance furnace being formed by volution nichrome wire (7), thermopair (5), temperature controller (1) and thermal insulation material (6), be placed in resistance furnace and fill the quartz glass tube (8) of titanium sponge (9), sealing the fixedly joint (2-1,2-2) at quartz glass tube (8) two ends, for the cooling-water machine (3) of cooling joint (2-1,2-2); Inlet suction port (2-1) connects high-purity argon gas source of the gas, and air outlet adapter (2-2) connects the under meter (10) of adjustable gas flow velocity, then is connected to gas equipment.
2. according to the device of the purification high-purity argon gas described in claims 1, it is characterized in that, the water coolant of described cooling-water machine (3) first arrives inlet suction port (2-1) through water pipe (4-1), then arrives air outlet adapter (2-2) through water pipe (4-3), finally by water pipe (4-2), flows back to cooling-water machine.
3. according to the device of the purification high-purity argon gas described in claims 1, it is characterized in that, described thermopair (5) is fixed on resistance furnace inwall by high-temp glue, and the thermometric termination of thermopair (5) is equal with the distance at resistance furnace two ends.
4. according to the device of the purification high-purity argon gas described in any one in claim 1～3, it is characterized in that, the working temperature of described resistance furnace is 700-900 ℃.
5. according to the device of the purification high-purity argon gas described in any one in claim 1～3, it is characterized in that, the length of described quartz glass tube (8) is 30-100cm, and external diameter is 5-20cm, and wall thickness is 0.5-2.5cm.
6. according to the device of the purification high-purity argon gas described in any one in claim 1～3, it is characterized in that, described titanium sponge (9) grade is 0 grade, and particle diameter is 0.1-10mm.
7. according to the device of the purification high-purity argon gas described in any one in claim 1～3, it is characterized in that, described thermal insulation material (6) is asbestos, and thickness is 5-40cm.
8. according to the device of the purification high-purity argon gas described in any one in claim 1～3, it is characterized in that, it is characterized in that, the power of described volution nichrome wire (7) is 1-5kw.
9. according to the device of the purification high-purity argon gas described in any one in claim 1～3, it is characterized in that, it is characterized in that, the refrigerating duty of described cooling-water machine (3) is 0.3-1kw.
10. according to the device of the purification high-purity argon gas described in any one in claim 1～3, it is characterized in that, it is characterized in that, the material of described inlet suction port (2-1) and air outlet adapter (2-2) is stainless steel or brass.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410247692.XA CN104030259A (en) | 2014-06-06 | 2014-06-06 | Device for purifying high-purity argon gas |
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| CN201410247692.XA CN104030259A (en) | 2014-06-06 | 2014-06-06 | Device for purifying high-purity argon gas |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110261459A (en) * | 2019-06-17 | 2019-09-20 | 北京科技大学 | A kind of device for controlling extremely low oxygen content in atmosphere and measuring its partial pressure of oxygen |
| CN114602260A (en) * | 2022-04-01 | 2022-06-10 | 遵义钛业股份有限公司 | Purification device of high-purity argon gas |
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| JPH05128594A (en) * | 1991-10-31 | 1993-05-25 | Sony Corp | Method for measuring displacement |
| CN1970133A (en) * | 2005-11-22 | 2007-05-30 | 先普半导体技术(上海)有限公司 | Ultra-high purity inert gas purification device and purification method |
| CN101181982A (en) * | 2007-12-05 | 2008-05-21 | 四川普瑞净化设备有限公司 | Device and method for preparing high-purity argon gas |
| CN102100999A (en) * | 2009-12-16 | 2011-06-22 | 贵阳铝镁设计研究院 | Method for purifying inert gases and purifying device |
| CN102795608A (en) * | 2012-08-15 | 2012-11-28 | 天津环煜电子材料科技有限公司 | Method for purification and recovery of argon, nitrogen and hydrogen by rare earth alloy-sponge titanium mixture |
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2014
- 2014-06-06 CN CN201410247692.XA patent/CN104030259A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05128594A (en) * | 1991-10-31 | 1993-05-25 | Sony Corp | Method for measuring displacement |
| CN1970133A (en) * | 2005-11-22 | 2007-05-30 | 先普半导体技术(上海)有限公司 | Ultra-high purity inert gas purification device and purification method |
| CN101181982A (en) * | 2007-12-05 | 2008-05-21 | 四川普瑞净化设备有限公司 | Device and method for preparing high-purity argon gas |
| CN102100999A (en) * | 2009-12-16 | 2011-06-22 | 贵阳铝镁设计研究院 | Method for purifying inert gases and purifying device |
| CN102795608A (en) * | 2012-08-15 | 2012-11-28 | 天津环煜电子材料科技有限公司 | Method for purification and recovery of argon, nitrogen and hydrogen by rare earth alloy-sponge titanium mixture |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110261459A (en) * | 2019-06-17 | 2019-09-20 | 北京科技大学 | A kind of device for controlling extremely low oxygen content in atmosphere and measuring its partial pressure of oxygen |
| CN110261459B (en) * | 2019-06-17 | 2024-07-19 | 北京科技大学 | Device for controlling extremely low oxygen content in atmosphere and measuring oxygen partial pressure thereof |
| CN114602260A (en) * | 2022-04-01 | 2022-06-10 | 遵义钛业股份有限公司 | Purification device of high-purity argon gas |
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Application publication date: 20140910 |