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"I":I.- Hole .-'F Substrates in the Growth of Self-Supporting Thin Films D. Ramsay ;•..'.: .Iru-Vnt of Physics, Stan

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151 "I":i.- Hole .-'f Substrates in the Growth of Self-Supporting Thin Films D. Ramsay ;•..'.: .iru-vnt of Physics, Stanford University, Stanford, California '34305 U.S.A. Tin • purpose of this report is to give the specific parting agents used in •_::•• ;. :vp.ir.il: i.ni of sc 1 f-;-;upporting targets of some 40 elements. I would dlso 1 ik'.• lo iv.'.\ :ie general ;:onc] usions that could be used as guidelines .and -.vhere ;. •oss: :.]• • • :iv" tin' Li.ita tliat led to these generalizations. With .".ill other conditions the same in a vacuum deposition, the choice 'if the sub:, t rate •..•an makJ the difference between depositing a uniform cohesive film <•>>- •r-niiin:-; i !i"; no film at. all. For example, when vanadium is evaporated onto a glass ..;lui-' •.-rated wit . a 2500 angstrom (80 iJgms/cm ) layer of potassium iodide, an ov-r. (•(•ntir.uoii.i film is formed, which can easily be floated off in water and is self- supporting at 500 angstroms (25 ;jgms/cin ). However, if barium iodide is the? sub- strate -outing layer, then the deposition is erratic and will not form a continuous film even if the charge of vanadium is increased by a factor of six. The crystal structure and lattice constant of the material, which is to be deposited, must be considered when choosing a substrate. The formation process of thin films (Fig. 1) begins with the arrival of a single vapor molecule at the substrate (a). If it condenses then it can either niigr.it o across the surface or re-evaporate (b). In migrating, collision can occur ,i:i:l .-ombi nation (c). With the subsequent loss of energy, stable islands are f'-n'H'.J ,\t preferred growth points or adsorption sites, in a process termed iij." 1 • ^jtion (d). With the impinging of more molecules, growth occurs (e) until the a.M-Lis start to coalesce (f). This is an oversimplification of the process, but it •.-.•ij] serve to illustrate how the substrate directly affects the formation of a : ; Jin. The condensing molecule must have an adequate number of adsorption sites (!•'!!!. '?) and these sites must be spaced at an interval which will allow coalesce:,^1 and inhibit re-evaporation. In epitaxial film growth, the matching of the lattice spacing:-; is critical. In pojycrystalline thin films the lattice constant nay not )..•..- critical but it is the determing factor for both the number of adsorption sites .uid the distance between discrete sites. The condensing coefficient and adsorption fiiomy of tiie particular compound are also contributing factors. For instance cadmium films will grow at room temperature on a substrate of ;^inc chloride." Both are hexagonal in structure and have lattice spacinqs of 2.08 and 'J.S2 angstroms, respectively. The critical area for causing stress and creating crystal defects is at the sul strat.e/f ilm interface. Cobalt, which in the bulk solid is normally hexagonal, .:!i!"ortwi in part bv the National Science Foundation- 152 D 'i<i. I- Film cjrowth ssliowinq impingement A; migration and re- evaporation 13; collision C; nucleation D; ijrowtli E; coalescence I-'. POSSIBLE SITE SUBSTRATE ABSORBED ATOM ATOM Fig. 2. Schematic of substrate surface. can be induced to grow at room temperature in a cubic arrangement on a substrate with cubic crystal structure. Below 20 angstroms the lattice is strained to exactly match the substrate. Above 20 angstroms dislocations are generated to accommodate part of the difference between the cobalt and copper lattices. If a film like this were to be removed from its substrate it would disintegrate from internal stress. Ideally, in order to obtain a uniform film, substrates with the same crystalline structure as the depositing material should be used. Fortunately this is not always absolutely necessary. Many elements can be satisfactorily formed on amorphous parting agents such as teepol and fonwar. About one half of 4 the metallic elements are cubic and so are many of the water soluble salts. For some of the hexagonal elements like titanium, yttrium and thulium, there are hex- agonal salts, in this case calcium iodide. Cobalt, scandium, holmium and 154 !•; is' • :x\\r:v.. um • \ r o\\: wo 1 1 on a J uin I n um oxide, J v,':i i f •"; i is . i" Li.- J in/xaqoridi . Jn pracf: _e , -3 2 i_: !• ,i ; .raisiuiii KUbstr.it.o may be as thic.-i as 2. J * 10 cm (/ nqs/cm ) and is etneu .- :" I' i y \i\ ;i:iq in s < ••<! i' un hydroxide and then distilled ijtur. Car-; nust bo taken i • :...- n! y aluminum which has been expGS"d to air ] a:w onouqh for the oxide cat :•.!•: !o i'yrn on the surface. In this method residua] contamination eould not : i . :• i.-.it-. ii iy iookinq for q.-iimiia rays from r rot on-induced roacti ons. This C.;YCS :n -:r:-i-r !i::i;t of :.<. r: ::• m-i/cm" to tlie aJumimi;:! conlent •:;•:' tJie tar(jdt. :h"ie ai"" exf [ft i'.ir.'- to tji i J a;!proiii.-h. Altliouqii barium rhlorido i:; ort::n- r : .• ii:: i i •, j i v,T(;rks we11 '! foi" bery] i i tiin w}]i';}i is hexagonal. .^ui -.'X^ la.nation may ;.-' ( in the '•,'•-]"/ snail ijiain si;.:e (dci-'idar structure) or the very iarqe lattici.- onn- -.;-.u!t rjf iia) i urn chloride^ ('i.V> anqstronis) . Also r. u'.-ianc -;.».:-, which is "ubi.?, con- '•• :!•••..: v.-r 1! us a roharorct fill-, on aluminun o:dd>', v/:iich i^; hexaqona!. .\:v \.\:Y fac"Lor in tiie pr^i'.tration of sel f-s'lpi'jort inq films is the tem; -eratar'j . ••!" 'h- ::.:;..; t rate . If the substrate temperature if; very low, say 76 Kelvin (liquid :. i !.!"•;:.••..•!.) i oiid,vn ; a t: on is so fast and the afci jnobi ] i tis.'S so low, that they can- not r.i':i thr; usual positions they occupy in tli> crystal lattice. The filn is :'•.• r, iinplelely disordered or amorphous. If the temperature is sufficiently hiqn thin i:i'il.,i l ; |-y of t!;e atoms is hiqii and sinq Le crystal films may be qrov.'n. I-Y-r ; ;.":•.'••:•',': til] im> si• 1 f-supp'Ortinq films the p.articular temperature is not as irripor- ''. in t a..; ::iru n t.ai :i i ::q the sarifj temperature durinq t'ne qrov.'tl; of tlie- film. 7 ":" you I] row a i"Ton film on a teopol-ooatea1 qlass slide, suspended by itself, •:..• fi 1 ni will, shatter around _!U00 anqstroms (50 ..qms/cm"). If it is grown on a ; •:. :,.:_.i., . .chlfride .aitoil q],oss slide; JOB ivin tjet to about 4000 angstroms (100 • :•••••./ :n"; . if i i i :•: qrown on a thin Jayor of boron on a glass slide which lias : • • :. •. x; . i:-.-.-d to .<!.'-" (f iius oxi ;1; zin'i the surface to boron oxide) you can qo to a ':,: •-.'.••.;:; of i.i. • 10 cm (4:lJi aqms/onD. Iri th i s case, what appears to bo an ::, ' ,,n •• "f therm.il strain is not entirely true. ;:. the coins./ of depositinq a film, an increase in the temperature of the ••.•:' ! it'' comes from tiie radiation <jf the evaporation source and the heat absorbed ! .'..:: !•!•• i.ondensinq atoms. If we i\ilculate the heat rise due to the latter for a .' ;•• :.'••!•'." :,i l'/rij- fiJm urown on .) qlass slide (Fiy. 5) we find it to lie 1.5°C. (.: 7 M C T ac; acj a-.: 1 qs •; s g s _ ^ C •- 'A C 'final a q a1j q yy q.s ma s s i n cj r ams i: - silver s ;. e ••.• i f i <_• heat t ois;.'r; r a t u re °C •i 1 ass slide Fiq. 3 155 ,: ! " i ::i.i>: imum increase from 15°C to 16.5°C. It is possible then to qrov: a i :-i •..-I'iicMt introducing any large temperature changes in the substrate due to :,.!"iisi]iq atoms. '.'ifTO are two approaches for avoiding temperature build-up in the substrata . •:. ; ,1.: i .it ion. Tile Eirst is to minimize the amount of heat radiated from the :: • MM!.ion iniurci:. If the time of evaporation is short, or the vaporization •; "r.itur" low (•' 1200°C) often no special precautions have to be taken at alJ . :..• i i i ::is liko bismuth and lead are simply grown with the parting agent (in this '.•••.: i mi! iodide and potassium chloride) on a glass slide suspended by itself. :: '.-.': M- v.ipori zation temperature is very high (> 1200°C) often the area of •.r'••:!- radiation can be reduced and effectively shielded or water cooled. ••In:- ; i I:;:; for example, with source temperatures of > 2700°C have been grown 9 : i! •:. slide coated with sodium chloride. The electrostatically focused • -i :' .i 'iun was water-cooled and the area of exposed radiation was only 1/8 of '.):•:, in diameter. Since the amount charged was small (~ 30 mgs) for thick i •. •.••V'MviI evaporations were made, but no curling or shattering was found even i • :.i V.IK'SS of 4!3OO angstroms (1 mg/cm ) . •':. • s.'ct'iid approach is to compensate for the radiant heat by removing hoat -:i -..•• subslrat" at a rate which will keep the temperature constant. What is ••I-:.mi. is that tiie initial condensation layer must not occur at a much lower •:•••!•.i' .:rc (".Ii-Tsi the final condensation. This would lead to excessive thermal ii.i.-. ;u'ii;ii built into the film. Temperature gradients across a 1 mm thick i ; sli.-'ii.
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