CN2165441Y - Integrative hydrogen permeability parameter measuring apparatus - Google Patents
Integrative hydrogen permeability parameter measuring apparatus Download PDFInfo
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- CN2165441Y CN2165441Y CN 93228795 CN93228795U CN2165441Y CN 2165441 Y CN2165441 Y CN 2165441Y CN 93228795 CN93228795 CN 93228795 CN 93228795 U CN93228795 U CN 93228795U CN 2165441 Y CN2165441 Y CN 2165441Y
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Abstract
The utility model relates to an integrative hydrogen permeability parameter measuring apparatus, which is composed of a sample chamber, a monitoring chamber, a hydrogen charging chamber, and a standard leakage chamber which is provided with standard leakage holes. The utility model is characterized in that the hydrogen charging chamber which is on the utmost front end is respectively connected with the upstream side of the sample chamber and one side of the standard leakage chamber, and the other side of the standard leakage chamber and the downstream side of the sample chamber are commonly connected with the monitoring chamber. The upstream side of the sample chamber is also connected with the monitoring chamber through a bypass pipeline; the monitoring chamber is connected with an ion pump, and each chamber room is separated with a valve. The utility model has the advantages of simple operation and higher stability and accuracy.
Description
The utility model relates to the vacuum analysis and testing technology, and a kind of device of measuring hydrogen permeability parameters in the metal is provided especially.
Hydrogen permeability parameters in the metal comprises permeability, coefficient of diffusion and solubleness, is the mechanism of hydrogen embrittlement of research material and the basic parameter of anti-hydrogen performance, also is the important design parameter of construction materials such as oil, chemical industry, ocean, space flight and nuclear technology.Therefore, accurately measure these parameters in the metal material no matter to the fundamental research of material, still, all significant to the Important Project design.In the assay method in the past, the most important thing is high temperature gas phase hydrogen infiltration technology, used instrument and equipment, more early stage work mostly is general glass vacuum system, the ultrahigh vacuum gas phase hydrogen permeability parameters determinator of all-metal construction has appearred in the late nineteen seventies early eighties, and vacuum tightness can reach 10
-5Torr greatly reduces the background hydrogen richness of system, has improved the sensitivity and the accuracy of assay determination, has enlarged the assay determination scope.List of references ［ 1～5 ］ provides four kinds of determinators, wherein with the typical case the most of Deventer ［ 5 ］, as shown in Figure 1, the all-metal construction ultra-high vacuum system of forming by two ionic pumps (1) unit, the garden disk-like sample, welded seal, with the hydrogen stream of partial pressure analyzer monitoring infiltration, the following shortcoming of existing apparatus ubiquity: 1. device is complicated, troublesome poeration, every covering device needs 2～3 ionic pumps (1) unit, troublesome poeration not only, and cost is also high.2. stability and poor accuracy.Because of downstream, existing apparatus sample chamber ionic pump pumping speed less, have only 20 liters/second as Quick device downstream ionic pump pumping speed, under the dynamic monitoring situation, be difficult to guarantee that monitoring chamber pumping speed is constant in the hydrogen process of osmosis like this, thereby influence the stability and the reliability of measured result.
It is a kind of simple to operate that the purpose of this utility model is to provide, stability and the high hydrogen permeability parameters determinator of accuracy.
The hydrogen penetrating parameters determinater that the utility model provides, form by sample chamber, monitoring chamber (3), hydrogen-filling chamber (12) and the mark leakage chamber (5) that contains referance leak, it is characterized in that: 1. hydrogen-filling chamber (12) is foremost, leak chamber (5) one sides with sample chamber upstream side (9) and mark respectively and link to each other, mark leaks chamber (5) opposite side to be tied with monitoring chamber (3) mutually with downstream, sample chamber (6) are common; Sample chamber upstream side (9) is also tied with monitoring chamber (3) mutually by bypass duct, and 2. tie mutually with a high sub-pump (1) monitoring chamber (3), and is 3. spaced apart with valve between each chamber.The bypass that hydrogen-filling chamber (12) and monitoring chamber (3) connect with mechanical pump is provided with molecular sieve well on the beam (15) and the cold well of liquid nitrogen (14).The utlity model has following advantage: 1. simple in structure, cheap, easy to operate.Because whole device only adopts an ionic pump, the document same device adopts 2 or three ionic pumps relatively, and structure is simplified greatly, has reduced cost, has made things convenient for operation.2. the stability and the reliability of measurement result have been improved.When the method that adopts dynamic monitoring is measured the hydrogen permeability parameters, must guarantee that monitoring chamber pumping speed is constant, otherwise that quantitative measurement becomes is impossible.This device adopts (300 liters/second) ionic pump that pumping speed is bigger, and the appropriate design by piping system, thereby has guaranteed the constant of monitoring chamber pumping speed in the hydrogen process of osmosis.Calculate proof, when vacuum tightness changes three orders of magnitude, monitoring chamber pumping speed change be no more than ± 1.5%.Thereby structure that this device is measured is more accurate than the document device, and is stable also better.3. applied range.The sample bigger (φ 43 gardens dish) of Yin Ben device design, so both can measure the higher body centred cubic material of permeability (as α-Fe, low alloy steel) the hydrogen permeability parameters in, can measure the hydrogen permeability parameters of the extremely low face-centered cubic material of permeability (as the low stainless steel of Ovshinsky, heat-resisting alloy etc.) again.By embodiment in detail the utility model is described in detail below in conjunction with accompanying drawing.
Accompanying drawing 1 is the determinator synoptic diagram of people's such as Van Deventer hydrogen permeability parameters.
A kind of hydrogen penetrating parameters determinater that accompanying drawing 2 provides for the utility model.
Embodiment:
This device as shown in Figure 2, can be described from following five aspects: 1. overall construction design: sample chamber (comprising upstream (9) side and downstream (6)), monitoring chamber (3), bypass duct between hydrogen-filling chamber (12) and sample chamber upstream side (9) and the monitoring chamber (3) leaks chamber (5) for partly main with the mark that contains referance leak, all design by ultrahigh vacuum, all the other are for partly auxiliary, by general high vacuum design.2. monitor chamber (3) design: key problem is that will to guarantee to monitor in the hydrogen process of osmosis chamber (3) pumping speed constant, ionic pump (1) (300 liters/second) that pumping speed is bigger of this device apolegamy, and appropriate design monitoring chamber (3) size (internal diameter 35mm, high 500mm), so both guaranteed that monitoring chamber (3) pumping speed was constant, guaranteed again that there was certain pumping speed monitoring chamber (3).Four-electrode spectrum rule heads (4) are positioned at upper end, monitoring chamber (3), and as far as possible near downstream, sample chamber (6) outlet, to improve detection sensitivity.3. sample chamber design: it is bigger that this device sample chamber is designed, the garden dish sample of the φ 43 that can pack into, and purpose is to enlarge the test material scope.In addition, contain referance leak mark leakage chamber (5) and link to each other, guaranteed like this to enter monitoring chamber (3) with the hydrogen stream that permeates by sample with same state, improved the reliability of standard by the hydrogen source of referance leak with downstream, sample chamber (6).A high-purity N has also been designed in downstream, sample chamber (6)
2Introduce arm, avoid air to enter the ultrahigh vacuum pipeline as far as possible.4. hydrogen-filling chamber (12) design: the hydrogen of hydrogen-filling chamber (12) both can have been introduced sample chamber upstream side (9), can introduce referance leak (5) again, also had an arm to link to each other with mechanical pump, so that hydrogen is discharged.Hydrogen-filling chamber (12) is equipped with a resistance strain gage (10), and it can accurately measure the hydrogen pressure of 0-800torr.Also has a pressure vacuum gauge (11), accurately to obtain the hydrogen pressure of hydrogen-filling chamber (12) fast.5. auxiliary partly design: the design that mainly is cold well (14) to ionic pump (1) and cold well to pipeline between the hydrogen-filling chamber (12) and annex.This partly pipeline be mainly used in elementary vacuum drawn and fill hydrogen and row's hydrogen, add the cold well of a liquid nitrogen (14) between they and the mechanical pump and molecular sieve keeps off oil well (15), purpose is to avoid mechanical pump oil to diffuse into ultra-high vacuum system.With pipeline that hydrogen-filling chamber (12) is connected on design one high-purity N
2Introduce arm, charge into high-purity N toward the ultrahigh vacuum pipeline when purpose is the dismounting sample chamber
2The concrete operations step of this device is as follows:
1. dress sample: valve-off A(18), C(20), E(22), G(24), J(26), Open valve D(21 simultaneously), H(25), M(28), N(29), charge into high-purity N toward downstream, sample chamber (6) and upstream side (9)
2, to an atmospheric pressure.Open flange of sample room,, with the fresh sample of packing into immediately after the absolute ethyl alcohol cleaning, sealing sample chamber.In the process that open the sample chamber, make high-purity N
2Slowly, flow out by sample (7) seal flange, in case air diffuses into the sample chamber by the both sides, sample chamber.After sample is packed into, valve-off D(21), N(29), start mechanical pump immediately, and open valve O(30), B(19), E(22), with the N in downstream, sample chamber (6) and the upstream side (9)
2Gas extracts.
2. system's baking: as both sides, sample chamber N
2After gas is got rid of, the upright ultrahigh vacuum part (comprising pipeline, flange, valve etc.) that reaches with the heating tape apparatus for baking, at this moment the forepump adsorption pump that starts ionic pump (1) is (at pipeline place, vacuum gauge (17) place, do not mark among the figure), valve-off O(30) and H(25), make valve B(19), C(20), E(22), G(24), F(23), J(26) be in opening, with (9), downstream (6) on adsorption pump suction monitoring chamber (3) and the sample chamber.And continue suction hydrogen-filling chamber (12) with mechanical pump.Toast after four hours, stop to toast valve-off B(19), found and open valve A(18), with upward (9), downstream (6) of ionic pump (1) suction monitoring chamber (3) and sample chamber, while valve-off M(28), stop mechanical pump.Baking is finished.3. mass spectrum standard: be the hydrogen stream of Quantitative Monitoring by the sample infiltration, four-electrode spectrum (4) must standard.We adopt metal to flatten referance leak (its leak rate is known) standardization, open quadrupole mass spectroscope (4), preheating half an hour, valve-off C(20), make E(22), G(24), F(23) still locate opening, by needle-valve L(31) charge into certain pressure hydrogen to hydrogen-filling chamber (12), open valve K(27 then), open the mass spectrum registering instrument simultaneously, the hydrogen that infiltrates monitoring chamber (3) by referance leak flows by mass spectrum with H
+The ion flow form is noted, and after ion flow signal to be recorded reaches steady state (SS), stops record, Open valve M(28), with mechanical pump hydrogen-filling chamber (12) hydrogen is got rid of, close M(28).Change hydrogen pressure, again standard, so a standard 4-5 pressure.Accurately hydrogen pressure should open valve K(27 one) afterwards indicate by the continuous instrument of resistance strain gage (10).Voltage power is emitted the leak rate of small opening, provides leak hole leak rate at last to H
+The ion flow calibration curve.Saturating parametric measurement: make valve A before the mensuration, (18) C(20), E(22), G(24), J(26) be in opening, other valves all are in closed condition, be warmed up to uniform temperature to heating furnace, treat to continue go up (9) that chamber (3) and sample chamber are monitored in suction with ionic pump behind the temperature stabilization, downstream (6) a period of time (about 2-3 hour), vacuum tightness up to B-A rule (2) indication is constant, valve-off C(20) and J(26), by needle-valve L(31) charge into the certain pressure ultra-pure hydrogen toward hydrogen-filling chamber (12), close needle-valve L(31), open valve H(25 rapidly), make hydrogen enter sample chamber upstream side (9), open H(25) time open the registering instrument of four-electrode spectrum (4), the hydrogen stream that is penetrated into monitoring chamber (3) by sample equally by four-electrode spectrum (4) with H
+The ion flow form is noted, after treating that ion flow reaches steady-state value, stop experiment, turn off mass spectrum, with mechanical pump the hydrogen in hydrogen-filling chamber (12) and the sample chamber upstream side (9) is extracted, valve-off H(25), open C(20), Open valve J(26 slowly again) make B-A rule (2) indication vacuum tightness be not less than 10 when (J(26 is opened in attention)
-5torr, make device return to the preceding state of experiment.Note, fill hydrogen pressure to open valve H(25 during experiment) after regulate (10) indicated force value and be as the criterion.The H that arrives according to experimental record
+Ion flow by calibration curve and respective formula, can calculate the permeability of hydrogen, coefficient of diffusion, solubleness and each activation energy data.
Claims (2)
1, a kind of hydrogen penetrating parameters determinater, form by sample chamber, monitoring chamber (3), hydrogen-filling chamber (12) and the mark leakage chamber (5) that contains referance leak, it is characterized in that: (a) hydrogen-filling chamber (12) is foremost, leak chamber (5) one sides with sample chamber upstream side (9) and mark respectively and link to each other, mark leaks chamber (5) opposite side to be tied with monitoring chamber (3) mutually with downstream, sample chamber (6) are common; Sample chamber upstream side (12) is also tied with monitoring chamber (3) mutually by bypass duct; (b) tie mutually with a high sub-pump (1) monitoring chamber (3); (c) spaced apart between each chamber with valve.
2,, it is characterized in that the bypass that hydrogen-filling chamber (12) and monitoring chamber (3) connect with mechanical pump is provided with molecular sieve retaining oil well (15) and the cold well of liquid nitrogen (14) by the described hydrogen penetrating parameters determinater of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93228795 CN2165441Y (en) | 1993-07-21 | 1993-07-21 | Integrative hydrogen permeability parameter measuring apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93228795 CN2165441Y (en) | 1993-07-21 | 1993-07-21 | Integrative hydrogen permeability parameter measuring apparatus |
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| Publication Number | Publication Date |
|---|---|
| CN2165441Y true CN2165441Y (en) | 1994-05-18 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93228795 Expired - Fee Related CN2165441Y (en) | 1993-07-21 | 1993-07-21 | Integrative hydrogen permeability parameter measuring apparatus |
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| CN (1) | CN2165441Y (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100427942C (en) * | 2005-12-30 | 2008-10-22 | 中国科学院海洋研究所 | Method and device for studying metal hydrogen infiltration in medium under dynamic load condition |
| CN103592206A (en) * | 2013-11-19 | 2014-02-19 | 中国科学院金属研究所 | Method for testing hydrogen diffusivity or permeability in metal and specific device therefor |
| CN113188974A (en) * | 2021-04-30 | 2021-07-30 | 中国特种设备检测研究院 | High-pressure hydrogen permeation test device and method for liner material of IV-type gas cylinder |
-
1993
- 1993-07-21 CN CN 93228795 patent/CN2165441Y/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100427942C (en) * | 2005-12-30 | 2008-10-22 | 中国科学院海洋研究所 | Method and device for studying metal hydrogen infiltration in medium under dynamic load condition |
| CN103592206A (en) * | 2013-11-19 | 2014-02-19 | 中国科学院金属研究所 | Method for testing hydrogen diffusivity or permeability in metal and specific device therefor |
| CN113188974A (en) * | 2021-04-30 | 2021-07-30 | 中国特种设备检测研究院 | High-pressure hydrogen permeation test device and method for liner material of IV-type gas cylinder |
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| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |