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Phase Change Indicators for Subambient Temperatures

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Phase Change Indicators for Subambient Temperatures II NASA CONTRACTOR REPORT 40 h ,-. ..../_,.,_..,.. - . ;:" ;'; _...,: -I e U PHASE CHANGE INDICATORS FOR SUBAMBIENT TEMPERATURES by D. R. Kasanof and E. Kimmel Prepared by i TEMPILO CORPORATION New York, N. Y. for LatzgZey Research Center NATIONALAERONAUTICS AND SPACE ADMINISTRATION WASHINGTON, D. C. MARCH 1970 ._ TECH LIBRARY KAFB, NM 00b0899 c-w, J NASA CR-1576 /PHASE CHANGE INDICATORS FOR SUBAMBIENT TEMPERATURES bL&~Q- By D. R. Kasanof and E. Kimmel Distribution of this report is provided in the interest of informationexchange. Responsibility for thecontents resides in the author or organization that prepared it. \ p- ' '\.prepared under ContractNO. L/.@&J31.-566by Luc.g9 "-.._--. TEMPILO CORPORATION New York, N.Y. for Langley Research Center NATIONAL AERONAUTICS AND SPACE ADMINISTRATION For sale by the Clearinghouse for Federal Scientific ond Technical Information Springfield,Virginia 22151 - CFSTI price $3.00 PHASE CIIANGE INDICATORS FOR SUBAMBIENTTEMPERATURES By D. R. Kasanof and E. Kinnnel TEMPIL" CORPORATION Forty candidate organic compounds were evaluated as possible fusible temperature indicators for use in the range -50°F to -150°F. Of these, thirty with melting points ranging from -37°F to -162°F were found to be useful as temperature indicators. Nine candidates were rejected because they did not yield opaque, crystalline coatings by any of the application procedures attempted. One candidate material was rejected because it proved to be unstable. Phase studies of several binary systems were also carried out. A number of application procedures were evaluated. An aerosol-spray procedure was adopted because it consistently yielded opaque coatings, was relatively simple to employ and could probably be adapted for use in the Langley Field test apparatus. The indicators were foundto signal properly at a reduced pressure of 2mmercury, as well as at sea-level barometric pressure. INTRODUCTION In the July 1964 issue of the Journal of the American Institute of Aeronautics and Astronautics, Messrs. RobertA. Jones and JamesL. Hunt of the NASA Langley Research Center published a paper captionedof "Use Temperature-Sensitive Coatings for Obtaining Quantitative Aerodynamic Heat Trans fer Data". This paper described the use of Tempilaq" phase-change temperature indicators for obtaining accurate heat-transfer data on models of complex shape in wind'tunnel tests. All of the work described was carried out using temperature indicators having ratings above 100"F, the lowest temperature for which these materials are commercially available. In a letter of March 4, 1965 Tempil" Corporation proposed to under- take the development of phase-change indicators which could be used to extend this technique to temperatures well below the normal climatic range. NASA Contract NAS1-5667, dated December 9, 1965, authorized an investigation to develop materials and corresponding application techniques that couldbe used as phase changetemperature indicators in the temperaturerange of -50°F to -150"F, andwould be suitable for aero- dynamic heat transfer testing by the method described in the Jones and Hunt paperreferred to above. The indicators wouldbe used at environ- mental pressures ranging from 2mm Hg to oneatmosphere. The following desired characteristics of the indicators wereoutlined in the contract to serve as developmentguidelines: a.me phase change of theindicators should be clearly visible so that it canbe recorded with black and white film. b. The indicatingtemperature should be unaffected by ambient pressures from 2mm Hg to oneatmosphere. c. The indicatingcoating should have a veryshort response time so thatthe phase change temperature will beunaffected by the heating rate. d. The method forapplying the indicator should besuch that repeatability of results canbe obtained. e. The indicatorsshould have a low order of toxicity and shouldbe chemically inert. LITERATURE EXPLORATION - The targetproperties -- meltingpoint range, low vaporpressure, long-term stability, inertness andlow order of toxicity -- appearto have fairly well restricted the chemical compounds availableas candidate temperature indicators. Examination of the literaturerevealed that two classes oforganic compounds, esters and aromatichydrocarbons, offered the most promising, readily available candidates. Our own experiencewith esters at elevated temperatures (over 100°F) led us tobelieve that this class of compounds mightalso havethe necessary crystallization properties, i.e., little or no tendencyto supercool below the freezing point and a strongtendency to formopaque, clearly visible crystals -- asopposed tothe formation of glasses which would be undesirable. Aromaticethers, cyclic aliphatic ketones and aliphaticalcohols were otherclasses of organic compounds which offeredseveral additional candidate materials. SOURCE OF CANDIDATE MATERIALS - All candidatesfor fusible temperature indicators actually used in -this work project were the best grades available from Distillation Products Industries, Eastman OrganicChemicals Department, Rochester, N.Y. 14603. All are listed inthe current D.P.I. catalog, and were evaluated without further purification or treatment. LOW-TEMPERATURETEST CHAMBER - The test chamberused throughout this work program was aneight cubic foot (2' x 2' x 2') capacity Model WF-8-175V 2 ~ " Low Temperature Environmental Chamber manufactured by the Webber Manufac- turing Company, Inc.,Indianapolis, Indiana. Air in this chamber was circulated by a fan and air temperatures were adjustable fromambient to -175°F. Provisions were availablefor evacuat- ingthe chamber topressures of less than 2mHg. On eachof the two sides of the chamber was a 2-inchservice port through which electrical leads, tubesor probes could be introduced. The side-hinged,overlapping door on the front of the chamber was supplied with two 6-inchport holes for glove and/or hand insertion and manipulation of articles within the chamber underatmospheric pressure conditions. These ports were flanged and could be sealed if the chamber was tobe evacuated. The door was alsoequipped with a 12'' x 12" observa- tion window consisting of a special hermetically sealed 6-panethermal glass assembly. SCREENINGOF CANDIDATE MATERIALS - Initialattempts to evaluate candidate materials involvedobservation of small quantities of liquid in glass test tubes and incapillaries. This method was found unsatisfactorybecause it was difficult to observe changes of state whichmight have taken place and becausethe length of time necessaryfor the relatively large quantities of liquid to reach thermal equilibrium with the air was found to be excessively long. After some experimentation,the following procedure was adopted and used in the initial screening of mostof the candidate materials: A dropor two of fluid was placed in the center of a 75x25mm glassmicro- scope slide and coveredwith an 18mm coverslide, thus sandwiching a thin layer of material between glasssurfaces. This glass sandwich was then placed on awooden rack inan almost vertical position. The rack was paintedblack to form a darkbackground. Illumination was provided by four 73 watt bulbs, two on eachside of therack. The chamber was thencooled until crystallization of thecandidate occured or until a temperature of -175°F was reached. Using this set-up, results were easilyobserved andphase-changes from liquid to solid, when accompanied by the formation of opaque white crystals, was verydramatic against the black background. The abovemethod was relatively simple and enabled us to evaluate several samples at once. Results obtained were thought to correlate well withthose which would be obtained under the anticipated end-use conditions. AEROSOLAPPLICATION OF INDICATOR MATERIALS - The followingaerosol application method was developed as a consequenceof our search for a final form for the temperature indicators and correspondingpractical method for applying them. It was usedprincipally for the final temperature calibra- tion of the indicators, although it would alsohave been an excellent means 3 for initially evaluating the crystallization properties of eachmaterial -- the evaluation carried out on almost all of thecandidates by themicro- scope-slide method described in the previous section. In employing this procedure, the substrate was cooledto a temperature below themelting point of theindicator. In the case of readilycrystallized materials,cooling the substrate to approximately thirty degrees Fahrenheit below themelting point of theindicator was sufficient.In other cases, coolingwith liquid nitrogen to temperatures approaching -300'F was found necessary. A six-ounceaerosol container containing 60 gramsof theindicator liquid and 75 gramsof Freon 12 propellant -- no solvent -- was then inserted into the test chamber through oneof theport holes anda spray was directedonto the cooled test piece from a distance of six to eight inches. The aerosolcontainers were stored under ambient conditions prior touse, but apparently cooling of the indicator particles by evaporation of theFreon 12, by passagethrough the cold atmosphere of the chamber,and, finally, by contact with the cold substrate was sufficient to yield a white, opaque,adherant, solid coating several thousandths ofan inch thick. All applications of indicatorcoatings by this methodwere carried outunder atmospheric pressure conditions. When calibrations were to be carried out in avacuum, application was followed by sealing of the chamber and evacuation. UNSUCCESSFUL APPLICATION FORMS AND PROCEDURES Suspensionsof materials
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