Helium Leak Test

Introduction Leaks are special types of defects which can have a major importance in systems where they have influence on safety and performance. Many objects will have a reduced reliability if they contain leaks. Leak testing is a non destructive examination method which is used for detection and localisation of leaks and for measurement of leakage in systems or objects which is under vacuum or pressure. Before a leak test examination is performed it is necessary to determine if the examination is to ascertain whether leaks are present or not, overall leak detection, or if the examination is to determine the location of a leak, localising leak detection. In some cases an examination for overall leak detection is performed first, and if leaks are detected, the localising method is applied for pinpointing of the leak. This is however not always required nor possible. Secondly it is necessary to determine the leak rate which can be tolerated, as no objects are 100% tight. That is the requirements to tightness of the object. If for example the object have to be watertight, a leak rate below 10-4 mbar l/s will be sufficient. But if the object for example is to be used in the chemical industry the requirements can be a leak rate below 10-6 mbar l / s. In leak testing a pressure difference between the outer and the inner side of the object to be examined is produced. Subsequently the amount of gas or liquid which is passing through a leak is measured. In helium leak test helium is used as a search gas, from this the nomination of the method. In principle two methods are applied for leak testing and localisation of leaks, the "Vacuum method" and the "Overpressure method". At the "Vacuum method" the object to be examined for leaks is evacuated and sprayed from the outside with a search gas, in this case Helium. The gas enters through any leaks present in the object and is detected by a sensor connected to the leak test instrument. At the "Overpressure method" the object to be examined for leaks is filled with a search gas, Helium, under slight overpressure. The search gas escapes through any leaks present to the outside and is detected by a detector probe. This detector probe is in most cases called a "sniffer" acting as a gas sampling probe. For both methods specially developed leak detectors are available. The object under test should, if possible, be tested according to its final mode of use, i.e. if it is used under vacuum, the vacuum method should be applied, if it is finally pressurised, the overpressure method should be adopted. Examples of testing with the two methods are illustrated below. The Vacuum method is illustrated with the Hood Test and the Tracer Probe Test and the Overpressure method with the Hood test, the Bombing test and the Detector Probe or Sniffer test. Vacuum method - Hood test The Hood Test is an overall leak test. The evacuated test object is covered with a (plastic) hood. The space between the test object and the hood is filled with Helium from the search gas reservoir so the total outer surface of the test object is exposed to the Helium search gas. The helium enters through all leaks present at

the evacuated test object and thus the detector connected to it. The detector now indicates the total leak rate. The hood test can for example be used for examination of small vessels.

Helium Leak Test, Vacuum Method, Hood Test Vacuum method - Tracer probe test At the tracer probe test the same set-up as used for the hood test is applied, but without the hood. A spray gun is used to spray a fine jet of helium search gas at areas suspected of leaking. Again the helium enters through leaks present at the evacuated test object and the detector connected to it. The detector indicates if a leak is present at the area the helium search gas is exposed to. The tracer probe test can for example be used on seals, flange connections, weld seams etc..

Helium Leak Test, Vacuum Method, Tracer probe test Overpressure method - Hood test As in the vacuum hood test the overpressure hood test is an overall leak test. A test set-up similar to the vacuum test is used. A vacuum chamber is used for the hood, which can be evacuated by a auxiliary pump and to which the leak detector is connected. The helium search gas which is escaping through leaks in the test object is indicated by the leak detector.

The use of a helium leak detector allows detection of extremely small leaks and is suitable for automatic leak detection in industrial equipment. The hood test can for example be used for examination of vessels, heat exchangers etc..

Helium Leak Test, Overpressure Method, Hood test. Overpressure method - Bombing test The bombing test is a pressure/vacuum method of leak detection used for testing of hermetically sealed components containing a cavity which can be gas-filled or evacuated. The objects to be tested, get in a pressure chamber exposed to the helium search gas. During an exposure time of up to several hours at a high helium pressure, the helium will penetrate through any leaks present in the test object. This is the part referred to as the "bombing". After the pressurisation or bombing the objects are tested for helium emission in a vacuum vessel, following the same procedure as in the hood test. This test permits detection of the smallest leak rates and is especially used for objects which can not be gas-filled by other means. The bombing test can for example be used for examination of transistors, ampoules etc..

Helium Leak Test, Overpressure Method, Bombing test. Overpressure method - Sniffer test At this type of test the suspected areas of the test object are carefully explored by means of a detector probe, a "sniffer", which is connected to the leak detector. The object to be tested are under helium search gas overpressure. The sensitivity of the method of the method and the accuracy of localising any leaky points depend on the nature of the search gas, the design of the sniffer and the time constant of the actual leak testing device.

The sniffer test can for example be used for examination of vessels, heat exchangers, seals, flange connections, weld seams etc..

Helium Leak Test, Overpressure Method, Sniffer test. Conclusion To summarise, some of the capabilities of the Helium Leak Test are listed below. o o o o o o o leak rates down to 10-10 mbar l / s can be detected both objects with vacuum or overpressure can be examined the objects can be examined during operation the examination can be performed fast and effective non poisonous, non explosive and inexpensive gasses are applied leaks can be detected in due time to prevent safety or operational hazards leaks can be detected in due time to prevent unplanned and expensive shut downs

Helium Leak Test at 950C

The leak detection methods used in industry and research range from the detection of a dripping valve up to a detectable gas loss of 1 cm over a period of 300 years! This corresponds to a difference in leak rate of about 12 orders of magnitude. Among the known leak detection methods, the leak test with helium as the tracer gas has become the most universal method due to its high sensitivity and versatile application. Stateof-the-art equipment enables the reliable detection of leaks with leak rates in the range of 1 to 10-10 mbar l s1, detection being normally performed at room temperature and a differential pressure of p = 1 bar. In the course of developing a high-temperature solid oxide fuel cell it was necessary to examine components for leak tightness under their later operating conditions of 950 C and only 200 mbar differential pressures. These components included special connectors for later gas supply. The connectors consisted of two concentric metallic tubes. Due to differently selected thermal expansion coefficients, the expansion of the inner tube was greater than that of the encasing tube. This resulted in a sealing effect at high temperatures merely due to this thermally induced contact pressure, which had to be quantified. This was done varying both the gap width and the surface finish. For the experiments, a special vacuum-tight test vessel heatable to 950 C was built to accommodate one test specimen at a time. The vessel was evacuated during the experiments. The test specimens were exposed to helium flowing through thin pipes leading outwards. A differential pressure of exactly 200 mbar was adjustable by means of a special valve cycle and pre-evacuated intermediate vessels. This made it possible to determine the leak rate on red-hot components.

Introduction In the case of a dripping tap it can be seen with the naked eye: it is leaky and liquid penetrates through the leak! However, leaks of this magnitude are not permissible for almost any technical application. As the leaks become smaller, the amount of liquid penetrating through them also decreases. Leakage is stopped when the leak is clogged by large liquid molecules. The leak rate is measured in mbar l s-1. A test object can be regarded as "fluid-tight" below a (helium) leak rate of 10-1 mbar.l s-1. For gases with their smaller atoms, however, leaks of this size are still huge holes whose leak rates are not tolerable in most state-of-the-art applications. Large amounts of gas can still escape even through a leak whose size is only about one millionth of the fluid-tight leak. In the case of a leak rate of 10-8 mbar l s-1 and a pressure difference of p = 1 bar, for example, the gas loss still amounts to 0.3 cm per year. In many cases, however, even these low leak rates are still much too high for special applications. Helium is used as the tracer gas for detecting these small leaks. Helium is nontoxic, does not react with other elements and can even penetrate through the smallest leaks due to its very small atoms. Moreover, helium is only contained in very small quantities (5 ppm) in the ambient air so that air does not substantially disturb the measurement. Efficient helium detectors can detect leaks in a measuring range from about 1 to 10-10 mbar l s-1, i.e. over ten orders of magnitude. Moreover, a helium leak rate of 10 -10 mbar l s-1, for example, only corresponds to a gas loss of about 1 cm in 300 years! However, about 250 million gas atoms per second still flow even through this unimaginably small leak! There are different test arrangements for leak detection. The test specimen is either externally sprayed with helium and the interior evacuated by the leak detector or the test specimen is encased and the interior exposed to helium. In the latter case, the outer encasing is connected to a leak detector. In both cases, the helium escaping through a possible leak is recorded by a special measurement cell (helium mass spectrometer) in the leak detector. The method to be used largely depends on the object to be tested and on the expected information concerning tightness. If the leak is to be localized (= local testing), the test arrangement is different from that required for a statement on the overall tightness of a test specimen (= integral testing). All test variants are normally operated at a pressure difference of p = 1 bar and at room temperature. In special cases, however, it may be necessary to specify the tightness of a component under special operating conditions. This will then require a special test arrangement. Task The Research Centre Jlich is concerned with the development of fuel cells for future energy supply. In a fuel cell, the bound energy of stored hydrogen is directly converted into electric current with the aid of oxygen. Depending on the fuel cell design, this may involve very high operating temperatures. In the course of these developments, the tightness of various components had to be examined under their future operating conditions, i.e. at 950 C and a differential pressure of only 200 mbar. The special test arrangement required for the leak test will be described in the following using an example. The objects to be examined are tube connectors for gas supply in a high-temperature solid oxide fuel cell. These connectors of very simple design (Fig. 1) consist of two steel tubes which can be loosely fitted into one another in the cold state. The inner tube is made of 1.4841 (X 15 CrNiSi 25 20) material with a thermal expansion coefficient of = 19.0 10-6 m/mC and the outer tube of 1.4742 (X CrAl 18) with = 13.5 10-6 m/m C.

When heated, the inner tube expands more than the outer tube due to its greater thermal expansion coefficient. Both parts are thus pressed so tightly onto each other that a sealing effect is achieved. When the fuel cell is placed out of operation, this connection can be very easily disengaged after cooling.

Fig 1: Object to be tested: connector The aim of the investigations was to quantify the leak rate of this pressure connection at high temperatures up to 950 C. For this purpose, both the gap between the two tubes and the surface roughnesses of the tubes were varied. In order to exclude corrosion influences and scaling on the connector surfaces, all tests had to be carried out in vacuum. Experimental Setup The experimental setup is schematically shown in Fig. 2.

1 2a 2b 3 4 5 6

heater vacuum vessel lid specimen, object to be tested thermal insulation cooling for O-ring seal connecting pipe to the specimen

7 8 9 10 11 12 V

two temperature measuring points helium leak detector PC, data acquisition helium storage tank mechanical forepump pressure (vacuum) measuring instrument ...valve

The specimen to be examined (3) is placed on a frame in the vacuum vessel (2a), which stands upright in the heater (1). The heater has a connected electrical power of 5.6 kW. The vacuum vessel made of heatresistant INCONEL can be closed vacuum-tight with a lid (2b). A thermal insulation (4) provided approximately at mid-height in the vacuum vessel reduces the temperature in the region of the lid. Additional water cooling (5) ensures that the permissible operating temperature of the O-ring seal in the lid is not exceeded. The vacuum vessel is connected with the helium leak detector (8). The vacuum is produced by the pumps of the leak detector. The interior of the specimen (3) is connected with a small helium storage tank (10) by two thin ( 2 mm) pipes (6). The pipes (6) and the helium storage tank (10) are evacuated by a small vacuum pump (11) during the heating phase and between the individual measuring points, so that the same pressure of pabs = 0 bar prevails in the vacuum vessel and in the specimen. The interior of the specimen is only exposed to helium when the temperatures are reached at which the leak rate is to be determined. This is the case at 400, 500, 600, 700, 800 and 950 C both during the heating phase and during cooling. In order to determine the leak rate, valves V1 and V3 are closed and the helium storage tank is filled with helium up to an absolute pressure of 200 mbar. Subsequently, valves V2 and V4 are closed and valve V1 is opened. This ensures a 100 % helium concentration in the specimen. In the absence of any major untightness, a differential pressure of p = 200 mbar is established between specimen and vacuum vessel during the measurement. The helium penetrating through the sealing gap on the specimen flows to the helium leak detector (8) where it is recorded as the integral leak rate. Fig. 3 shows a photograph of the experimental setup. On the left you can see the heater with built-in vacuum vessel. The LEYBOLD UL 100-plus helium leak detector can be seen in the centre on the right.

Results Since this report concentrates on the special testing technique applied here, the result of one test series will only be presented as an example in the following. Fig. 4 shows the leak rate curves for four different specimens at different temperatures during one heating and one cooling cycle. As was to be expected, the leak rate decreases with rising temperature, i.e. with increasing pressure per unit area in the sealing gap. Helium leak rates in the range from 10-2 to 10-3 mbar l s-1 were measured at 900 to 950 C. The different leak rates of the specimens are attributable to different gap widths and surface roughnesses. The measured leak rates are composed of the gas loss (leak rate) in the sealing gap of the specimen (3) and of the helium permeation through the material walls. Permeation takes place through the walls of the two connecting pipes (6) leading from the specimen through the lid (2b) of the vacuum vessel (2a) outwards as well as through the walls of the specimen (3).

A test was carried out to determine the leak rate through the connecting pipes (6) to the specimen, which will not exist in the actual fuel cell. For this purpose, the connecting pipes were built into the test vessel without a specimen, heated and then exposed to helium from the inside. However, no helium leak rate due to permeation significantly influencing the results was measured even at 950 C for a prolonged test time of approx. two hours. Conclusion A special experimental setup has been conceived to investigate the leak tightness of tube connectors for gas supply at high-temperature solid oxide fuel cells. In this way, it was possible to carry out a helium leak test under future operating conditions, i.e. at 950 C and a differential pressure of 200 mbar. The measurements revealed leak rates in the range from 10-2 to 10-3 mbar l s-1 at 950 C. The leak rate can be further optimized by varying the gap and surface finish. Helium permeation through material walls does not play any significant role. The tests have shown that the connectors are suitable for use at 950 C.