CN2727730Y - A hydrogen charging-discharging performance testing device by volumetric method - Google Patents

A hydrogen charging-discharging performance testing device by volumetric method Download PDF

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CN2727730Y
CN2727730Y CN 200420070419 CN200420070419U CN2727730Y CN 2727730 Y CN2727730 Y CN 2727730Y CN 200420070419 CN200420070419 CN 200420070419 CN 200420070419 U CN200420070419 U CN 200420070419U CN 2727730 Y CN2727730 Y CN 2727730Y
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hydrogen
valve
testing device
performance testing
volumetric method
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CN 200420070419
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成会明
吴成章
刘畅
徐世涛
***
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Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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Abstract

The utility model provides a hydrogen charging-discharging performance testing device by volumetric method, mainly comprising a high voltage hydrogen gas source, an air receiver, a sample chamber, a vacuum air pump, a discharging hydrogen test system and a computer. The utility model is characterized in that the air receiver is connected with the high voltage hydrogen gas source, the discharging hydrogen test system, the sample chamber and the vacuum air pump separately passing through a valve 1, a valve 2, a valve 3 and a valve 4. The air receiver and the sample chamber are arranged in a constant temperature cabinet. The air receiver is provided with a pressure sensor and a temperature sensor 1, the sample chamber is provided with a temperature sensor 2. The valve 1, the valve 2, the pressure sensor, the temperature sensor 1, the temperature sensor 2 are connected with the computer through a collecting tray. The utility model has the advantages that it can provide the high voltage hydrogen gas in high purity, and reduce greatly leak rate of the system, exactly test the change of pressure and temperature in the system and amend the change of the pressure in the system because of temperature fluctuation through calculating.

Description

A kind of volumetric method stores the hydrogen performance testing device
Technical field:
The utility model relates to the device that a kind of volumetric method test hydrogen storage material stores the hydrogen performance, the particularly proving installation that stores the hydrogen performance of hydrogen storage material under mesohigh and middle low temperature.
Background technology:
The method that mensuration hydrogen storage material commonly used stores the hydrogen characteristic mainly contains volumetric method and gravimetric method.The volume ratio juris mainly is dependent on the equation of gas state:
n = P × V Z × R × T
Wherein: n is the amount of hydrogen; P is a pressure in the system; V is the volume of system; R is a gas law constant; T is the temperature of system; Z is the compressibility factor (being determined by pressure P and temperature T) of hydrogen.
As can be seen, the amount of hydrogen is determined by the pressure and temperature of hydrogen in the system in the certain volume from formula.So can come the amounts of hydrogen in the counting system by volume, the temperature and pressure of accurate mensuration system, and if hydrogen storage material is housed in this system, then the variable quantity of hydrogen is the hydrogen storage content of hydrogen storage material.
In the PCT device that the hydrogen storage property of routine is tested, generally Hydrogen Vapor Pressure lower (being lower than 6MPa), and main pipeline and hydrogen storage system all are in the room temperature, and system pressure is subjected to room temperature influence bigger.
Carbon nano-material is the hydrogen storage material that present a kind of tool has great prospects for development, but according to relevant report, needs very high pressure (reaching more than the 10MPa) when the absorption hydrogen such as materials such as CNT and nano carbon fibers.Under so high pressure, some leakage part a little of fluctuation, system of temperature can cause the very mistake of measurement, even test error can surpass actual hydrogen storage content.This also is that at present different seminars has a very major reason of big difference when the hydrogen storage content of test CNT.
Summary of the invention:
The purpose of this utility model is to provide a kind of test hydrogen storage material that reduces test error to store the device of hydrogen performance.
The utility model provides a kind of volumetric method to store the hydrogen performance testing device, mainly by the High Pressure Hydrogen source of the gas, air storage chamber (10), sample chamber (11), vacuum pump (19), putting hydrogen test macro (21) and computing machine (18) forms, it is characterized in that: air storage chamber (10) is respectively by valve I (6), valve II (7), valve III (8), valve IV (9) and High Pressure Hydrogen source of the gas, put hydrogen test macro (21), sample chamber (11) is connected with vacuum pump (19), air storage chamber (10) and sample chamber (11) place the constant temperature Xiangli, air storage chamber (10) has pressure transducer (16), temperature sensor I (14), sample chamber (11) has temperature sensor II (15), valve I (6), valve II (7), pressure transducer (16), temperature sensor (14) I, temperature sensor (14) II links to each other with computing machine (18) by hub (17).
The volumetric method that the utility model provides stores the hydrogen performance testing device, and its High Pressure Hydrogen source of the gas can be hydrogen cylinder (1) and hydrogen supercharger (2), and the hydrogen that hydrogen cylinder (1) comes out has become high pressure hydrogen through hydrogen supercharger (2).
The volumetric method that the utility model provides stores the hydrogen performance testing device, can be provided with filtrator I (5) between its High Pressure Hydrogen source of the gas and the valve I (6), with the purity that guarantees to enter intrasystem hydrogen.
The volumetric method that the utility model provides stores the hydrogen performance testing device, can be provided with liquid nitrogen cold trap (20) between its vacuum pump (19) and the valve IV (9), is back in the system to prevent pump oil gas.
The volumetric method that the utility model provides stores the hydrogen performance testing device, can be provided with joint (13) and/or filtrator II (12) between its sample chamber (11) and the valve II (7), with the purity and the oxidation of minimizing sample in operating process of hydrogen in the assurance system.
The volumetric method that the utility model provides stores the hydrogen performance testing device, and its High Pressure Hydrogen source of the gas place is parallel with the helium tank (3) of band valve V (4), so that with helium each relevant portion of system is carried out volume calibration.
The volumetric method that the utility model provides stores the hydrogen performance testing device, and its valve I (6), valve II (7) use the procedure auto-control switch, with the operation that realizes semi-automation.
The advantage that the volumetric method that the utility model provides stores the hydrogen performance testing device is: this proving installation can not only provide the hydrogen of high-purity high pressure, and greatly reduce the slip of system, accurately test system internal pressure and variation of temperature, and revise because the variation of the system pressure that the fluctuation of temperature causes by calculating.
Description of drawings:
Fig. 1 is the structural representation of this device;
Fig. 2 is this device test curve of 120 hours of pressurize under 125 atmospheric pressure;
Fig. 3 for survey the pressure-temperature curve.
Embodiment:
The structural representation of this device as shown in Figure 1.
High pressure hydrogen origin system part, adopt high-purity high pressure hydrogen, the hydrogen that is about in the hydrogen cylinder (1) is incorporated in the hydrogen supercharger (2), control the Hydrogen Vapor Pressure of supercharger (2) outlet by the heating-up temperature of control supercharger (2), and pressure can be regulated arbitrarily between 0MPa~15MPa, pass through two-stage filter I (5) then, just can guarantee to enter intrasystem hydrogen and be 99.9999% High Purity Hydrogen.
The vacuum system part adds liquid nitrogen cold-trap (20) between vacuum pump (19) and hydrogen storage system, can prevent effectively that pump oil gas is back in the system.
Data acquisition and control system part, with the data of 16 bit data capture cards collection, carry out data storing and can show pressure and variation of temperature in real time by computing machine (18) again from high-precision pressure sensor (16) and temperature sensor I (14), temperature sensor II (15).
Constant temperature oven in the utility model (22) be a temperature range from-80 ℃~100 ℃ adjustable constant temperature ovens, its temperature fluctuation is less than 0.5 ℃.In this proving installation, valve I (6), valve II (7), valve III (8), valve IV (9), air storage chamber (10), sample chamber (11), filtrator II (12), rapid-acting coupling (13), temperature sensor I (14) and temperature sensor II (15), pressure transducer (16) and the stainless steel pipes joint (13) etc. that connects them are all put in the constant temperature oven (22), in the time of can reducing to test since the pressure that the room temperature fluctuation causes change.
Adopt rapid-acting coupling (13) in the utility model, so that being connected of sample chamber (11) and hydrogen storage system, and when disconnecting this rapid-acting coupling (13), joint (13) two ends are sealing automatically all, can make like this sample externally (as in glove box) dress get in the process and can not be exposed in the air, reduced the oxidation of sample.Valve I (6), valve II (7), valve III (8), valve IV (9) are the autoclave diaphragm valve in this device, slip is low, pipeline is an inwall electropolishing pipe, reduced the leakage of hydrogen to a great extent, and (11) export department adds 0.5 μ m filtrator II (12) in the sample chamber, can reduce the pollution that system is caused by sample.
Valve I (6) and valve II (7) are pneumatic diaphragm valve in the utility model, by the computer program gauge tap, have realized the semi-automation of operation substantially.The utility model has taken into full account source of error in the test of storage hydrogen, makes whole test process improve precision, and makes operation more simple and convenient.
The utility model mesohigh sources of hydrogen place is parallel with the helium tank (3) of band valve V (4), so that with helium each relevant portion of system is carried out volume calibration.
The operation of this device is as follows:
1. hydrogen storage system volume calibration
Open valve I (6), valve II (7), valve III (8), valve IV (9), system vacuumized, and with the helium of helium tank (3) to system each relevant portion segmentation carry out volume calibration.
2. hydrogen storage system slip test
Under 125bar hydrogen to pressure maintaining performance of the present utility model test, the gained test curve as shown in Figure 2, the amount of hydrogen does not almost change behind the pressurize 120h as can be seen.To obtaining its slip after the curve linear match is 3.02 * 10 -8Mmol/s.
3. store up the hydrogen testing procedure
Carry out accurately storing the hydrogen performance test after the volume calibration.
Open rapid-acting coupling (13), in the sample chamber (11) of in glove box sample being packed into, strict restriction sample water oxygen content because joint (13) seals, can guarantee not have the introducing of oxygen in operating process.After installing sample, connect rapid-acting coupling (13), and open valve II (7), valve IV (9), and regulate constant temperature oven (22) temperature and be 60 ℃~80 ℃ and sample chamber (11) and air storage chamber (10) were vacuumized about 2 hours, regulate constant temperature oven (22) temperature then to experimental temperature.
Valve-off II (7), valve IV (9), the temperature of regulating hydrogen supercharger (2) makes Hydrogen Vapor Pressure reach a certain desired value, opens valve I (6) then, and high-purity high pressure hydrogen is introduced in the air storage chamber (10).Hydrogen is opened valve II (7) then in about 2 hours balances of this balance, makes hydrogen storage material inhale hydrogen.After suction hydrogen finishes, open valve III (8), by putting hydrogen test macro (21) test hydrogen desorption capacity.
The collection of pressure and temperature can have two kinds of acquisition modes according to program setting in the utility model: 1 for sampling by the time; 2 is pressing force or temperature variation sampling.The switch of valve I (6) and valve II (7) can be manual, also can be according to the procedure auto-control switch.
4. pressure correction
The temperature-pressure curve that records during pressurize as shown in Figure 3.As can be seen from the figure, in 12 hours, the interior temperature substantially constant of constant temperature oven (22), its temperature wave momentum only is 0.2 ℃, the size of Hydrogen Vapor Pressure vary with temperature and change and coincide mutually fine, the pressure that 0.2 ℃ temperature fluctuation brings changes and is about 0.01MPa.
In theory, have according to the equation of gas state:
n = P × V Z × R × T
From formula as can be known, for a certain amount of gas in the certain volume,
Figure Y20042007041900082
Be a constant (wherein Z is the function of P and T, at room temperature, Z=0.99987+0.0062P).Choose 2 points (seeing the following form) from experiment, P/ZT is a constant substantially in the table as can be seen, and the variation of pressure only causes owing to variation of temperature in the illustrative experiment, so in actual computation, can come calibrating (base measuring) pressure by the variation of real-time detected temperatures:
P?(MPa) T (K) Z P/ZT
12.174 292.65 1.07534 0.038685
12.165 292.46 1.07528 0.038683
Annotate: P is an absolute pressure in the table, promptly records gauge pressure+0.1MPa

Claims (7)

1, a kind of volumetric method stores the hydrogen performance testing device, mainly by the High Pressure Hydrogen source of the gas, air storage chamber (10), sample chamber (11), vacuum pump (19), putting hydrogen test macro (21) and computing machine (18) forms, it is characterized in that: air storage chamber (10) is respectively by valve I (6), valve II (7), valve III (8), valve IV (9) and High Pressure Hydrogen source of the gas, put hydrogen test macro (21), sample chamber (11) is connected with vacuum pump (19), air storage chamber (10) and sample chamber (11) place the constant temperature Xiangli, air storage chamber (10) has pressure transducer (16), temperature sensor I (14), sample chamber (11) has temperature sensor II (15), valve I (6), valve II (7), pressure transducer (16), temperature sensor I (14), temperature sensor II (15) links to each other with computing machine (18) by hub (17).
2, volumetric method according to claim 1 stores the hydrogen performance testing device, it is characterized in that: described High Pressure Hydrogen source of the gas is hydrogen cylinder (1) and hydrogen supercharger (2).
3, volumetric method according to claim 1 stores the hydrogen performance testing device, it is characterized in that: be provided with filtrator I (5) between described High Pressure Hydrogen source of the gas and the valve I (6).
4, volumetric method according to claim 1 stores the hydrogen performance testing device, it is characterized in that: be provided with liquid nitrogen cold trap (20) between described vacuum pump (19) and the valve IV (9).
5, volumetric method according to claim 1 stores the hydrogen performance testing device, it is characterized in that: be provided with joint (13) and/or filtrator II (12) between described sample chamber (11) and the valve II (7).
6, volumetric method according to claim 1 stores the hydrogen performance testing device, it is characterized in that: described High Pressure Hydrogen source of the gas place is parallel with the helium tank (3) of band valve V (4).
7, store the hydrogen performance testing device according to the described volumetric method of one of claim 1~6, it is characterized in that: described valve I (6), valve II (7) use the procedure auto-control switch.
CN 200420070419 2004-08-25 2004-08-25 A hydrogen charging-discharging performance testing device by volumetric method Expired - Fee Related CN2727730Y (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101788443B (en) * 2010-01-29 2011-07-20 青岛科瑞新型环保材料有限公司 Prediction method for service life of vacuum thermal-insulation plate
CN102269666A (en) * 2011-03-31 2011-12-07 哈尔滨工业大学(威海) Gas sample enrichment apparatus for ultra-low leakage rate detection, and method thereof
CN101561382B (en) * 2008-04-15 2012-02-15 哈尔滨理工大学 Aluminum alloy melt hydrogen partial pressure dynamic measuring method
CN103439474A (en) * 2013-08-14 2013-12-11 扬州大学 Method for determining hydrogen absorption/desorption thermodynamic parameter of hydrogen storage alloy
CN104181075A (en) * 2014-08-27 2014-12-03 四川材料与工艺研究所 Comprehensive hydrogen storage bed performance testing device and determination method using same
CN105606767A (en) * 2015-12-28 2016-05-25 中国工程物理研究院材料研究所 High vacuum-high pressure combined hydrogen storage property testing device for low hydrogen absorption equilibrium pressure material
CN105628294A (en) * 2014-10-31 2016-06-01 中国航空工业集团公司西安飞机设计研究所 Oxygen source pressure correction display method
CN105928855A (en) * 2016-04-20 2016-09-07 中国原子能科学研究院 Measuring apparatus and method for surface micropressure tritium absorption rate constant of material
CN108225470A (en) * 2017-12-31 2018-06-29 合肥通用机械研究院 A kind of hydrogen-holder volume calculations method in hydrogen cyclic fatigue test system
CN114428034A (en) * 2021-12-13 2022-05-03 中国原子能科学研究院 Alloy hydrogen storage performance testing device and connection structure layout method thereof

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101561382B (en) * 2008-04-15 2012-02-15 哈尔滨理工大学 Aluminum alloy melt hydrogen partial pressure dynamic measuring method
CN101788443B (en) * 2010-01-29 2011-07-20 青岛科瑞新型环保材料有限公司 Prediction method for service life of vacuum thermal-insulation plate
CN102269666A (en) * 2011-03-31 2011-12-07 哈尔滨工业大学(威海) Gas sample enrichment apparatus for ultra-low leakage rate detection, and method thereof
CN103439474A (en) * 2013-08-14 2013-12-11 扬州大学 Method for determining hydrogen absorption/desorption thermodynamic parameter of hydrogen storage alloy
CN104181075A (en) * 2014-08-27 2014-12-03 四川材料与工艺研究所 Comprehensive hydrogen storage bed performance testing device and determination method using same
CN104181075B (en) * 2014-08-27 2016-05-11 四川材料与工艺研究所 A kind of storage hydrogen bed performance comprehensive test device that adopts carries out method for measuring
CN105628294A (en) * 2014-10-31 2016-06-01 中国航空工业集团公司西安飞机设计研究所 Oxygen source pressure correction display method
CN105628294B (en) * 2014-10-31 2018-12-14 中国航空工业集团公司西安飞机设计研究所 A kind of oxygen source pressure correction display methods
CN105606767A (en) * 2015-12-28 2016-05-25 中国工程物理研究院材料研究所 High vacuum-high pressure combined hydrogen storage property testing device for low hydrogen absorption equilibrium pressure material
CN105928855A (en) * 2016-04-20 2016-09-07 中国原子能科学研究院 Measuring apparatus and method for surface micropressure tritium absorption rate constant of material
CN108225470A (en) * 2017-12-31 2018-06-29 合肥通用机械研究院 A kind of hydrogen-holder volume calculations method in hydrogen cyclic fatigue test system
CN114428034A (en) * 2021-12-13 2022-05-03 中国原子能科学研究院 Alloy hydrogen storage performance testing device and connection structure layout method thereof

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