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Advances in Materials. Proceedings of a Symposium Organised by the North Western Branch of the Institution of Chemical Engineers Held at Manchester, 6–9 April, 1964 PDF

251 Pages·1966·21.149 MB·English
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Preview Advances in Materials. Proceedings of a Symposium Organised by the North Western Branch of the Institution of Chemical Engineers Held at Manchester, 6–9 April, 1964

ORGANISING COMMITTEE Mr. L. Holliday, M.A., B.Sc., F.R.I.C., C.Eng., M.I. Chem.E. Mr. B. F. Street, B.Sc., C. Eng., A.M.I. Chem.E. Dr. P. E. Evans, M.A., Ph.D. Mr. J. M. Hutcheon, B.Sc, A.R.I.C. Mr. M. Shaw, B.Sc, D.L.C., A.R.I.C, C.Eng., A.M.I. Chem.E. Honorary Editor of these Proceedings Mr. P. A. Rottenburg, M.A., C.Eng., A.M.I.Chem.E. ADVANCES IN MATERIALS Proceedings of a Symposium organised by the North Western Branch of the The Institution of Chemical Engineers held at Manchester, 6-9 April, 1964 Published for THE INSTITUTION OF CHEMICAL ENGINEERS by PERGAMON PRESS OXFORD · LONDON · EDINBURGH · NEW YORK TORONTO · PARIS · FRANKFURT Pergamon Press Ltd., Headington Hill Hall, Oxford 4 & 5 Fitzroy Square, London W.l Pergamon Press (Scotland) Ltd., 2 & 3 Teviot Place, Edinburgh 1 Pergamon Press Inc., 44-01 21st St., Long Island City, New York 11101 Pergamon of Canada Ltd., 6 Adelaide Street East, Toronto, Ontario Pergamon Press, S.A.R.L., 24 rue des Ecoles, Paris 5e Friedr. Vieweg & Sohn Verlag, Postfach 185, 33 Braunschweig, West Germany The Institution of Chemical Engineers, 16 Belgrave Square, London S.W.i © 1966 This compilation of articles PERGAMON PRESS LTD. Papers are reproduced by the authority of the individual authors, but copyright is not vested in The Institution of Chemical Engineers. First edition 1966 Library of Congress Catalog Card No. 65-26566 PRINTED IN GREAT BRITAIN BY C. F. HODGSON & SON, LTD. (2374/66) PREFACE THE symposium on "Advances in Materials" was held in the Renold Building, Manchester College of Science and Technology, Altrincham Street, Manchester 1. The organisers and hosts were the North Western Branch of The Institution of Chemical Engineers. The object of the symposium was to survey the latest developments in materials science and technology. The limitations imposed by mater­ ials on the progress of modern technology were examined, together with developments to meet the increasingly exacting requirements of industry. The meeting considered the subject on a broad front and was not re­ stricted to chemical engineering. CHALLENGES TO MATERIALS SCIENCE IN THE CHEMICAL INDUSTRY: INDUSTRIAL NEEDS AND AN INFLUENCE ON DESIGN By C. EDELEANU, M.A., Ph.D.* SYNOPSIS During recent years very much effort has been devoted to studies of materials largely as a result of defence requirements. Progress has been extremely fast in certain fields, and perhaps the largest current problem is the assimilation of new information. In a new project there are three district stages at which questions of materials arise. The earliest stage is that represented by laboratory work. At this stage various process possibilities may be discounted as liable to present insurmountable materials difficulties. Frequently these decisions are made almost subconsciously and tend to reduce both the challenge to the materials specialist and the scope of the project. The next stage is the preparation of the flowsheet when the physical shape of the plant is visualized. During this stage materials " problems " can be avoided but it is equally easy to miss opportunities which progress in materials have made possible. The final and most common stage at which materials are considered is the detail or functional stage of design. By this time practically all the major decisions have already been made, but clear thinking on materials is still important. Attention to detail will make all the difference between a plant which works satisfactorily and one which gives a great deal of trouble during start-up. Frequently this is the only stage at which materials are considered seriously because it is the only one during which the result of not doing so is obvious. Introduction Not so obvious, time is of the utmost importance not only because of the cost of idle capital which is very high if con­ Not all of us who are interested in materials are motivated struction is slow but because, in a competitive world, being by the same things, but the final expression of our work is a ready just at the right time may make all the difference between piece of hardware. Expressing ourselves through the winning or losing a market. Being late, after having sold the designers involves establishing understanding and this presents product of a yet unfinished plant, can be a disaster. These some of the most challenging problems which have to be are among the things which have to be considered by anyone solved if anything is to happen. Important as the designer expecting to have his recommendations taken seriously. may be to us there are others who are more directly involved The problem is one of communication and it is worth in creating the ever-pressing technical challenge in the field considering some of the difficulties which are found in of materials. The purpose of this paper is to examine just practice. Two types of people are involved in the exercise: how problems arise and how we can resolve them so that our the engineers and the materials specialist are the technical work is eventually used rather than to dwell on actual present parties while the buyer and salesman are concerned with the problems. Naturally many people in the materials field are commercial aspects of the negotiations. Roughly the techni­ not greatly concerned with practical issues and, to some, the cal people decide what is to be bought whilst the commercial study of materials and their properties is an end itself. No people decide how it is bought. Difficulties arise when either one must underestimate the contribution made by such people, the buyer or the salesman does not know what is being but when they feel let down by the practical people who are bought, and unfortunately this is not unknown. Perhaps the slow to " appreciate " and use their work they might like to task is made even more difficult when the materials expert has know some of the difficulties involved. If they then still feel no idea of the commercial implications of his recommendations strongly perhaps they might even consider giving a helping and has no appreciation of the engineer's problems. Equally hand to the rest of us, but not necessarily at the expense of frustrating is the situation when the engineer is so engrossed their own task.The presentation of their work in a suitable in his own problems that he does not stop to think just what " language " would help a great deal. are his problems, and asks for answers to meaningless questions. In practice, difficulties arise just as frequently because of the shortcomings of the technical people as those of their commercial colleagues. The matter is even further Final Selection of a Material complicated when for either good or bad reasons secrecy on The critical step in the selection of a material is an engin­ either commercial or technical matters is involved. eering decision and it is important to realize what is involved It is perhaps worth illustrating the problem with a few in it. Basically this is a marriage between the technicalities examples. New materials and some which are not at all and economics, and both words are used in the broadest new are sold under trade names and there are no national possible sense. The economic decision does, of course, take specifications, standards, etc. The technical information is account of capital costs but this is only one of the many available in trade publications and, as often as not, gives factors such as process and maintenance costs, probable " typical " properties, and is very uninformative about market fluctuation, transport, storage and other such costs. actual minimum properties. Recommendations on design stress or on similarly useful matters are not given and even * Imperial Chemical Industries Ltd., Billingham. greater coyness is displayed on costs, availability or anything 3 4 EDELEANU. CHALLENGES TO MATERIALS SCIENCE else that may help anyone to decide whether it is even worth system operating at say 900°C which would be highly shortlisting the material. All this is done presumably for economic. It could well be that he would get no further since good commercial reasons and the relevant information can the consequential container problem might label the whole eventually be extracted, normally after spending time first with idea as unrealistic. This is a case which actually arose at a commercial man who cannot help with the technical side but Billingham a few years ago but fortunately the project was not agrees to send along his technical people who are then floored killed even though it was fully appreciated that the conventional by any questions of price, delivery, etc. Commercial contact power industry was having difficulties in going even to 650°C. is then made again in the form of a firm enquiry and as sure Chances had to be taken, but in a matter of some three years as fate the preliminary information on cost, delivery, etc., is the first pressure steam reforming plant for light distillate was utterly wrong, and if it is not, it turns out that say Grade B on line, and now some two years later there are at least 33 strongly recommended by the technical man as slightly such plants on line or in various states of completion. superior and worth having every time is twice the price of Assuming that an idea is not killed from the start, and Grade A, or it is an experimental grade which is on a year's laboratory work proceeds, various decisions on materials are delivery. Naturally there are alternatives to this but it is no made again sometimes almost subconsciously during the wonder that a project engineer faced with numerous routine research. For instance, everyone knows that hydrochloric materials decisions, possibly hundreds, and with a year to acid is a difficult acid and no matter what other merits it has complete detailed design, clear a site and erect a plant will it could well be excluded in an investigation simply on this not be delighted to consider what he thinks, and rightly so basis. It may also be that artificial limits on pressure, under the circumstances, are crackpot ideas. The meals that temperature or other such factors may be imposed just in have to be consumed in order to arrive at an understanding are order to avoid potential materials problems. Naturally this in themselves a reason to avoid novelty. In most projects may be justified and certainly it will reduce the eventual there are only one, two, or at the most three really important demands on materials, but it is also likely to reduce the novel decisions to make, but even so the work which has to be chances of a really spectacular new project. The nitric acid done in connection with the remainder does tend to make life process universally used now is a good example, also from difficult. Billingham, of a process which would not have seen the light The most valuable contribution a materials man working of day when it did had it not occurred to someone at the time for a supplier can make is to be sure that the trade literature that there was what then was a novel material—stainless steel means something and fulfils a purpose. This exercise will —and that it was not merely a laboratory curiosity and that teach him a few lessons and he must not forget that it is no it could be considered seriously for a major engineering use him recommending, which is the polite word for selling, a construction. The realization, of course, not only caused material on the basis of its physical or chemical properties progress in chemical engineering, but brought forward the if he ignores the price (which includes delivery, fabrication, development of the stainless steel industry which in turn etc.) and which is also a property. Furthermore, when he transformed chemical engineering. selects topics for development or research work and looks at The second stage in the project comes when the laboratory the various properties of materials he must look realistically work has been finished and it has been established that some­ at the one universally important property which is cost to the thing can be done. During this stage it is necessary to buyer. This property is at least as complicated as any others decide exactly what shall be done and finish up with a flow­ the material has and it is sometimes governed by what at first sheet. This stage is very similar for a really new or for an appear completely illogical laws. The relationship with only slightly modified process, and again a variety of decisions production costs is sometimes statistically non-existent, and are made which, consciously or subconsciously, involve whilst sometimes there are good commercial reasons for this assumptions about materials. For instance, important there are situations in which a good product which may cost factors are the size of plant, the operating pressures, tempera­ the same or even less to manufacture than a bad one does not tures, compositions of various streams, etc., and the limits require extra manufacturing capital or cause any other in­ are imposed by what are commonly called engineering factors. convenience is priced out. It may not be the recognized A typical such limit may be the size of the pressure vessel, but function of a materials man to concern himself with prices is this really a true engineering limitation ? The basic physics but it is the thesis of this paper that he should, and it is of a pressure vessel are not affected appreciably by size, and if suggested that he will find at least as much challenge in there are limits to the size of pressure vessels these are imposed investigating the interesting laws governing accountants and by metallurgical factors such as the metallurgy of thick plates, bodies such as the Iron and Steel Board as the physical laws on being able to weld and inspect the vessel, and other factors of nature. which are in the materials field. Naturally there are also Price as stated above means price of the final item, and this practical matters such as the transport of the vessel to a in turn involves a knowledge of methods of construction and particular site which may impose limits, but the metallurgist their costs. It is no use for instance specifying a PTFE lining can overcome sometimes even these by allowing site welding. and stating the price of PTFE without also considering whether By the time this second stage is reached generally time is and how such a construction can be made and the final cost. becoming short, and unless the necessary homework was done during the first stage, conventional materials and modes of construction are the order of the day. Savings, even if considerable, which might be possible by adopting completely Stages in a Project at which Material Decisions are Taken novel methods have become less attractive especially since it Thinking in terms of a chemical project it is possible to has already been established that the exercise as a whole is divide the decisions made on materials into three stages. economically rewarding and there is already a " bird in the Initially there is a stage during which an idea is conceived and hand ". laboratory work on the chemistry of the various reactions is Finally, when it has been established what shall be done, done. During this stage a great many materials decisions can design starts which involves decisions on how it is to be done. be made, either consciously or subconsciously. Indeed even By now things are moving at all possible speed, capital has before laboratory work is sanctioned the matter of materials been committed and every single day may cost £1000 or more may influence the project. To give an example, a chemist depending on the size of the project. The project has may say that he can visualize a process involving a pressure splintered into various design tasks and many designers are EDELEANU. CHALLENGES TO MATERIALS SCIENCE 5 involved. It is perhaps regrettable, but by far the greatest well known to the engineer and easy to use since there are number of decisions on materials have to be taken during this many codes, national specifications, standards, etc., and a stage. Even if the major decisions have been taken, there are well-organized and established engineering industry to back numerous minor ones and these involve, amongst other them up. Strangely these are also their handicaps because things, the laying down of detailed specifications, establish­ many of the standards and established engineering practices ment of standards, instruction on welding, inspection, and the are out of date and greatly restrictive. For instance, unforeseen difficulties which crop up during detail design. B.S. 1500 lays down that pressure vessels must be designed to The odd joint, gland, inspection point or delay in delivery a quarter of the U.T.S.—a standard laid down countless years of a preferred material are typical details which all cause ago which admittedly is being revised, but only after it has hold-ups, and equally important, if not considered adequately, been shown by many years experience in Germany that much endless start-up troubles. At this stage, like at all others, higher stresses are safe in practice. There are countless other decisions must be correct, but one thing is never permitted examples—to quote one other it is traditional to use forged now and that is to take time to make them. These two steel for critical items, but why ? The economics of the steam requirements may appear contradictory but in practice they reforming process already mentioned were greatly affected by frequently are not and the way out may be to do something using centrispun tubes of high alloy steel at roughly a third the which appears quite stupid economically or clumsy from a cost of the extruded tubes, and on a six-week delivery instead design point of view but which is bound to work. When it of one year. As it happens they have also proved technically has worked unfortunately it then becomes established and the better, but in order to obtain these advantages one has to fight mistakes, because this is what these compromises are, are then tradition. Those who feel safe that they have a good quality repeated when new plants are built. product unlikely to be replaceable by others may be fortunate, To sum up, the really big challenge arises at the conception but are more likely to be mistaken, and they have to consider of a novel idea for a process. There is then freedom of exactly what the customer buys and not assume that this is action and time. Unfortunately decisions at that stage are the same thing as the manufacturing description. A manu­ often made subconsciously and even at the next stage, the facturer may think he is selling forgings but in fact the flowsheet stage, when worthwhile things can still be done, it is customer buys vessels, tubes, etc., and provided they are not always appreciated just where materials stand. The final technically sound he does not care if they are knitted. An stage is a race against time, the decisions are still important example is provided by the railways which would not be in because they make all the difference between a plant with or trouble now if from the start they had realized they were in the without start-up difficulties. That engineering is applied transport business and not in the railway business. material science amongst other things is appreciated at this Many of the people in the traditional metal industry would stage especially when things go wrong, but it is too late to do do well to spend more effort on the deadly boring subject of anything really big. codes, standards, etc. If they feel that, as highly trained people, it would be a waste of time to do so, they have to remember that ultimately the man at the drawing board can only make use of developments when these have been in­ Present Challenging Problems corporated in such codes or at least in trade publications. This is a most difficult topic and each person is bound to be Papers in the various metallurgical journals are no use at all for influenced by his immediate experience. As I see it, the most this particular purpose and there are obvious disadvantages in interesting feature at present is the hotting up of the com­ sending the second fifteen to B.S. committees. petition between metallic and non-metallic materials, and this Technically it is hardly worth saying that most of the is becoming quite real. It is not confined to the exotic novel challenge comes from the desire to go even to higher tempera­ ceramics, cermets, etc., which allow one to do things tures, the wish to build even larger cold items, the use of undreamt of only a few years ago. A simple thing like the higher pressures, and from the numerous compatibility tile lining of a vessel was a very adequate way of dealing with a problems {i.e. corrosion, product purity, catalyst performance, reasonably innocuous acid, but now it is possible to build a etc.). There are numerous challenges in every field, but a prestressed tile-lined vessel and consider for instance holding practical hint may amuse some. Pumps, fans and other such hyrdochloric acid in it, or building a pressure vessel in this items sometimes suffer rapid deterioration in service. They way. The first French reactors showed how quite large are then buttered up with various hard metals, etc., and are pressure vessels can be built in concrete whilst the Dracone still in trouble, and then someone bodges them up with an and the various smaller rubber-cum-plastic transport vessels epoxy resin or some similar compound, and that often is the are finding many uses. end of the problem. It is these small things which are often In this competition metals have a great advantage in being so very important. DESIGN FOR DIFFICULT ENVIRONMENTS By D. R. LOVELL, D.L.C., M.Inst.F., A.M.I.Chem.E.,* and A. E. S. WHITE, A.R.C.S., B.Sc* SYNOPSIS Difficult environments are defined for the purposes of this paper as those in which mechanical stress, chemical attack, and thermal shock occur at high temperatures (above about 1200 C). Existing or new designs may be combined with existing or new materials to form four possible methods of combating these conditions. Examples of each method are discussed with reference to problems of kiln-roof design; tube-furnace design; liquid-metal temperature measurement; reactive-metal containers: high- temperature gas-turbine blades and rocket nozzles. Two cases are mentioned where design and materials have advanced independently with the result that progress has been very limited. It is emphasised that the design must suit the properties of the material and that when new materials are developed the application of theoretical principles of, for example, thermodynamics and solid-state physics, can be of great value in guiding the practical investigations and in predicting new compounds and properties. Introduction challenging and, if successful, the most satisfying to a designer, since it requires all his ingenuity and inspiration to devise In the design of chemical-engineering plant it is necessary a solution which in effect avoids the difficulties. to select materials of construction that will withstand the The third route—existing design, new material·—is en­ operating conditions and to produce the component in an countered in three forms: appropriate shape to suit both the available methods of manufacture for the chosen material and the application. (1) The development which occurs in a family of Where the difficult environments considered in this paper materials. The heat-resisting alloys are an example where occur, consisting of chemical attack, erosion, mechanical improvements in materials allow furnace components of stress, and thermal shock at temperatures above about 1200°C, the same design to withstand more difficult environments— the material selected is frequently a ceramic and design higher temperature and larger stresses in corrosive atmo­ problems are increased by the special properties of this type spheres—and successive alloys of a series are suitable for of material and the variability in properties from piece to progressively more severe conditions. piece. (2) When a material of the same family with the neces­ Sometimes it is possible to avoid the difficulties by modi­ sary properties is not available, a change of material can fying the design and using ordinary materials, but as environ­ sometimes be made without affecting the design. In the ments become more difficult new materials have to be de­ construction of muffle tubes for furnaces it is often possible veloped, and these often require a different design because of to use a similar design, although a ceramic is substituted limitations imposed by the material. for a metal casting. There are four possible routes to the solution of a problem. In order of complexity, cost, time required, and effort involved (3) Where neither of these approaches provides a satis­ these are: factory material an attempt has to be made to produce a " tailor-made ", entirely new material to meet the appli­ (1) The use of an existing design using an existing cation. This is a challenge to the materials scientist and material. it becomes increasingly necessary as environments become (2) The production of a new design using an existing more difficult. To carry out such a development success­ material. fully, the thermodynamics and solid-state properties of the (3) The use of an existing design using a new material. system must be considered and this makes possible the (4) The production of a new design using a new material. prediction of properties and of possible new compounds. For the designer to be able to consider all these routes it is The fourth route—new design, new material—has to be essential that the problem is clearly understood and stated used if the available form of the new material prevents the in the broadest terms. For example, by stating a problem as existing design being used, e.g. the new material is available " Design a plant to melt titanium " rather than restricting it only as a casting when the previous design was formed from to " Provide a crucible to contain molten titanium " it is wrought materials, or if the properties of the material impose possible to avoid a difficult materials problem. some restriction on the shape or size of the article, as fre­ The first route is worth some study because a knowledge quently occurs with ceramics. In this case especially, the of the present " state of the art ", especially under operating designer must consider both the material and the application, conditions approaching the limits which the materials will and the interrelation between them.1 withstand, provides a basis on which to develop new designs. Sometimes the designer and the materials scientist find The second route-—new design, existing material—has been themselves out of step so that materials are available that the illustrated in the example on melting titanium and other designer can find very little use for, or the materials scientist examples will be mentioned later. This route is the most is unable to provide a material meeting the designer's needs and the designer cannot devise an economic way of avoiding * Morganite Research and Development Ltd., Battersea Church Road, London, S.W.I 1. the problem. 7 8 LOVELL & WHITE. DESIGN FOR DIFFICULT ENVIRONMENTS of hot-face insulating bricks their mechanical strength is low. These same properties, however, mean that they can be cut easily to shape and rubbed to make mating joints which require only a very thin layer of cement. s mi CAS/MS. TABLE I.—Comparison of Some Properties of Firebrick and Hoi-face Insulation Brick Firebrick H.F.I, brick Refractoriness: Seger cone 32(1710°C) 32(1710°C) Porosity (%) 23 72 Bulk density (lb/ft3) 125 47-5 Thermal conductivity at mean temperature of 800°C (Btu/h ft2 degF in.) 10 3 Cold crushing strength (lb/in2) 2500-5500 140 We have had in use for many years a series of round down- draught kilns working up to 1450°C on a five-day cycle and some of these have been constructed or reconstructed using hot-face insulating bricks. The general arrangement of this type of kiln is shown in Fig. 1 and the roof illustrates the effect of the properties of the material on design. This roof weighs only one-third as much as it would if constructed in firebrick and is best built by laying the bricks in circular courses, each brick being rubbed down from a standard rectangular shape to match the curvature required and the dome being developed by a rotating jig (Fig. 2). It is necessary to cut bricks occasionally to prevent radial joints in a number of courses coming into line, because this would provide a path for a crack to develop. Fig. 3 shows a well- constructed roof and Fig. 4 a poorly-constructed one in which staggering of the radial joints has not been carried out and the rotating jig has moved during the construction. It Fig. I.—Generai arrangement of round downdraught kiln should be noted that the use of cement between the bricks is theoretically unnecessary as the bricks are tapered and should Examples of each of the above routes to a solution have support each other. Although cement is in fact used to occurred in our experience and a description of some of the enable the rings to be built, the movement of the roof during more interesting ones will illustrate the close interrelationship firing produces a number of radial and circumferential cracks between design and materials which is essential when dealing between courses which separate the dome into a series of with difficult environments. mutually supporting panels. Because the expansion cracks open and close as the roof rises and falls on heating and cooling, it is not desirable to cover it with powder insulation Existing Design Using Existing Materials since this percolates into the cracks and prevents them closing. The use of hot-face insulating bricks has become widespread However, a diatomaceous-brick insulation or a slightly in the last 10 to 15 years because of their two great advantages, flexible asbestos-sodium silicate paste layer can be used. low-heat storage capacity and low thermal conductivity, One disadvantage of hot-face insulation bricks has recently compared with ordinary firebrick. Table I provides com­ been overcome by mechanically keying a thin layer of dense parative figures. Because of the low density and high porosity castable refractory to the hot face. This provides an erosion Fig. 2.—Method of constructing domed roof LOVELL & WHITE. DESIGN FOR DIFFICULT ENVIRONMENTS 9 and abrasion-resistant surface without sacrificing much ther­ mal efficiency. A thin firebrick lining to achieve the same purpose would be difficult to bond into the brickwork. In some cases a washcoating can be used. Later in this paper we refer to metal-ceramic thermocouple sheaths for temperature measurement in liquid metals. The design of the furnaces in which these pieces are fired is another interesting example of the effect of the use of refractory materials on design. The problem is essentially that of heating a tube of the largest economic diameter to a tem­ perature of 1600-1850°C over a length of about 18 in. uniformly while maintaining an atmosphere which may be slightly oxidising, inert or reducing, inside it. The heating and cooling rates are not critical but the selected temperature must be controlled to within 5°C (Le. i% of the operating temperature). The cost of kilning the product must be kept reasonably low. The problem is about as easy, in general terms, as it is possible to imagine—merely to heat repeatedly the central portion of a tube to a given temperature—but because the temperature is close to the melting-point of the ceramic material, and the atmosphere must be closely controlled, necessitating an impermeable tube, it is in fact difficult to achieve an economical solution. Nine major issues must be considered: these are detailed below (see also Fig. 5). Material The most readily available material capable of with­ standing 1850°C and providing an impermeable tube about 48 in. long (to give an 18-in. uniform hot zone) is recrystallised Fig. 3.—Well-constructed domed roof alumina. It can be obtained in tubes with diameters up to about 4 in. O/D from stock and larger as special orders. Heating method The cheapest way of heating 30 in. of tube (to give 18 in. uniform) to 1850°C is to wind a molybdenum wire on the tube and use it as an electrical element in a hydrogen atmo­ sphere to prevent oxidization. Size The larger the diameter of the tube the more expensive it is and the lower its resistance to thermal gradients, shock, and mechanical stresses. It is therefore most economic to use the smallest permissible diameter. Temperature control For the accuracy stated a total-radiation pyrometer sighted on a closed sheath touching the heating element is now used. This controls the power to the winding by on/off switching. The performance of tungsten/rhenium thermocouples is now being investigated. Temperature gradients Longitudinal gradients must be restricted to about 125°C/in. for alumina, and with the available length of tube being 48 in. the 15 in. at each end just accommodates such a gradient, provided the distribution is a uniform rate of fall from the end of the 18-in. hot zone. Insulation The insulating material must be of equal purity to the alumina tube to prevent contaminants migrating, and alumina powder is used. To reduce the quantity of expensive powder the lower-temperature outer areas are constructed in insulating brick. The whole is cased in steel to provide a gas-tight container for the hydrogen used to protect the heating element. Fig. 4.—Poorly-constructed domed roof

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