On the Emissivity of Silver Coated Panels, Effect of Long Term Stability and Effect of Coating Thickness

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1 JET P(98)57 P A eladarakis W Obert On the Emissivity of Silver Coated Panels, Effect of Long Term Stability and Effect of Coating Thickness

2 This document is intended for publication in the open literature. It is made available on the understanding that it may not be further circulated and extracts may not be published prior to publication of the original, without the consent of the Publications Officer, JET Joint Undertaking, Abingdon, Oxon, OX14 3EA, UK. Enquiries about Copyright and reproduction should be addressed to the Publications Officer, JET Joint Undertaking, Abingdon, Oxon, OX14 3EA.

3 JET P(98)57 On the Emissivity of Silver Coated Panels, Effect of Long Term Stability and Effect of Coating Thickness P A eladarakis, W Obert. JET Joint Undertaking, Abingdon, Oxfordshire, OX14 3EA, Preprint of a Paper to be submitted for publication in Proceedings of Inter. Cryogenics Eng. Conference. January 1999

4 ABSTRACT Silver plated panels have been extensively used for the LHe surfaces of JET s largest cryopumps for more than 15 years now. ITER, the next-generation fusion device, also favours silver plated shields for its cryostat and vacuum vessel. This paper is concerned with the effect of ageing, coating thickness, temperature, moisture and corrosion on the emissivity of silver coated stainless steel samples, as a measure of optimisation for both performance and cost issues. 1 INTRODUCTION JET has long experience with the high reliability and efficiency of silver coated aluminium substrates, used for the LHe panels of the Neutral Beam (NB) Cryopumps, (40 m 2 surface area, 8*10 6 l/s pumping speed). Silver coated stainless steel is currently the choice for the thermal shields of various components at ITER, the next-step fusion device, which is being designed under an international collaboration among Europe, USA, Russia and Japan. The relatively large size of ITER means that the surface of its radiation shields exceeds many hundreds of m 2. Longterm stability, coating thickness, corrosion resistance, etc., become extremely important factors on account of the large area. Their effect on the emissivity, a critical property strongly associated with the performance and efficiency of any cryogenic shield, has been the focus of this work. The emissivity of both aluminium [1] and stainless steel substrates was measured. However, this paper reports mainly on the results of the latter type of material, in view of its future use for ITER. Twenty stainless steel rectangular samples, 100 x 60 x 3 mm, have been silver plated at a variable coating thickness, ranging from 500è to 60 µm, by an electrolytic process. One µm of Woods-Ni was normally used as the bonding interlayer between the substrate and the silver deposit. It was important therefore to examine any possible effect of the interlayer on the emissivity of substrates with relatively low silver coating thickness (< 3µm), since the latter might be transparent to incident thermal radiation. Two samples (21, 22) were deposited with solely 6µm Woods-Ni. The final coating thickness was measured by an X-Ray Fluorescence technique at the Prodec - Metal Ltd, France. The results are shown in Table 1. Table 1 Non-aged SS Samples (X-ray fluorescence measurements) Sample Number Coating Type Non Non Coat. thick. (µm) N/A N/A 0,010 0,010 0,050 0,0500 0,500 0,500 1,000 1,000 3,000 Measured Thick. (µm) N/A N/A 0,235 0,228 0,261 0,257 0,572 0,613 0,985 1,043 3,222 Sample Number Coating Type Wood-Ni Wood-Ni Coat. thick. (µm) 3,000 6,000 6,000 10,000 10,000 20,000 20,000 50,000 50,000 6,000 6,000 Measured Thick. (µm) 3,048 7,588 7,335 10,36 10,65 20,34 20,28 60,62 59,38 6,071 6,220 JG98.425/8c 1

5 A second set of 4 stainless steel samples with 25 µm silver coating, stored in JET for more than 15 years, was also included in the measurements in order to examine the long term stability of the coating. 2 EMISSIVITY INSTRUMENT The emissivity of the samples was determined by an optical measurement, based on the diffuse infrared reflection capacity of (flat) objects or coatings, using a portable Dornier - Selectometer appliance, [2]. The appliance comprises an infrared radiation thermometer (Heinmann model 15.99) covering a spectral range of 0.6 to 40 µm, and a black radiator. The object to be measured is placed next to a concave opening of the radiator at a specified distance. The object reflects back part of the thermal radiation emitted from the relatively hot radiator, kept constantly at 100 C by a control/power supply unit. The emitted and reflected radiation is measured by the infrared thermometer which displays an output, in mv, at a response time of 1 s. The emissivity is then evaluated by linear regression using reference points obtained during calibration. The instrument is calibrated before each series of measurements, by means of two objects with known emissivities, namely a black varnished hollow cylinder (ε = 94.05%) and a reflective gold sample (ε = %). An additional reflective object (infragold) with a calibrated hemispherical spectral emissivity factor of 0.38 was used for calibration to increase the measurement accuracy at low emissivity values. 3 MEASUREMENTS AT AMBIENT TEMPERATURE The results of the measurements at room temperature are given in Figure 1. The emissivity is practically lower than 1% for substrates with a silver coating thicker than 3 µm. The lowest value (ε = 0.34%) was found on samples 15 & 16 where the silver deposition is 10 µm thick. The effect of the silver coating on the emittance can be evaluated easily by comparing samples with no coating, (i.e. just plain substrates e.g. samples 1, 2), with samples comprising relatively thin silver layers (e.g. samples 3,4 with ~0.23 µm silver coating). It can be seen (Fig. 1) that even a layer of ~0.23 µm of silver reduces the emissivity by, almost a factor of three, from ~14.22 % to ~5.16%. If thicker silver coatings Measurment 1 Measurment 2 are considered, then the emissivity decreases Measurment 3 by a factor of 15 (for coatings thicker that 3µm) Non coated samples or even 40 (e.g. sample 15). The results from samples 21, 22 which were deposited with only a (6µm) Woods-Ni Ni-wood coating layer are also shown in Fig. 1. Their emissivity ed samples (8.12 %) is 63%, higher than the value of the thinner silver plated sample, suggesting that the Coating thickness (µm) Fig. 1. Room Temperature Tests of & Ni plated samples as well as aged coating on the latter is not totally transparent ones. Emissivity (%) JG98.425/3c 2

6 to incident radiation flux. The range of emissivity is complimented by the measurement of two black objects, namely Larin Copper and Larin Aluminium, which showed an average emissivity value of ~ 83.72%. In an attempt to quantify the ageing effect, aluminium and stainless steel silver plated substrates, stored at JET for more than 15 years, have also been measured [1]. The tests of the latter type of samples, which comprise a 25 µm silver layer, showed emissivities of ε < 0.58%, i.e., lower than their non-aged counterparts. 4. MEASUREMENTS AT LN 2 TEMPERATURE The ITER thermal shields will operate at ~ 80K, being cooled by gaseous helium. Therefore, it was important to examine the effect of temperature on the emissivity. LN 2 was used to cool the specimens down to ~77K. A controlled (dry and oxygen free) atmosphere was required for the performance of LN 2 measurements since, moisture and oxygen would have been condensed immediately on the sample cold surfaces, increasing dramatically their emissivity, as it will be shown later. A plastic glove-box was designed and constructed at JET for this purpose (Fig. 2), comprising a feed pipe, two ports for the handling of a LN 2 portable dewar, the samples and the emissivity appliances, a hand relief valve on top, two glove-tubes and a feedthrough for the instrument cables. The inlet pipe was connected via two pressure regulating hand valves to the dry gaseous nitrogen feed of the JET cryoplant. The tent was initially vented with dry N 2 to remove the enclosed air volume, and thereafter kept under pressure by shutting first the relief valve and then the supply valve. Each sample was submerged in LN 2 until thermal equilibrium 1000 Emissivity measurements at 77K Emissivity (%) Black samples at 77K Black samples at 300K Non coated samples Ni-wood coating 1 Test 1 (non-corroded) Test 2 (non-corroded) Test 1 (corroded) Test 2 (corroded) ed samples Coating thickness (µm) JG98.425/4c Fig. 2. The test apparatus used for the emissivity tests at LN temperature Fig. 3. LN tests of & Ni plated samples, including; aged, corroded & non-corroded samples 3

7 was achieved. The boil off during the cooling process pressurised further the tent preventing any air ingress. The pressure at this stage was regulated by the relief valve. The cold sample was removed from the dewar and its emissivity was immediately measured by the instrument, placed inside the tent, at virtually 77K. The results of these measurements are shown in Fig. 3. It can be seen that the emissivity has increased by a factor of 1.6, in average, as compared to the results at room temperature (Fig. 3). Although the difference is not significant, one might have expected a decrease in the emissivity instead, as e.g. in [2],[3] (although the decrease is more pronounced at 4K). The emissivity increase shown in Fig.3 might be attributed to the formation of a very thin layer of frost detected on the samples shortly after they were measured, suggesting possible air inleaks in the tent. Once more, the lower emissivity values (ε < 2%) were encountered for samples with a silver coating thicker than 3µm. This is still significantly lower (by a factor of 12.5) than the emissivity of plain stainless steel plate. The aged JET samples show remarkably lower emissivities ( 0.54%) compared with their non-aged counterparts (ε 2 %) proving once more the reliable long term stability of the coating. On the other side of the range, the two black samples acquired an emissivity of almost unity at LN 2 temperature. The effect of the controlled atmosphere 1000 on the emittance behaviour is shown in Fig Samples have been submerged in LN 2 and exposed to air for up to 30 min, while their emis sivity was measured at intervals. The frost layer formed on all sample surfaces resulted in a dramatic increase of their emissivity, to an average value of 16.5%, 7 times higher than the 10 values of Figs, 1 & 3, after 1.5 min of exposure. Since the coating thickness was not im Time (min) portant here, five samples (7, 10, 15, 18, 20 ) Fig 4. Emissivity of silver plated SS samples vs exposure time at air from 77K have been monitored up to ~30 min, at which point their emissivity started to decrease again (Fig. 4). Another test employed to demonstrate the effect of moisture was the measurement of wetted samples, after being dipped into water at room temperature. The emissivity once again increased to an average value of 6 %, independent of the coating thickness, with the actual value depending upon the surface condition and its capacity to retain a liquid water film (i.e. the aged samples with apparent sulphide layers showed higher retention, although temporarily). Emissivity (%) JG98.425/6c 4

8 5 EFFECT OF CORROSION ON SILVER SURFACES It is a well known factor that silver is prone to corrosion from sulphide compounds. In fact, all silver surfaces contain a native sulphide layer of 20nm. To examine the effect of corrosion on the emissivity, 11 out of 22 SS silver coated samples were exposed to dry, pure H 2 S gas for 5 hrs and the rest for 50 hrs. The tests were performed at 40 o C, since no significant surface discoloration was detected after an exposure of 45 hrs at room temperature. Even this severe corrosive environment did not produce black samples. The emissivity of all corroded samples was measured at room and LN 2 temperatures. It was found that the samples retained a relatively low emissivity even after the exposure (ε lower than 1.73% or 1% for samples with a coating thicker than 3µm or 6 µm respectively, at room temperature). The emissivity of the corroded samples was 34% and 33% higher on average than their emissivity values prior to exposure. The results of the LN 2 tests are shown in Fig.3 6 CONCLUSIONS The minimum silver coating thickness which can ensure the lowest emissivity values is found to be 3µm. The emissivity of stainless steel substrates is lower than 1% for silver coatings thicker than 3µm, at room temperature. At LN 2 temperatures the emissivity was found to be ε < 2% again for samples with silver coating thicker than 3µm. The results though showed an average increase of 33% as compared to room temperature results, attributed perhaps to minute air inleaks in the test apparatus. ed (more than 15 years) 25µm plated samples show remarkably low emissivity (ε < 1%), demonstrating a long term stability of the coating. Stainless steel samples retain relatively low emissivity even after exposure to H 2 S vapours for up to 50 hrs at 40 o C. The emissivity is increased by 37% or 34% compared to the values of un-corroded samples at room and liquid nitrogen temperature respectively. 7. REFERENCES [1] P. A. eladarakis & W. Obert: Long Term Effects on the Emissivity of Silver Plated Panels, JET-IR(97)09. [2] G Perinic et al: A portable Instrument for Measuring Emissivities, Advances In Cryog. Eng., Vol 41, New York, 1996, pp [3] W Obert et al: Emissivity Measurements of Metallic Surfaces used in Cryogenic Applications, Advances In Cryogenic Engineering, Vol 27, San Diego, 1981, pp [4] K H Hawks & W Cottingham: Total Normal Emittances of Some Real Surfaces at Cryogenic Temperatures, Advances In Cryogenic Engineering, Vol 16, 1970, pp

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